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  • Column liquid chromatography  (495)
  • phosphorus  (208)
  • Springer  (703)
  • 2020-2024
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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Aquatic sciences 53 (1991), S. 263-272 
    ISSN: 1420-9055
    Keywords: Lake ecosystem ; chl-a ; phosphorus ; nitrogen ; river flow ; thermocline ; simulation model ; multiple regression
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract The management variables which primarily affect phytoplankton biomass (as chl-a) in Lake Mjøsa, Norway, are total phosphorus loading (TP) and the timing and volume of water through flow (by active storage reservoirs). The response of the lake to changes in these factors is studied using a simulation model of the lake ecosystem. Chl-a responses from both observed data and the simulated results are extracted by multiple regression. Results show that decreasing TP load decreases chl-a, but less at low TP levels (〈 10 mg TP · m−3). There is also a certain time period for peak river flow which gives the least yield of chl-a per unit TP. This time period occurs in early summer (i.e., around June 10) if the total phosphorus load is low, and later if the load is high. Both observations and simulation results show that a high water flow increases chl-a at low epilimnion depths (〈 15 m), but that the same high water flow decreases chl-a when epilmnion is deep.
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  • 2
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    Aquatic sciences 52 (1990), S. 199-220 
    ISSN: 1420-9055
    Keywords: Eutrophication ; lake management ; phosphorus ; ecosystem ; chlorophyll-a ; mathematical modelling
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract We compare results of a new model for predicting the short term inter annual changes in chlorophyll-a (chl-a) in lakes after reductions in total phosphorus (TP) to predictions made by least squares regression models. In the new method, slopes of chl-a/TP graphs (both axes in mg · m−3) are depicted in frequency diagrams and used to extract information on the expected, short term chl-a/TP response. The short term response for nine shallow (〈 10 m deep) and nutrient rich lakes to changes in TP was found to be: Chl-a = 0.49 · TP + 17.3, and for nine deep, P-limited lakes: Chl-a = 0.08 · TP + 3.5. If the TP-reduction is known to be greater than 10 mg · m−3, the expected slope increases to 0.58 for shallow lakes and to 0.26 for deep lakes. The slope, 0.58, is 8% lower than the slope for the long term response calculated by regression for the shallow lakes. For deep lakes the slope, 0.26, is 2 to 3 times higher than that calculated by regression, indicating that reductions in TP for deep lakes give greater effects than least squares regression equations suggest. We have also calculated the reduction in TP which will give about 80% probability that a reduction in chl-a will be observed next year. For shallow, P-limited lakes this reduction is about 30 mg · m−3 (5% of average initial in-lake TP concentration), and for deep lakes about 14 mg · m−3 (35% of average initial in-lake TP concentration).
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  • 3
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    Aquatic sciences 52 (1990), S. 256-268 
    ISSN: 1420-9055
    Keywords: Vertical mixing ; stratification ; phosphorus ; Lake Constance
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Depth variable vertical eddy diffusion coefficients for heat (K z) were calculated from continuously measured temperature profiles in Überlinger See (western part of Lake Constance). The temperatures were averaged over vertical intervals of 10 m yielding 14 discrete values (maximum depth of Überlinger See: 147 m). A linear fit from 10 June to 29 September 1987 was used to smooth the significant temperature fluctuations caused by internal seiches of Lake Constance. Assuming horizontal homogeneity for the smoothed data the Gradient-Flux-Method was applied to compute vertical diffusion coefficientsK z at different depths using the depth variable volumes and surfaces of the 14 layers. The resulting mean diffusion coefficients for the period from June to September are 0.04 cm2/s near the thermocline and up to 0.8 cm2/s in deeper strata (accuracy: ± 50%). It is shown that horizontal mixing between Überlinger See and Obersee (main lake) alters the computation ofK z by less than 50%. A relationship betweenK z and stability (Brunt-Väisälä) frequencyN is found which corresponds well to the theory of internal wave induced turbulence. Combining the diffusion coefficients with measured phosphorus profiles, a phosphorus flux from the hypolimnion to the epilimnion of (0.7 ± 0.4) mg P m−2 d−1 was calculated, corresponding to about 20% of the average external loading per area of Lake Constance in 1986.
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  • 4
    ISSN: 1420-9055
    Keywords: Sediment ; interstitial water ; phosphorus ; iron ; persulfate digestion
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract It is shown that sorption of orthophosphate to iron compounds, formed during persulfate digestion, can cause a significant underestimation of total dissolved phosphorus in interstitial waters rich in iron and poor in phosphorus. Labelling the samples with carrier free32PO4 before digestion allows to correct for these losses.
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  • 5
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    Microchimica acta 101 (1990), S. 273-279 
    ISSN: 1436-5073
    Keywords: aluminium analysis ; phosphorus ; sulfur ; chlorine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Multi-step procedures for the determination of phosphorus, sulfur and chlorine are described and tested against established methods and on reference materials. Phosphorus is separated as hydrogen phosphide, extracted as phosphomolybdic acid, reduced to molydenum blue and measured photometrically (detection limit 0.05 μg/g). Sulfur is separated after reduction as hydrogen sulfide or by means of pyrohydrolysis and measured by ICP-OES (detection limit 0.1 μg/g). Chloride can be measured by ion chromatography after pyrohydrolytic separation (detection limit 0.1 μg/g). The determination of sulfur was also successfully tested on copper and steel samples.
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  • 6
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    Microchimica acta 109 (1992), S. 201-209 
    ISSN: 1436-5073
    Keywords: phosphonate base scale inhibitor ; brine ; direct current plasma ; inductively coupled plasma atomic emission spectrometry ; phosphorus
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The determination of phosphonate base scale inhibitors in brines by direct current plasma (DCP) and inductively coupled plasma atomic emission spectrometry (ICP-AES) is described. The first method is based on a direct nebulization of the brine samples and plasma using the phosphorus line at 213.618 nm. The second method involves extraction of phosphorus as phospho-antimonyl molybdate complex into methylisobutyl ketone (MIBK) phase and analysis of the extract for molybdenum using the Mo 313.260 nm line. Comparison between the proposed methods and an established recommended method [1] shows excellent agreement between the results in addition to the sensitivity and ease of automation provided by AES.
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  • 7
    ISSN: 1573-0417
    Keywords: Great Basin ; climatic variations ; productivity ; organic matter ; nitrogen ; phosphorus ; hardwater lake
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Geosciences
    Notes: Abstract Sediment cores from the shallow and deep basins of Pyramid Lake, Nevada, revealed variations in composition with depth reflecting changes in lake level, river inflow, and lake productivity. Recent sediments from the period of historical record indicate: (1) CaCO3 and organic content of sediment in the shallow basin decrease at lower lake level, (2) CaCO3 content of deep basin sediments increases when lake level decreases rapidly, and (3) the inorganic P content of sediments increases with decreasing lake volume. Variations in sediment composition also indicate several periods for which productivity in Pyramid Lake may have been elevated over the past 1000 years. Our data provide strong evidence for increased productivity during the first half of the 20th Century, although the typical pattern for cultural eutrophication was not observed. The organic content of sediments also suggests periods of increased productivity in the lake prior to the discovery and development of the region by white settlers. Indeed, a broad peak in organic fractions during the 1800's originates as an increase starting around 1600. However, periods of changing organic content of sediments also correspond to periods when inflow to the lake was probably at extremes (e.g. drought or flood) indicating that fluctuations in river inflow may be an important factor affecting sediment composition in Pyramid Lake.
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  • 8
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    Nutrient cycling in agroecosystems 36 (1993), S. 127-133 
    ISSN: 1573-0867
    Keywords: hydrology ; water balance ; phosphorus ; Streamflow ; Peel-Harvey
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract This paper discusses the land types, hydrologic characteristics and processes, and the major modification of these, in relation to mechanisms and magnitude of phosphorus losses to drains and riverine systems which discharge to the Peel-Harvey estuary. About 75% of the coastal plain part of the catchment is cleared of native vegetation and used for dryland, dairy and beef grazing. There are small areas devoted to irrigated pasture and commercial horticulture. Seventy-five percent of the soils of the catchment are sandy surfaced with a poor capacity to retain phosphorus. Though the area is flat, catchment water yields are high because of a large winter rainfall excess and low soil storage capacity. Drainage schemes have been constructed in much of the catchment to remove excess water quickly. This was required initially to allow agricultural expansion and is now important for protecting a growing infrastructure which serves the most populous region of Western Australia.
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  • 9
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    Nutrient cycling in agroecosystems 37 (1994), S. 1-22 
    ISSN: 1573-0867
    Keywords: animal slurries and manures ; applications to soils ; carbon- ; nitrogen- ; phosphorus ; contamination ; crop production ; dissemination ; hazardous organics ; heavy metals ; inputs ; macro- and micronutrients ; pathogens ; sewage sludges ; survival- ; transfer- ; transport and adsorption rates in soils
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract The European Community is producing annually about 300 × 106 tons of sewage sludges as well as about 150, 950,160 and 200 tons of domestic, agricultural, industrial and other wastes (street litter, dead leaves etc.). About 20–25% of the German sewage sludges, which contain in average about 3.8,1.6, 0.4, 0.6, 5.3% DM−1 N, P, K, Mg and Ca, 202, 5, 131, 349, 53, 3 and 1446 mg kg−1 DM Pb, Cd, Cr, Cu, Ni, Hg, Zn as well as ca. 37 and 5 mg kg−1 Dm polychlorinated hydrocarbons and biphenyls, are recycled annually as fertilizer. In addition environmental impacts on the arable land of Germany may derive from 76,19.2, 64.7, 33.6, 7.8 and 0.1 kg ha−1 a−1 of N, P, K, Ca, Mg and Cu added as animal manures. Besides heavy metals and hazardous organics pathogens are disseminated with organic wastes. Crop production and soil fertility generally profit from the considerable amounts of plant nutrients and carbon in sewage sludges, animal slurries and manures, but the physicochemical soil properties, the composition of microbial, faunal and plant communities as well as the metabolic processes in the soil-, rhizo- and phyllosphere are changed by organic manuring. Consequences for the soil carbon-, nitrogen-and phosphorus-cycle are discussed. Impacts of heavy metals and hazardous organics on the soil biomass and its habitat as well as on transport mechanisms and surival times of disseminated pathogens in soils are reviewed with emphasis on the German situation. A proposal for future strategies (landscape recycling) is made.
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  • 10
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    Nutrient cycling in agroecosystems 27 (1991), S. 107-111 
    ISSN: 1573-0867
    Keywords: Liming ; phosphorus ; heathland ; copper ; fertilization ; forest
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract Forest fertilization in the Netherlands has played an important role in the phase of afforestation of former heathlands. Research started in the early fifties, but results were not applied in practical forestry. A review is presented on forest fertilization in practice, and on the main results of the activities of De Dorschkamp on NPK fertilization, liming and micronutrients application. Attention is paid to problems which have developed during the past ten years.
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  • 11
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    Nutrient cycling in agroecosystems 26 (1990), S. 253-269 
    ISSN: 1573-0867
    Keywords: Nitrogen ; phosphorus ; sulphur ; nutrient balances ; surface waters ; North Sea ; Baltic Sea ; eutrophication ; hypertrophication ; primary production
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract Dissolved inorganic nitrogen and phosphorus, their relationship to each other (DIN/DIP) as predisposing (nutrient) factors, as well as prevailing weather as a triggering factor all work together to induce the primary production and hence the eutrophication (hypertrophication) process in surface waters. Sulfate likewise is a decisive predisposing factor influencing the eutrophication process by reducing N availability but increasing P availability and thus acting towards an N limitation of the primary production. This is one of the reasons why marine (coastal) waters and estuaries often exhibit N limitation with respect to primary production, while freshwater ecosystems often tend to exhibit P limitation. Within the N and P balance of agriculture of some countries of Western Europe (Netherlands, Denmark, Switzerland, FRG, UK and Sweden for N, resp. Netherlands, FRG and GDR for P) more the level than the efficiency of the N and P applications indicates the extent of the nutrient surplus. Despite 59–73% N utilization in plant production, the rate of 13–23% for agriculture as a whole equals to the 12–21% efficiency of N use in animal production. The varying N surplus in agriculture in the separate countries of 124 to 465 kg N ha−1 a−1 is determined almost exclusively by the level of the N application and not by its efficiency. The situation is similar for P: In spite of P utilization in plant production of 59–76%, P utilization in total agriculture is only 11–38%, or comparable to the P efficiency within animal production of 10–34%. The differing P excess balance of 55 to 88 kg P2O5 ha−1 a−1 is influenced by the level of the P application. The N and P efficacy of total agriculture hence is determined almost completely by that of animal production, since 83–95% (N basis) and 76–94% (P basis) of the total plant production (on top of the nationally varying levels of N and P use via imported feeds) are fed to animals — with the low N and P utilization cited above. Agriculture's share of the N and P emissions into surface water of several countries/regions in Western Europe (FRG, Netherlands, Italy, Denmark, Switzerland, Norway) ranges from 37 to 82% resp. 27 to 38%. Its share in the flus into the North Sea catchment basin will be about 60% for N and 25% for P related only to the anthropogenic material carried by the rivers. Agriculture's share in the atmospheric N emissions into the North and Baltic Seas can be estimated at about 65% or 55%, resp. while the remaining approx. 35% or 45%, resp. are traceable primarily to anthropogenic burning processes. For agriculture the priority lies in limiting N emissions into surface water caused by leaching, erosion and NH3 emissions, and reducing P emissions mainly through soil conservation (protection against erosion) and water protection. As regards N this means a demand for comprehensive protection of groundwater and atmosphere differentiated according to the potential for losses or the risk of losses on a site, also outside the protection zones. As regards P only those areas can be included in the demand for reduction of emissions that are actually threatened by erosion or surface runoff. Plenty of short-term and long-term measures are available to agriculture to reduce N and P emissions. Especially the long-range measures (such as creating nutrient balances on farms and fields, the integration of animal and plant production, maintaining maximum livestock densities according to the ability of areas to absorb nutrients, altered feeding programs in animal nutrition, changes in livestock keeping (slurry→deep litter), increasing the internal and external recycling of N and P) are capable of bringing about a satisfactory degree of success within the next 20 to 30 years.
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  • 12
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    Nutrient cycling in agroecosystems 40 (1994), S. 165-173 
    ISSN: 1573-0867
    Keywords: Animal manure ; eutrophication ; ground water ; nitrogen ; phosphorus ; surface runoff
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract With the rapid growth of the poultry industry in Oklahoma, U.S.A., more litter is applied to farm land. Thus, information is required on the impact of applications on regional soil and water resources. The effect of soil and poultry litter management on nitrogen (N) and phosphorus (P) loss in runoff and subsurface flow from four 16 m2 plots (Ruston fine sandy loam, 6 to 8% slope) was investigated under natural rainfall. Plots under Bermudagrass (Cynodon dactylon) received 11 Mg litter ha−1, which amounts to contributions of approximately 410 kg N and 140 kg P ha−1 yr−1. In spring, litter was broadcast on 3 of the plots; the upper half of one and total area of the other two. One of the total-area broadcast plots was tilled to 6 cm, the other remained as no till. The fourth plot served as a control. Relative to the control, litter application increased mean concentrations of total N and total P in runoff during the 16-week study for no-till (15.4 and 5.8 mg L−1) and tilled treatments (16.7 and 6.1 mg L−1). However, values for the half-area application (5.6 and 2.0 mg L−1) were similar to the control (5.7 and 1.3 mg L−1). Interflow (subsurface lateral flow at 70 cm depth) P was not affected by litter application; however, nitrate-N concentrations increased from 0.6 (control) to 2.9 mg L−1 (no till). In all cases, 〈 2 % litter N and P was lost in runoff and interflow, maintaining acceptable water quality concentrations. Although litter increased grass yield (8518 kg ha−1) compared to the control (3501 kg ha−1), yields were not affected by litter management. An 8-fold increase in the plant available P content of surface soil indicates long-term litter management and application rates will be critical to the environmentally sound use of this nutrient resource.
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  • 13
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    Nutrient cycling in agroecosystems 37 (1994), S. 107-113 
    ISSN: 1573-0867
    Keywords: Ensete ventricosum ; fertilizer response ; nitrogen ; phosphorus ; potassium ; sulphur ; starch
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract Ensete (Ensete ventricosum W. Cheesm.) is a root crop which stores starch in the root and in the lower part of the stem. It is grown in the southwest of Ethiopia and due to its drought resistance, it is of outstanding importance for the supply of food to the local population. Until now virtually nothing is known about the response of Ensete to fertilizer application. Field trials carried out on three representative soils in Ethiopia showed that Ensete biomass yields were increased significantly on all three soils by nitrogen and phosphorus application. Potassium had only marginal effect on biomass growth but favourably influenced starch production. Sulfate application had no major impact on growth and starch yield. The yield response was well related to the level of available nutrients in the soil, as determined by electroultrafiltration (EUF). Leaf analysis provided preliminary evidence that optimum levels of N, P, and K may be 3.8%, 0.3%, and 4.8%, respectively.
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  • 14
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    Nutrient cycling in agroecosystems 35 (1993), S. 217-226 
    ISSN: 1573-0867
    Keywords: calcium ; dry matter distribution ; fertilizer ; harvest index ; magnesium ; manure ; millet ; nitrogen ; nutrient uptake ; phosphorus ; potassium ; Senegal
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract In a fertilizer and manure experiment, millet was grown under four treatments (no fertilizer or manure, farmyard manure, chemical fertilizer, and both). Grain yield and total aboveground biomass production of the unfertilized plot were relatively high. The observed differences in total dry matter production must be attributed to differences in nutrient availability, as amount of rainfall and its distribution were favourable. Results show only small differences in distribution of dry matter among the various plant organs between the best and the non-fertilized treatments. Nutrient supply from natural sources, defined as crop content of N, P, and K at maturity without fertilizer application, amounted to 104, 16 and 103 kg ha−1, respectively, which are very high values. Total uptake of calcium and magnesium is related to that of potassium, as the combined content of these three elements is linearly related to total aboveground biomass production. Minimum removal of nitrogen and phosphorus per ton grain dry matter amounts to 29 and 4kg, respectively, and 9 kg potassium per ton total aboveground dry matter. A possible double function of phosphorus as element of structural biomass and for maintenance of electro-neutrality is discussed.
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  • 15
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    Nutrient cycling in agroecosystems 36 (1993), S. 95-103 
    ISSN: 1573-0867
    Keywords: eutrophication ; phosphorus ; fertilizer ; Peel-Harvey estuary ; algal blooms
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract An excess of plant nutrients has caused serious eutrophication in aquatic ecosystems of southwestern Australia manifested by excessive growth and accumulation of green and bluegreen algae. Phosphorus is generally the limiting nutrient for algal growth and phosphatic fertilizers applied to nutrient-deficient, leaching, sandy soils are the main source of P, supplemented by rural industry point sources. Nitrogen is the limiting nutrient in marine embayments with little drainage from the land. Measures to reduce the load of P delivered to drainage include basing fertilizer application rates on soil testing for P and the use of less soluble P fertilizers. Catchment management plans are being implemented with community involvement to reduce P loads and maintain agricultural production. This introductory paper reviews the history of eutrophication in southwestern Australia and of studies into its causes, principally in the large Peel-Harvey estuary. It briefly summarises other papers in this special issue concerned with different aspects of the problem: how to fertilize the land without causing eutrophication.
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  • 16
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    Nutrient cycling in agroecosystems 36 (1993), S. 115-122 
    ISSN: 1573-0867
    Keywords: phosphorus ; retention ; release ; sandy soils
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract In order to manage phosphorus (P) losses from soils to waterbodies, knowledge of the mechanisms through which P is retained or released from the soil is essential. Sandy soils of the Peel-Harvey catchment (Western Australia) were subjected to a range of environmental and management factors in the laboratory and field in order to gain an understanding of the mechanisms that affect the magnitude of P losses. Sandy soils accumulated P, despite having little sorption capacity, and this accumulation could be monitored by measuring an acid-extractable fraction. The potential, short-term P loss could be estimated by determination of water-soluble soil solution P prior to winter rains. An annual cycle of the change in arbitrarily defined soil-P pools is discussed in relation to environmental and management factors. Laboratory experiments indicated that P rundown and potential annual P loss in the absence of P fertilizers could be estimated using bicarbonate extractable P. Phosphorus losses were decreased by the application of fertilizers with a low content of water-soluble P. The low ability of sandy soils of the Peel-Harvey coastal catchment to retain P, when compared to other Western Australian soils, is because of low contents of clay minerals and iron and aluminium hydrous oxides.
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  • 17
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    Nutrient cycling in agroecosystems 26 (1990), S. 229-235 
    ISSN: 1573-0867
    Keywords: Grass ; wheat ; nitrogen nutrition ; dilution curve ; mineral content ; mineral removal ; phosphorus ; potassium
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract The important effect of nitrogen in changing the patterns of mineral content and mineral removal is analysed for grass swards and wheat. Different models are proposed; accumulated dry matter developed throughout a growing period is shown to be an excellent reference for assessing the evolution of the plant mineral content and the mineral removal the growing crop. Applications in diagnosing mineral nutrition status and optimising fertilizer use are proposed and discussed.
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  • 18
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    Nutrient cycling in agroecosystems 32 (1992), S. 223-227 
    ISSN: 1573-0867
    Keywords: Soil testing ; phosphorus ; relative yield
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract A greenhouse experiment, with Okra (Abelmoschus esculentus L.) as the test crop, was conducted on twenty-one soils ranging in Olsen's extractable phosphorus from 1.8 to 15.5µg Pg−1 soil. The experiment was conducted at Punjab Agricultural University, Ludhiana, India. The soils were nonsaline with pH ranging from 7.7 to 8.6. A critical level of 2.55µg Pg−1 soil was predicted by Cate and Nelson's (1971) statistical procedure. Because of a wide range in relative yields, this value did not accurately predict response to applied P. An approach to compute minimum response to applied fertilizer, which is likely to be obtained at a particular Olsen P level, has been presented. It involves calculation of lower 60 percent confidence limits for relative yield and fitting loge-linear regression to the transformed data. The regression was tested on a published data set and was found to hold well.
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  • 19
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    Nutrient cycling in agroecosystems 32 (1992), S. 259-267 
    ISSN: 1573-0867
    Keywords: Nitrogen ; phosphorus ; timber increment ; fertilization ; Pinus radiata
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract Two trials inPinus radiata growing on different sites in N.S.W. allowed consideration of fertilizer applications after 2nd or 3rd thinning. The trials included factorial applications of N and P at a single thinning intensity plus a further treatment which allowed assessment of different thinning intensities. The most significant growth responses were obtained by application of N and P in combination. The largest response (additional productivity compared with the unfertilized control) occurred 4 years after application and after 7 years there was no additional absolute response for either of the two sites. The largest fertilizer response was 70 m3 ha−1 over 7 years on one site and 36 m3 ha−1 on the other, indicating differences in absolute responses between sites. It was concluded that in planning treatments the most responsive sites near the end of the rotation should be selected to maximise economic returns. Foliage analyses indicated differences between sites at the commencement of the study. It was concluded that either a single year of foliage analyses at study commencement is of value, or sampling every year of the study should be used to analyse responses, but a single year of analysis during or at the end of the study would not be of value.
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  • 20
    ISSN: 1573-0867
    Keywords: interaction ; isotopic exchange ; phosphorus ; plant-availability ; selenium ; soil
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract Phosphate, applied at 5µg P cm−3, decreased selenite sorption by from 30–70% in three soils studied. Both maximum sorption (Xm) and the binding-energy of sorption as indicated by the binding-energy related constant (k) or the molar free energy (ΔG) of the sorption reaction derived from the Langmuir equation were considerably decreased. On the other hand, phosphate sorption was decreased by increasing concentration of selenite from 0.2µg Se cm−3 to 1.0µg Se cm−3 in the initial solution. The competitive sorption of phosphate with selenite was likely the main mechanism involved in the P-Se interactions. The competitively sorbed selenite exhibited much larger desorption in 0.01M CaCl2 solution, more readily extractable to 0.5M NaHCO3 and significantly higher isotopic exchangeability compared to that sorbed without the competing anion. Results from pot trial using ryegrass indicated that phosphate application increased more efficiently the plant-availability of applied fertilizer Se than that of indegeneous Se in soil.
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  • 21
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    Biodegradation 14 (1991), S. 167-191 
    ISSN: 1572-9729
    Keywords: leaf longevity ; nitrogen ; nutrient use efficiency ; phosphorus ; requirement ; retranslocation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Energy, Environment Protection, Nuclear Power Engineering , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract Aboveground nitrogen (N) and phosphorus (P) requirement, retranslocation and use efficiency were determined for 28-year-old red oak (Quercus rubra L.), European larch (Larix decidua Miller), white pine (Pinus strobes L.), red pine (Pinus resinosa Ait.) and Norway spruce (Picea abies (L) Karst.) plantations on a similar soil in southwestern Wisconsin. Annual aboveground N and P requirements (kg/ha/yr) totaled 126 and 13 for red oak, 86 and 9 for European larch, 80 and 9 for white pine, 38 and 6 for red pine, and 81 and 13 for Norway spruce, respectively. Nitrogen and P retranslocation from current foliage ranged from 81 and 72%, respectively, for European larch, whereas red pine retranslocated the smallest amount of N (13%) and Norway spruce retranslocated the smallest amount of P (18%). In three evergreen species, uptake accounted for 72 to 74% of annual N requirement whereas for two deciduous species retranslocation accounted for 76 to 77% of the annual N requirement. Nitrogen and P use (ANPP/uptake) was more efficient in deciduous species than evergreen species. The results from this common garden experiment demonstrate that differences in N and P cycling among species may result from intrinsic characteristics (e.g. leaf longevity) rather than environmental conditions.
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  • 22
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    Aquatic sciences 54 (1992), S. 58-76 
    ISSN: 1420-9055
    Keywords: Eutrophication ; lake management ; phosphorus ; nitrogen ; chlorophyll-a ; slope estimator
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    Topics: Biology
    Notes: Abstract We estimate the response of chl-a (mg · m−3) to changes in concentrations of total phosphorus (TP) by calculating the slopeS = Δchl-a/ΔTP in chl-a =f(TP) graphs. Results show that in years where algae are P-limited oligotrophic lakes respond less (median slope 0.21) to changes in nutrient concentrations than eutrophic lakes, (median slope 0.31) and these again less than hypereutrophic lakes, (median slope 1.02). We find no saturation value for the slope within the TP range considered (6–480 mg · m−3). Chl-a in eutrophic lakes responds more frequently to non-nutrient factors than oligotrophic and hypereutrophic lakes. Results obtained by replacing TP with a new nutrient parameter, TP′ = 0.056 · TP · IN0.226, in which inorganic nitrogen, IN, is factored in, suggest that nitrogen has an influence on chl-a in oligotrophic lakes. Blue-green algae respond less to changes in TP than other algal species, e.g., diatoms.
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  • 23
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    Aquatic sciences 54 (1992), S. 381-390 
    ISSN: 1420-9055
    Keywords: Eutrophication ; phosphorus ; lake restoration ; internal restoration measures for lakes ; Swiss lakes ; Lake Lugano (Lago di Lugano)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract In most lakes eutrophication is linked to an excessive input of phosphorus. Lake restoration by reduction of P-input (external measure) has led to a considerable drop of the P-concentration in all major Swiss lakes as well as in many other lakes. Internal restoration measures such as artificial mixing, drainage of hypolimnetic water, flushing, aeration, biomanipulation and others serve to improve and accelerate the response of a lake to external measures. For the case of Lago di Lugano, a simple two-box model is employed to demonstrate that a reduction of the P-input to about 25% of the present values is necessary to reach the “P-criterion” (P-concentration below 30 µg/l). Internal measures could possibly accelerate the extremely slow response of the northern basin.
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  • 24
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    Aquatic sciences 55 (1993), S. 132-142 
    ISSN: 1420-9055
    Keywords: nitrogen ; phosphorus ; uptake ; regeneration
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    Topics: Biology
    Notes: Abstract Dissolved inorganic nutrient pools are small relative to particulate pools, and dissolved pools turnover rapidly. It has been observed that pools change little from day to day on the sampling scales usually employed. A simple model is presented where uptake and regeneration rates balance to cause a local steady state concentration for dissolved inorganic nutrients. Enrichment and dilution perturbation experiments with lake water support the idea of steady state nutrient concentrations. Although inorganic nutrient concentrations are often controlled by biota, the absolute concentrations present tell little about the activity of that biota.
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  • 25
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    Aquatic sciences 56 (1994), S. 16-28 
    ISSN: 1420-9055
    Keywords: Chlorophyll-a ; phosphorus ; nitrogen ; lake ecosystem ; nutrient limitation ; regression analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract Regression results based on data from 46 northern temperate lakes show that total phosphorus (TP) is the best predictor for phytoplankton (as chl-a) at lower trophic levels, TP 〈 200 mg · m−3. A regression including both TP and TN as regressors is the best predictor for lakes with TP 〉 200 mg · m−3. However, the good correlation is probably due to a high correlation between lake average chl-a (all years observed) and lake average TP and TN. Within single hypereutrophic lakes, TN alone is the best predictor. It was not possible to identify a medium trophic domain where TN and TP in combination was the best predictor for chl-a. The ratio TN:TP in the water decreases from about 40 to about 5 with increasing trophic level. Optimum TN:TP ratio for algal species with high abundance during late summer and autumn reflects this decreasing ratio, but within a lesser range, i.e., 20 to 5. In contrast, TN:TP ratios for species abundant during the early vernal period showed no, or an inverse, relation to the TN:TP ratio of the water.
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  • 26
    ISSN: 1432-0495
    Keywords: Nitrogen ; phosphorus ; Precipitation collector ; Nutrients rates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences
    Notes: Abstract The contribution of nitrogen and phosphorus due to precipitation constitutes the second most important route after superficial runoff. The sampling carried out during a two-year period by means of a precipitation collector allows us to determine the contribution of this route both qualitatively and quantitatively. Nitrogen is mainly supplied in an inorganic form, while phosphorus is principally supplied as orthophosphate. During the period of this study (March 1986–February 1988) it was found that in the Santillana Reservoir Watershed the level of nitrogen supplied by precipitation constitutes an average of 4.87% and the level of phosphorus constitutes 8.01%. The contribution of nitrogen varies in inverse ratio to precipitation and the contribution of phosphorus varies in direct ratio.
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  • 27
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    Journal of chemical ecology 16 (1990), S. 2429-2439 
    ISSN: 1573-1561
    Keywords: Cucumis sativus ; ferulic acid ; split root ; phosphorus ; potassium ; water ; net uptake
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Since distribution of allelopathic compounds in soils is highly variable, injurious effects by such compounds should be related to the frequency of contact with roots. Experiments were conducted to determine how P, K, and water uptake of cucumber seedlings were affected as the fraction of roots in contact with ferulic acid (FA) was increased. Seedlings were grown in Hoagland's nutrient solution for 14 days and then transferred to 0.5 mM CaSO4 solution for 24 hr before being placed into a split-root culture system. The containers in the system were filled with 0.5 mM concentrations of KH2PO4 and CaSO4 or 0.5 mM concentrations of KH2PO4, CaSO4, and ferulic acid (FA). Net uptake of P by seedlings (milligrams per seedling) decreased in a curvilinear (concave) manner as the fraction of the roots in contact with FA increased. Net uptake of K (milligrams per seedling) and water (milliliters per seedling) by seedlings decreased linearly as the fraction of the roots in contact with FA increased. Net uptake of P, K, and water by seedlings was reduced 57, 75, and 29%, respectively, when the whole root system was exposed to FA. Net P and K uptake of roots (milligrams per gram root fresh weight) not in contact with FA decreased in a linear and curvilinear (convex) manner, respectively, as the fraction of roots in contact with FA increased. Net P and K uptake of roots in contact with ferulic acid increased in a linear and curvilinear (convex) manner, respectively. Net water uptake of roots (milliliters per gram root fresh weight) not in contact with FA increased in a curvilinear (concave) manner as the frequency of the roots in contact with FA increased. Net water uptake of roots in contact with FA did not show a trend. Transpiration (milliliters per square centimeter) was reduced in a linear manner as the fraction of roots in contact with FA increased. A very slight compensation by roots not in contact with FA for roots in contact with FA was observed for net water uptake rates. No compensation for P and K uptake rates was observed.
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  • 28
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    Potato research 33 (1990), S. 13-21 
    ISSN: 1871-4528
    Keywords: hormones ; media ; phosphorus ; rooting depth ; solar radiation ; temperature
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    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Summary To expand potato production in developing countries using cuttings as a source of good quality planting material, requires simple low cost methods to root and establish them. Experiments at a warm tropical site in the Philippines, to determine appropriate methods, showed that simple media ranging from fine sand to clay subsoil mixed with rice hulls enabled rooting which was not improved by hormones. Nitrogen rich media, such as volcanic soil or compost with additional P, were best for developing cuttings into strong transplants but there were no major differences in root and shoot development from cuttings differing in size and age. Tuberizations was favored by increasing the number of nodes buried in the media. Low solar radiation of 7 MJ/m2/day enabled high cutting survival up to root initiation, after which higher radiation supported larger root and shoot production.
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  • 29
    ISSN: 1573-9171
    Keywords: EPR ; radical ; fluorine ; conformation ; phosphorus
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract EPR spectra of radical adducts of phosphonyl radicals with 2-hydroperfluoro-4-methyl- and 4,4-dimethyl-2-pentene have been studied. The molecular mechanics method has been used to determine the preferred conformation of the (CF3)2CF-CF-HCF3P(O)(OMe)2 radical. The eclipsed conformation of the C–P bond and 2p z -orbital of an unpaired electron is stabilized due to steric factor and hyperconjugation.
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  • 30
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Bovine milk ; Multivariate optimization ; Glycerophospholipids ; Molecular species separation ; Chemometrics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The molecular species profile, representing the fatty acid combinations on the glycerol backbone, is the most fundamental description of an intact glycerophospholipid class and provides a key to understanding its functional characteristics. We have developed a powerful RP-HPLC method for the separation of molecular species, including so-called “critical pairs”, of natural mixtures of 1,2-diacyl-sn-glycero-3-phosphocholine 1,2-diacyl-sn-glycero-3-phosphoethanolamine from bovine milk and other natural sources. We have used a novel multivariate development and optimization strategy to locate the region of optimum separation conditions within a prechosen domain of the chromatographic parameter space.
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  • 31
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Open tubular columns ; Cross-linked polyacrylate stationary phase ; Photopolymerization ; Antracene derivatives
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    Topics: Chemistry and Pharmacology
    Notes: Summary Polyacrylate films containing a lauryl moiety were fabricated on about 12 μm I.D. fused silica capillaries by in-situ photopolymerization of acrylates. Relatively thick films up to 1 μm were obtained by the technique. The films were tested as retentive layers for reversed phase open tubular liquid chromatography (OTLC). Due to the presence of the incorporated lauryl moiety in the layer considerable retention could be achieved for polar compounds with aqueous mobile phases. The efficiency of the prepared columns approximates to the theoretical value. The polyacrylate films appear to be extremely stable even under strong basic conditions. The films swell considerably in the presence of nonpolar solvents resulting in more favourable retention and a significant improvement of the chromatographic performance.
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  • 32
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    Chromatographia 35 (1993), S. 627-630 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fatty acid analysis ; Fish oils
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    Topics: Chemistry and Pharmacology
    Notes: Summary A chromatographic method has been developed for the determination of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) in fish oil dietary supplements containing triglycerides rich in (n−3) polyunsaturated fatty acids (PUFAs). Following the ester saponification, free fatty acids were resolved by TLC into two fractions: i) a more mobile group of saturated and monounsaturated fatty acids and ii) a less mobile group containing PUFAs. The PUFA fraction was further analyzed by HPLC to determine the levels of EPA and DHA in the fish oil sample.
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  • 33
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carbidopa and levodopa in plasma ; Electrochemical detection
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    Topics: Chemistry and Pharmacology
    Notes: Summary A validated reversed-phase high-performance liquid chromatographic procedure employing electrochemical detection (LCEC) for the analysis of carbidopa and levodopa in human plasma is reported. The method is sensitive and specific with amperometric detection at a glassy carbon working electrode with Eapp=0.75 V vs. Ag/AgCl. The retention times of levodopa, internal standard, and carbidopa are 3.3, 4.5, and 9.7 minutes, respectively, with an overall chromatographic run time of 12.0 minutes. The peak height ratio versus plasma concentration is linear over the range of 5.0 to 500 ng/mL for each analyte and exhibits correlation coefficients of 0.9957 or better (n=9). The mean absolute recovery of carbidopa and levodopa using the described assay is 36.6 and 66.0%, respectively. The inter- and intra-day accuracy and precision are within 11.8% of the actual values for all concentrations. Also, due to the demonstrated instability of carbidopa and levodopa in plasma a procedure is provided to circumvent this. Blood collected in pre-treated Vacutainer tubes can be stored in an ice bath for up to 4 hours without any significant degradation, thereby providing a practical means for processing several clinical samples simultaneously.
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  • 34
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fullerenes ; FullereneSep® ; Separation factor ; HPLC-particle beam mass spectrometry
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    Topics: Chemistry and Pharmacology
    Notes: Summary High-performance liquid chromatographic separation of fullerene mixtures in the range C60 to C100 can be achieved using a novel stationary phase which rivals the performance of the more expensive ‘Pirkle-type’ columns currently employed.
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  • 35
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    Chromatographia 35 (1993), S. 675-678 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion chromatography ; Trace metal determination ; Sample contamination ; Human hair
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The dynamic ion-exchange chromatographic analysis of bivalent ions, such as Cu, Pb, Zn, Ni, Co and Mn in resistant organic matrices needs preliminary wet ashing with oxidizing acids (HNO3 and HClO4). Such treatment may lead to an increase in the amounts of metals present in the sample due to their release from containers or equipment used in an acidic environment and to metal impurities contained in the acids. The effect of these interferences in the determination of trace metals in human hair was studied.
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  • 36
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Normal phase separations ; Cyanopropyldimethyl silica ; Chloro-added polycyclic aromatic hydrocarbons ; Environmental samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Retention characteristics in normal phase HPLC of highly biologically active chloro-added polycyclic aromatic hydrocarbons (PAHs) were studied. Silica, cyanopropyldimethylsilyl- and aminopropylsilyl- modified stationary phases were investigated. Retention properties of chloroadded PAHs on these phases were shown to be strongly influenced by the number of chloro-additions. This is due to the strong polarity of the methylene carbon at the chloro-addition site. Active silica had a strongly degrading effect on the unstable chloro-added PAHs during separation. Aminopropylsilica did not exhibit sufficient selectivity towards chloro-added PAHs when compared to chlorosubstituted PAHs. Cyanopropyldimethylsilica was shown to be applicable to a group separation of chloro-added and chloro-substituted PAHs. A fast clean-up procedure for chloro-added PAHs in complex samplesis outlined. It involves an initial elimination of more polar substances on a short open column with strongly deactivated silica and a subsequent separation on a cyanopropyldimethylsilyl HPLC column in normal phase mode.
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  • 37
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    Chromatographia 32 (1991), S. 345-349 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Column packings ; Pore size distribution ; Diffusion and adsorption ; Band broadening
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    Topics: Chemistry and Pharmacology
    Notes: Summary The complex intraparticle structure typical of chromatographic column packings has been analyzed by use of an equivalent network model which emphasizes pore size distribution and connectivity. Special attention is given as to the way in which diffusion and adsorption interact and display modified peak spreading characteristics according to the morphology of the pore space. This study reveals a very significant increase in the column band broadening over that expected from physical adsorption which can arise from particular distributions of pore sizes. This has implications for designing packings which take advantage of the separating power due to adsorption but do not compromise the resolution of the chromatographic system.
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  • 38
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; GC/ECD detection ; PCBs, ortho and non-ortho ; Chromatographic separation ; Congener determination ; FTIR identification
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An analytical procedure for the individual determination of ortho and non-ortho PCB congeners in sediments, using high performance liquid chromatography (HPLC) preseparation and gas chromatography/ECD detection, is described. Gas chromatography/FTIR spectrometry (GC/FTIR) and gas chromatography/mass spectrometry (GC/MS) were employed for individual congener identification and determination. Sample extraction, clean-up of extract and selective elution procedures were optimized by using reference certified marine sediment samples. Recovery and precision were typically 83% and 16% respectively at 2 ng/g of total PCB content. The proposed procedure, tested by analyzing real sediment samples, showed a reproducibility better than 20% at 13 ng/g PCB level.
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  • 39
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Glutamine ; Pyroglutamic acid ; Amino acids formulations
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    Topics: Chemistry and Pharmacology
    Notes: Summary The aminoacid glutamine in aqueous solution and in conditions of high temperature and long term storage is partly transformed into pyroglutamic acid which exhibits potential neurotoxic effects. Commercially available aminoacid mixtures supplemented with glutamine are heat-sterilized and some losses of glutamine and formation of pyroglutamic acid may occur. The aim of the work was to set up an easy and reliable HPLC method which allows the determination of pyroglutamic acid as a degradation product of glutamine. The column was a 5 μm Hypersil ODS (100×4.6 mm) and the mobile phase 100% 0.007 M phosphate buffer pH 3.5. Stability studies in different conditions of temperature and time of storage were performed on aminoacid mixture available in the commerce.
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  • 40
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carbonyl compounds ; Luminarin hydrazides ; Fluorescence detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Fluorogenic reagents (luminarin 3, luminarin 11 and luminarin 12), having a quinolizinocoumarin moiety as fluorophore and a carboxylic acid hydrazide function as reacting group, have been developed. These reagents were found to be highly sensitive fluorescence derivatization reagents for aldehydes and ketones in high-performance liquid chromatography. The reagents readily react with carbonyl compounds in aqueous sulphuric acid solution (0.1 M) at room temperature to produce the corresponding hydrazone derivatives, which can be separated on both reversed or normal-phase column. The structures of the derivatives were studied, together with their properties in reversed and normalphase chromatographic systems. UV absorbance, corrected fluorescence spectral data and quantum yields of luminarin 3, luminarin 11 and luminarin 12 are presented. The detection limits (signal to noise ratio=3) for aldehydes and ketones were in the sub-pmol range. Luminarin 3 was also applied to the determination of hydroxymethylfurfural (HMF) in orange juices and concentrates. The method for HMF involves the solid-liquid extraction of the juice by using a C-18 cartridge prior to derivatization and normal-phase separation of the derivative with fluorimetric detection at 387 nmex., 444 nm em. The calibration curve was linear for amounts of HMF ranging from 0.1 to 10 nmol. Intrarun relative standard deviation was 12.8% for 0.1 nmol and 2.6% for 1 nmol. Recovery studies indicated an average of 98.7±1.9% for juice concentrate and 99.8±3.2% for pasteurized juice.
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  • 41
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Method development ; Chemometrics ; Response criteria ; Analysis of drug purity
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    Topics: Chemistry and Pharmacology
    Notes: Summary Optimization procedures require adequate response criteria to assess the quality of each chromatogram obtained during the process. The objective of this paper is to evaluate the possibility of using different resolution functions, in the chromatographic separation of a drug and its impurities (particularly the impurity just eluted after the drug). This study shows the limits of some resolution expressions. The interest of the simple Δt criterion, the difference between retention times, is presented in this paper.
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  • 42
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    Chromatographia 36 (1993), S. 147-151 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polarity ; Retinoids
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    Topics: Chemistry and Pharmacology
    Notes: Summary The retention of retinoids in reversed-phase liquid chromatography was studied using aqueous mobile phases of different composition (methanol 94–86% and acetonityrile 92–82%) at five temperatures (40–60 °C). With both organic modifiers the effect of the molecular structure increased as the water content and the polarity of the mobile phase increased. The temperature-dependence increased in the same manner with aqueous acetonitrile mobile phases. The π-π interactions between the retinoids and acetonitrile diminish when the water content of the mobile phase is increased, as happens also to the hydrophobic interactions with both organic modifiers. The net effect of these changes depends on the composition of the mobile phase. There was excellent correlation of retention with all polarity parameters studied(ϕ, P′, xe, xd, xn, E T N , δT, δ, δo and δd), when the calculations were made separately with methanol and acetonitrile. The volume fraction of the organic modifier, ϕ, was the only parameter describing the retention well in both organic modifiers simultaneously.
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  • 43
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Aromatic amines ; Arylbenzylamide methylthioether derivative ; SL 85.1016 ; Pharmacokinetics
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    Topics: Chemistry and Pharmacology
    Notes: Summary An HPLC method has been developed for the determination of SL 85.1016, a new calcium antagonist arylbenzylamide methylthioether derivative. SL 85.1016 and the internal standard, SL 87.0210, are extracted from alkaline human plasma withn-hexane and back extracted into 0.05 M phosphate buffer (pH 2.5; 0.2 ml). Acetonitrile (50 μl) is added to the final aqueous extract in order to prevent absorption of the compounds of interest onto the walls of the glass tube; this solution then is partially processed by HPLC on a C18 column with UV detection (254 nm). The determination limit of the method is 2 ng.ml−1 of SL 85.1016 in human plasma; the response to the drug is linear in the range 2–200 ng.mg−1.
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  • 44
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    Chromatographia 36 (1993), S. 347-350 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Allium ; Derivatization ; S-alk(en)yl-L-cysteine sulfoxides ; Sulfur amino acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two pre-column derivatization procedures coupled with reversed phase HPLC have been compared for the analysis ofS-Alk(en)yl0L-cysteine sulfoxides in variousAllium species. In order to establish external standards some (+/-) sulfoxides were synthesized, using a new method to enhance asymmetric synthesis of the diastereoisomers. The first derivatization method is the formation ofo-phthaldialdehyde/tert.-butylthiol derivatives which can be analyzed using UV detection. The second, presently used for amino acid analysis, is the Waters Pico-Tag method, which employs phenylisothiocyanate as derivatization reagent. As the Pico-Tag method was found to be the most efficient for determination ofS-alk(en)yl-L-cysteine sulfoxides it was used to determine the alliin content of various samples of garlic.
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  • 45
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fatty acids and bile acids ; Fluorogenic precolumn derivatization ; 2-Bromoacetyl-6-methoxynaphthalene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The use of 2-bromoacetyl-6-methoxynaphthalene as a fluorogenic labelling reagent in pre-column derivatization for the HPLC separation of biologically active carboxylic acids (fatty acids and bile acids) has been investigated. The compound reacts (30 min. at 70°C) with carboxylic acids to give fluorescent esters that can be separated by reversedphase HPLC and detected at λ ex. 300 nm, λ em. 460 nm. The experimental conditions for the derivatization and chromatographic separation are discussed. Applications to the determination of valproic acid and chenodeoxycholic acid in pharmaceutical formulations are described.
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  • 46
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Valproic acid ; Simultaneous determination of anticonvulsants
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The derivatizing procedure of Moody et al. [20] for valproic acid has been simplified and applied to the simultaneous HPLC determination of valproic acid (VPA), barbital (B), primidone (PRM), phenobarbital (PB) and carbamazepine (CBZ) in serum or plasma of epileptic patients. The sample is deproteinized with acetonitrile containing esterification agents and an aliquot of the supernatant is heated to 70°C for 15 min with 4-bromophenacyl bromide. The reaction mixture is analysed on a C18 column at ambient temperature, with gradient elution and with detection at 205 nm. The time required for the chromatographic analysis is 13 min; identification is based on retention time and quantification is by peak area determination with an internal standard. The calibration curves show good linearity in the range 6.25 to 100 mg/L. The detection limits at a signal: noise ratio ≥3, ranged from 1 mg/L for B and CBZ to 2–3 mg/L for PRM, PB and VPA. The method described for the simultaneous determination of the five drugs in the same plasma pool, correlated well with isocratic HPLC methods specific for each drug. The simultaneous procedure described allows a reproducible (CVs≤6.5% within run) and rapid (25 min for sample preparation: 13 min for chromatographic run) therapeutic monitoring of patients treated with VPA and two or more antiepileptic drugs.
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  • 47
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Porous polymer spherical packings ; Vinyl ether ; Alkali resistance ; No abnormal adsorption
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Spherical, porous-polymer particles for column packing in high-performance liquid chromatography were prepared by suspension copolymerization of alkylvinyl ether with triethyleneglycol divinyl ether. The hydrophobicity of the packings was easily adjusted by changing the monomer ratio. The packings showed the usual reversed-phase liquid chromatographic properties, but did not sho abnormal retention, tailing and broadening of peaks and irreversible adsorption of ionic and aromatic substances, owing to the lack of ionic or aromatic groups. In addition, the packings were stable in alkaline solutions because of the relative alkali stability of C−O−C bonds as compared with CO−O and Si−O−C bonds in conventional packings.
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  • 48
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Anion exchange ; Indirect photometric and direct conductivity detection ; Naphthalenesulfonate ; Inorganic anions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Indirect photometric and unsuppressed direct conductivity detection modes are examined using naphthalene mono-, di-, and tri-sulfonate as mobile phases for the separation of several anions such as F−, Cl−, NO2 −, Br−, NO3 −, SO4=,I−, and SCN− using a commercial anion exchange column. With all three mobile phases, conductivity detection shows better sensitivities and detection limits than indirect photometry. Conductivity detection is 5 to 16 times more sensitive than indirect photometry for all analytes. Detection limits achieved using these mobile phases are, for example, 0.04 ng and 0.1 ng for chloride ion with conductivity and indirect photometry, respectively. Both detection modes give wide linear ranges extending from at least 100 ppm to the detection limit of each anion which is generally about 0.02 ppm. Sulfur oxide anions such as dithionate and tetrathionate are separated using flow programming with naphthalenetrisulfonate as the mobile phase in less than 20 minutes. With both detection modes, desired chromatographic performance of these three eluents is achieved without pH adjustment of the mobile phase.
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  • 49
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Heat-treated milk ; Milk quality indicators ; 5-Hydroxymethyl-2-furfuraldehyde
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An enhanced method of HPLC for the determination of 5-Hydroxymethyl-2-furfuraldehyde (HMF) in fluid milk was perfected. Its resolving capacity permitted the specific separation of this compound. The real concentration (μmol/l) of HMF was determined and not the HMF value, as in the colorimetric analysis, where an intermediary coloured compound (HMF-TBA) is utilised. The optimum pH condition (pH=4.0–4.2) for the mobile phase to prevent overlapping between the HMF peak and the peaks of the other compound (α and β) that coeluted with the HMF and also the optimum organic solvent content (3% or 7%) were established. This is a sensitive, quick and safe method for the determination of HMF in fluid milk.
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  • 50
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chlortetracycline ; Reversed-phase silical gel ; C8 bonded phase ; Collaborative study
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An established method for the analysis of chlortetracycline by liquid chromatography using octylsilylated silica gel as the stationary phase was examined in a multicentre study involving five laboratories and a total of six columns. Three chlortetracycline hydrochloride samples were analysed. The main component and the impurities were determined. An analysis of variance, treating each column as a different laboratory, showed an absence of consistent between-laboratory bias and the presence of a significant laboratory-sample interaction. The repeatability and the reproducibility of the method, expressed as relative standard deviations of the result of the determination of chlortetracycline hydrochloride, were calculated to be 0.9% and 1.1% respectively.
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  • 51
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    Chromatographia 37 (1993), S. 627-634 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; ODS phases ; NMR and FTIR characterization ; Stationary phase functionality
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Two spectroscopic methods, solid state NMR and diffuse reflectance FTIR, have been used in conjunction with liquid chromatographicretention data to identify and distinguish the functionality of octadecylsilica (ODS) stationary phases. NMR and FTIR spectra are indicative of various features of the different functionalities of the phases and this information can be used to elucidate the configuration of the organosilyl moiety in the ODS on the silica surface and explain why DSS phases have different molecular shape (mainly planarity) recognition capability.
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  • 52
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    Chromatographia 37 (1993), S. 423-428 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polymer-modified silica ; Polypyrrole cloride ; Polypyrrole dodecylsulfate ; Small molecules ; Polyaromatic hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Polypyrrole chloride and polypyrrole dodecylsulfate coated-silica packing materials have been synthesized. Reverse-phase chromtographuy was employed to characterise both packings. A series of test compounds with known properties was used as molecular probes. They included benzene and derivatives, basic drugs, and polyaromatic hydrocarbons. A commericial C18 column was also used for the purpose of comparison in some cases.
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  • 53
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Arsenic compounds ; Polymeric styrene divinylbenzene phase ; Ion-pairing
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The resolving power of an ion-pair reversed-phase liquid chromatography method, on a polymeric stationary phase (PRP-1) with an alkaline aqueous mobile phase (pH=9) containing tetrabutylammonium cation as ion-pairing agent, is compared with a traditional ion-pairing system using an octadecyl-modified silica column and a neutral aqueous mobile phase (pH=7.3). This chromatographic system (PRP-1 column) provides a rapid means for the determination of two of the most important arsenic species, arsenobetaine and arsenite. Addition of methanol (5%) to the aqueous mobile phase allows the differentation of arsenobetaine from the system peak when using UV detection.
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  • 54
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gravity-flow column chromatography ; Provitamin A determination
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The provitamin A content of some food samples was determined by methods involving MgO: Hyflosupercel gravityflow column chromatography (GFCC) and reversed phase high performance liquid chromatography (HPLC), the quantitation being done by external standardization (HPLC-ES) or internal standardization (HPLC-IS) with Sudan. The results obtained with α- and β-carotene in carrots, β-carotene and β-cryptoxanthin in papaya and β-carotene in tomato and kale agreed well, showing that any of the these techniques can be used, provided the analysis is done under optimum conditions. Good separation of the different provitamins using GFCC depends on the analyst's skill and visual acuity. HPLC-ES required a constant supply of provitamin standards, thus the varying purity of commercially available standards and the high instability of these compounds could pose grave problems. Due to the stability of Sudan, HPLC-IS appeared to be the method of choice although passage of the extract through a MgO: Hyflosupercel minicolumn was required prior to injection to separate chlorophylls, dihydroxy- and polyoxycarotenoids which would otherwise elute with Sudan. Nonconformity of the Sudan structure to those of the provitamins did not effect the quantitative results. The chromatographic separation, identity and quantification of the provitamins could be more easily established by using HPLC-IS, complemented with GFCC.
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  • 55
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    Chromatographia 33 (1992), S. 103-112 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography ; Chiral separations ; Allethrin ; Cypermethrin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Liquid and gas chromatographic separations of the pyrethroid insecticides allethrin and cypermethrin have been investigated with various achiral and chiral stationary phases. Diastercomeric and enantiomeric selectivity was observed for cypermethrin on a Pirkle-type chiral LC stationary phase, but very strong interactions and therefore long retention times prevented the separation of allethrin on this phase. Trans-allethrin isomers were separated on a chiral β-cyclodextrin RP-HPLC column while cypermethrin showed some difficulties on this phase due to isomerization. Diastereomeric but no enantiomeric selectivity by GC was achieved for cypermethrin with an apolar DB 5 capillary. GC separation of the diastereomers was used to study the selective photodegradation of cypermethrin isomers after forestry applications. Chiral β-cyclodextrin-based GC phases showed some enantioselectivity for cis- and trans-allethrin isomers. A separation of the eight isomers into six partially resolved peaks was achieved by GC with a coupled column consisting of chiral permethylated β-cyclodextrin and DB 1701 as stationary phases. This combination was used to characterize allethrin formulations intended for indoor use and to investigate allethrin products formed by ozonolysis of thin films of the insecticide.
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  • 56
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiralcel OD ; N-Alkyl-N-methylanilineN-oxide enantiomers ; Chiral nitrogen centre ; Flavin-containing monooxygenase
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A high-performance liquid chromatographic method for the resolution of the enantiomers of a series ofN-alkyl-N-methylanilineN-oxides is reported. The resolutions were achieved using a Chiralcel, OD chiral stationary-phase with a mobile-phase of hexane and ethanol in varying proportions. The chromatographic order of elution of the enantiomers ofN-ethyl-N-methylanilineN-oxide was determined to be (+)-(R) before (−)-(S).
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  • 57
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    Chromatographia 37 (1993), S. 539-542 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Sotolon ; Vin jaune ; Flor-sherry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Sotolon (4,5-dimethyl-3-hydroxy-2(5H)-furanone) is a key flavour compound in the french flor-sherry “Vin jaune”. This compound was determined quantitatively by extraction of 25 ml of wine on a XAD-4 resin, elution with diethyl ether, separation by HPLC on a Lichrospher 100 Diol column, elution with dichloromethane/hexane (60/40) and UV detection at 232 nm. The amount of sotolon in “Vin jaune” (120 to 268 μg/l) was related to the development of the yeast film over a period of 6 years. Only 6 to 51 μg/l were found in the “Vin de paille” which is made with overmaturated grapes of the same Savagnin vine-plant but without development of yeasts, and 80 to 140 μg/l in “Tokai” which are partly grown under a yeast film.
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  • 58
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Column-switching ; Determination of triamterene ; Fluorescence detection
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    Topics: Chemistry and Pharmacology
    Notes: Summary A liquid chromatographic method incorporating column-switching and fluorimetric detection for the determination of triamterene in untreated urine, is described. The urine samples (5 μL) were directly introduced onto an Hypersil ODS-C18, 30 μm (20 mm×2.1 mm I.D.) pre-column. Polar urinary compounds were removed by flushing the pre-column with water for 1 min, and the analyte was then switched onto an HP-LiChrospher RP C18,5 μm (125 mm×4mm ID) analytical column using an acetonitrile/phosphate buffer gradient elution. Fluorescence detection was performed at 230 nm excitation and 430 nm emission wavelengths. The recovery of drug was 102±2% in the 0.10–20.0 μg/mL concentration range, the limit of detection being 5 ng/mL. A validation of the usefulness of this procedure was accomplished by analysing urine extracts obtained from real samples.
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  • 59
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Characterization of reversed phases ; Column hydrophobicity ; Column hydrophylicity
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    Topics: Chemistry and Pharmacology
    Notes: Summary The validity of a method for characterizing stationary phases for reversed-phase, liquid chromatography, based on the use of homologous series, has been evaluated. The method is based on a retention model which describes the dependence of the logarithm of the capacity factor on mobile phase composition and the carbon number of specific homologous series. A first-order as well as a second-order version of this model was investigated. The second-order model proved to be a significant improvement on the first-order model, even for smaller mobile-phase ranges. Nevertheless both models showed a significant lack of fit, reflecting the incompleteness of these models. Therefore, it is very questionable whether this method is suitable to describe HPLC-column characteristics like hydrophobicity and hydrophylicity.
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  • 60
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Copoly(styrene/acrylonitrile) ; Gradient elution ; Precipitation chromatography of polymers ; Solubility of polymers
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    Topics: Chemistry and Pharmacology
    Notes: Summary Copolymers from styrene and acrylonitrile could be separated according to composition by gradient elution through methanol after injection inton-heptane and sudden addition of 50, 60, or 70 vol% tetrahydrofuran. The peak sequence was the same as with a common binary gradientn-heptane/tetrahydrofuran, i.e., retention increased with acrylonitrile content of the samples. With copolymers containing 37, 31, or 26% acrylonitrile, the elution characteristics in the ternary systems could be logically extrapolated towards the points measured in the corresponding binary gradient system.
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  • 61
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral recognition ; Aminoalkylphosphonic acid derivatives ; β-cyclodextrin bonded phases
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    Topics: Chemistry and Pharmacology
    Notes: Summary An acetylated β-cyclodextrin column was used to analyse the enantiomeric resolution of a number of aminophosphonic acids. Effects of the structure of these compounds on the extent of separation was examined. Molecular modelling studies were also carried out in an attempt to relate any interaction between the amino and phosphonic acid groups to chiral recognition by the stationary phase.
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  • 62
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    Chromatographia 33 (1992), S. 177-185 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Diuretics ; Screening and determination of diuretics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary This critical review of different methods proposed for the determination and screening of diuretics is directed mainly, because of its potential application, towards highperformance liquid chromatography.
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  • 63
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    Chromatographia 33 (1992), S. 218-224 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Peak ; Pattern recognition ; Prediction interval
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary It is still difficult to determine peaks and peak boundaries properly, though peak recognition is very important for the precision of quantitative data. A new computer program overcomes these problems using a method which is adapted from human judgements. The algorithm was developed for HPLC but can also be used in other fields of analytical chemistry.
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  • 64
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral separation ; Association constants ; Frontal analysis ; Cyclodextrin bonded-phases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The interaction between cyclodextrin and the drug (1R,2S,3S,4S)-(5Z)-7-(3-((phenylsulfonyl)amino)bicyclo[2.2.1]hept-2-yl)hept-5-enoic acid ((+)-S-145), was studied using α-, β-, and γ-cyclodextrin bonded-phase columns. Retention behavior of (+)-S-145 on these columns revealed that the strength of inclusion was β→γ→α-cyclodextrin. Interaction between β-cyclodextrin and (+)-S-145 was found to increase as the proportion of carboxylic ion in the (+)-S-145 molecule increased. Comparison of binding capacities of these bondedsilica gels obtained by frontal analysis and surface coverage indicated that availability of the immobilized β- and γ-cyclodextrin was 20–25%. The synthesized β-cyclodextrin bonded-phase column was superior to that of commercial columns in terms of chiral separation of (±)-S-145. A typical usage of the β-cyclodextrin column is discussed for separation of (±)-S-145 in plasma samples.
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  • 65
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Primary and secondary aliphatic alcohols ; Aqueous derivatization ; Phthalic acid monoesters
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    Topics: Chemistry and Pharmacology
    Notes: Summary Determination of primary and secondary aliphatic alcohols in aqueous and nonaqueous solutions by high-performance liquid chromatography (HPLC) is described. The alcohol is derivatized with phthalic anhydride to yield the corresponding monophthalate. Separation of the derivative is achieved on an ODS-10 reverse phase (RP) column by elution with an appropriate isocratic mobile phase of acetonitrile and aqueous phosphoric acid (0.1%). Detection is accomplished by UV absorption at 230 nm or 280 nm giving linear calibration plots, for alcohols in aqueous solution from 0.05% to 0.50% (w/v) and in pyridine solution from 0.0025% to 0.0250% (w/v).
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  • 66
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Hybrid mobile phases containing alcohols ; Solute-micelle association constants ; Polynuclear aromatic hydrocarbons
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    Topics: Chemistry and Pharmacology
    Notes: Summary The interaction between some polynuclear aromatic hydrocarbons of environmental concern, and sodium dodecylsulphate and hexadecyltrimethylammonium bromide in the presence of methanol, 2-propanol and n-butanol has been evaluated by high-performance liquid chromatography using micellar mobile phases. Solute-micelle association constants have been determined for the compounds investigated. The results show that the addition of the alcohol to the mobile phase decreases the association constant values, methanol 〈2-propanol 〈n-butanol, relative to those in the absence of any additive.
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  • 67
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    Chromatographia 38 (1994), S. 571-578 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Wine ; Biogenic amines ; Solid-phase extraction ; Derivatization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method suitable for the determination of 19 biogenic amines in wine has been developed. The method involves derivatization of amines by treatment with dansyl chloride and solid-phase extraction of the derivatives. Prior to the derivatization procedure, clean-up of the wine sample with polyvinylpyrrolidone is carried out. Reversed-phase gradient elution HPLC with UV detection at 250 nm was used to determine these compounds. Some consideration was given to the effect of temperature on the separation process. Linearity of derivatization was obtained for amounts of all the biogenic amines ranging from 500 μg·L−1 to 20 mg·L−1. Limits of detection (signal-to-noise ratio=3) of the amines were similar for all the dansylderivatives (between 50 and 150 μg·L−1). Addition of standard amines was used for the determination of amine recoveries. These were better than 85% for ethanolamine, tryptamine, phenetylamine, putrescine, cadaverine and histamine. The overall process was succesfully applied to identify and quantify biogenic amines in white and red wines.
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  • 68
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chiral/enantiomeric iseparation ; Cellulose-based chiral phases ; Tifluadom analogues ; 2-acylaminomethyl-1,4-benzodiazepines
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The resolution of nine recamic mixtures of tifluadom analogues has been evaluated using the chiral stationary phases Chiralcel OD and Chiralcel OJ. The separation was performed on an analytical scale to optimize the conditions for chiral resolution, approaching baseline separation, of the two enantiomers. Eight racemates were baseline separated on Chiralcel OJ using a mobile phase of hexane/2-propanol.
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  • 69
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Diol silica gels ; Carbohydrates ; Evaporative light scattering detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Bonded silica columns have been evaluated for their ability to separate carbohydrates and polyols. Mobile phases consisting of dichloromethane/methanol produced the best separations in comparison with the acetonitrile/water mixtures commonly used with amino columns. Of all the bonded phases tested, LiChrospher Diol silica provided the best separations, and selectivities were not very different from those obtained on the most popular system using an amino bonded phase and acetonitrile/water as eluent. In addition, diol columns with a dichloromethane/methanol eluent offer excellent stability with no Schiff’s base formation of reducing sugars. Using an evaporative light scattering detector, low limit detection is obtainable (20 ng of glucose from a column) and gradient elution is quite feasible.
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  • 70
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Phenolic compounds ; Ion-pair solid-phase extraction ; Comparison of sorbents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A comparative study of the solid phase extraction of phenolic compounds in water was carried out. Three different sorbents, C18, CH and PLRP-S, were tested for the preconcentration process in order to determine phenolic compounds in water at μg l−1 levels by reversed-phase LC separation and diode-array detection. The addition of an ion-pair reagent in the extraction process was also studied in order to increase the breakthrough volume of some compounds. Using the optimized conditions the limit of detection was less than 0.5 μg l−1, the maximum admissible concentration (MAC) in drinking water. The method was applied to determine phenolic compounds in Ebro river water however no phenols were found within the detection limits of the method.
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  • 71
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Extraction-determination ; Basic drugs ; Blood
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new method for the extraction of basic drugs from whole blood based on the use of a buffered protein precipitating reagent at pH9, to form NiWO4 in biological fluids and a ternary organic extracting phase of density below 1 is proposed. The extract is analysed by high performance liquid chromatography using a Hypersil C8 column and detection at 230 nm; the mobile phases used consist of binary mixtures of acetonitrile and aqueous solutions containing 20 mmol/l ofn-propylamine at pH 5 andn-hexylamine at pH 4, as blockers of the free silanol groups. The proposed method was applied to the determination of 16 basic drugs including narcotics, analgesics, cocaine-related compounds and adulterants, as well as 8 benzodiazepines, in whole blood.
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  • 72
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    Chromatographia 39 (1994), S. 62-66 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Column switching ; Imidazolinone herbicides in soil ; Imazethapyr ; Imazapyr
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A column-switching method using two separation columns combined with UV detection at 260 or 236 nm has been used to determine the imidazolinone herbicides imazethapyr and imazapyr in soils. The residues were extracted from the soil with 0.1 M aqueous sodium carbonate solution and, after adjusting the pH to 2.0, the solution was partitioned with dichloromethane. Limits of determination for imazethapyr and imazapyr were 3 μg/kg. Recoveries were from 55 to 75% for both imidazolinone herbicides in the range 3–100 μg/kg in soil.
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  • 73
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Porous graphitized carbon ; Ring-substituted aniline derivatives ; Electronic interactions ; Principal component analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention characteristics of 22 aniline derivatives were determined on a porous, graphitized-carbon column in unbuffered acetonitrile-water and methanol-water mixtures. Each aniline derivative gave symmetrical peaks in each eluent without buffers. Good linear correlations were found between the log k′ and the concentration of the organic component in the eluent. The slope and intercept values differed according to the type of organic modifier and the charcter, number and position of substituents, indicating the different selectivities of methanol and acetonitrile and the good separating power of the column. Multivariate mathematical-statistical calculations proved that the retention of ring-substituted aniline derivatives is mainly governed by electronic parameters and the hydrogen acceptor capacity of substituents.
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  • 74
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion-pairing ; Furosine ; Pyridosine ; Milk
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An ion-pair, reversed-phase, liquid chromatographic procedure using UV detection for quantitation of furosine is described. The standard plot was linear (r〉0.999) over a 5 ng range. An authentic synthesised sample of furosine was used for calibration. Commerical milk samples were analyzed by the described procedure.
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  • 75
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Automated peak detection ; Discrete Fourier transform ; Frequency acquisition and filtering ; Peak detection
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The principle of automated chromatographic peak detection and analysis software is summarized, and critical steps are systematically studied. As the only parameter to be entered is the acquisition frequency, evaluation of its effect on software performance is discussed. In the case of relatively noisy chromatograms, it is shown experimentally that numerous points per peak have to be taken, leading to quite fast computer acquisition procedures. The use of discrete Fourier transform filtration techniques can modify peak shapes and a comparative study evaluates the relative errors induced in the shapes and characteristics of the chromatographic profiles. Optimisation of filtering conditions is achieved and it is shown that for a filter position only 2% of the Nyquist frequency no deformation occurs in the chromatographic profile. Detection of the start and finish of chromatographic peaks is optimized according to a simple four step iterative procedure. In the case of simulations, the difference between the values used to simulate peaks and those calculated by the software are less than 1%.
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  • 76
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    Chromatographia 39 (1994), S. 246-248 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Mercury ; Diphenylethynylmercury
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new procedure for derivatisation of inorganic mercury(II) to diphenylethynylmercury with simultaneous extraction into dichloromethane is proposed. The organomercury derivative is effectively analysed by HPLC using UV detection. The calibration curve is linear over three orders of magnitude (0.02–50 mg L−1 Hg); the detection limit is 0.1 ng Hg. A preliminary study of the effect of potential interfering agents, in particular Cu(II), Zn(II), Cd(II), Pb(II), and cysteine, and applications of the present methodology to real environmental samples are presented.
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  • 77
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Fluoropyrimidine drugs ; Pharmacokinetics of doxifluridine ; Chemotherapy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A reversed phase high performance liquid chromatographic method has been developed for the simultaneous determination of the pro-drug 5′-deoxy-5-fluorouridine (5′-dFUR), its metabolite 5-fluorouracil (5-FU) and some fluorinated pyrimidines involved in the metabolic activation process of 5-FU. The method has been used to monitor the bioavailability of 5′-dFUR and 5-FU in patients undergoing anticancer chemotherapy. Serum sample treatment involves addition of internal standard (5-bromouracil), protein precipitation with saturated ammonium sulphate solution and liquid-liquid extraction with ethyl acetate-isopropanol (90 ∶ 10 v/v). Urine is simply diluted with mobile phase and injected. The average recovery from serum (at 0.5 μg/mL level) was 95.0%±1.4 for 5′-dFUR and 86.3%±3.5 for 5-FU. A linear response extending over four decades of concentration was observed. Detection limits in the low ng/ mL range were obtained using a 250 μL sample size and a 20 μL injection volume. Within-day and between-day coefficients of variation were below 4 and 10%, respectively.
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  • 78
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Flow injection analysis ; Combined flow injection/HPLC ; Carbamate pesticides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An integrated flow injection (FI)/HPLC system for the total and individual determination of carbamate pesticides (propoxur, carbofuran and carbaryl) is proposed. The determination is based on the alkaline hydrolysis of the analytes and subsequent coupling with diazotized sulphanilic acid to yield the monitored dyes with or without a prior separation step by HPLC in a C18 column. The calibration curves obtained are linear in the μg/ml range and r.s.d. values are between 0.5 and 3.7% in all instances. Injection of the sample into the FI manifold allows the total pesticide content in the sample to be screened. The manifold thus acts as a post-column reactor/detector of the chromatograph for samples with high overall carbamate content, which are also injected into the HPLC instrument. The performance was checked with contaminated water samples.
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  • 79
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; α1 glycoprotein ; Enantioseparation ; β-blocking agents
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The enantioselectivity of the α1 glycoprotein chiral stationary phase, Chiral AGP® has been evaluated for a number of β-blocking agents. A correlation has been found between the retention behaviour on this stationary phase and the hydrophobicity of the compounds. The separation factor α is higher for compounds that are well retained. Retention, and thus α, are also controlled by pH and the percentage of organic modifier in the mobile phase.
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  • 80
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Perfluoroalkylated polymer-gel packings ; Aromatic and fluorine-containing compounds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Porous, perfluoroalkylated polymer-gels for column packings in high-performance liquid chromatography (HPLC) were prepared by suspension polymerization of heptadecafluorodecyl arcylate and ethylene glycol dimethacrylate. The packings showed no abnormal retention for ionic or aromatic compounds, due to the lack of ionic or aromatic groups. In addition, the packings showed no excessive retention for strongly hydrophobic compounds which is often the case with long-chain, alkylated silica gels and polymer gels. This is due to the extremely low surface energy of perfluoroalkyl groups. Therefore, perfluoroalkylated polymer gels enable isocratic HPLC separation of solutes with significantly different hydrophobicity.
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  • 81
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Porous glass ; Surface free energy ; Film pressure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
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  • 82
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    Chromatographia 33 (1992), S. 478-484 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Porous glass adsorbents ; Surface free energy ; Oriented adsorption of hydrocarbons
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The relationship between the specific capacity factor (k/S, where k is the capacity and S is the surface area of the sorbent, in m2) in the liquid chromatography of aromatic hydrocarbons and the adsorption energy (-°GA) has been investigated. The previously published results, based on the calculation of the work of adhesion (WSA) from contact angles, were re-examined and a new hypothesis on interactions at interfaces was employed. Direct proportionality has been found between k/S and-°GA, which allows prediction of the chromatographic behavior of adsorbates on sorbents. The surface free energy components were calculated in order to determine-°GA in terms of the work of adhesion. The dispersion component of the surface free energy of glass was obtained from the adsorption isotherm of n-octane and it was found that the hydrocarbon molecules are adsorbed in an oriented position. The contact angles of liquids on the outer surface of porous solids do not yield reliable values of WSA and of the surface free energy components. A higher intermolecular attraction increases WSA and decreases the contact angle in pores.
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  • 83
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Adenosine and some metabolites ; Extraction from brain tissue ; Quantitative determination
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An analytical procedure has been developed for the assay of adenosine and some metabolites in brain tissue extracts of rats. This paper reports the extraction method, the technique adopted to avoid enzymatic transformations and the chromatographic conditions for the identification and quantitation of these nucleosides and bases. Peaks in the chromatograms of brain tissue extracts were identified by retention times, absorbance ratios of reference compounds and by enzymatic peak-shift.
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  • 84
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    Chromatographia 34 (1992), S. 573-580 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Chemically bonded phases (CBP) ; Surface heterogenity ; Surface purification
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The surface chemistry of eight silica-gels with different siliceous matrix structures have been described. The influence of surface impurities on the chemical modification process (coverage density) with monooctadecylsilane has been studied. The surfaces of the adsorbents, before chemical modification, were cleaned by extraction with 20% HCl. Bare and modified materials were characterized using different physico-chemical methods e.g.: SIMS, CP/MAS NMR, porosimetry, pH measurement, elemental analysis and chromatography (GC & HPLC). The presence of trace amounts of different metallic elements creating new adsorption centers on the surfaces of the packings, have been demonstrated. Moreover, it has been shown that washing of silica gel adsorbents increases the coverage density of alkylsilyl ligands and improves the chromatographic properties of prepared packings.
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  • 85
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Zone-electrophoretic sample treatment ; Basic and acidic compounds ; Biological samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A modified valve arrangement for zone-electrophoretic sample treatment (ZEST)-which is coupled on-line with column liquid chromatography — is used to pretreat biological (plasma) samples. Carry-over of plasma proteins depends on the pH of the electrophoresis buffer. The determination of propranolol, metoprolol, cromolyn and salicylic acid demonstrates that both basic and acidic analytes can be isolated from the plasma matrix with high selectivity. Analogous piperazines, with different protein binding properties, were used to study the influence of protein binding on the recovery. It is shown that high protein can cause a decreased recovery.
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  • 86
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    Chromatographia 34 (1992), S. 597-600 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Oxindole alkaloids ; Uncaria tomentosa
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The main oxindole alkaloids from the root bark ofUncaria tomentosa were separated by reversed phase HPLC with an acetonitrile/methanol/phosphate buffer solvent gradient. UV detection was carried out at 245 nm. The chromatographic parameters for the separation of the alkaloids were optimized by studying the impact of the pH value of the mobile phase and the column temperature on the separation efficiency of the analytical system. The best separation was achieved with a mobile phase pH of 6.6 and a column temperature of 15°C. The method developed is suitable for the qualitative characterisation and quantitative determination of oxindole alkaloids in crudeUncaria tomentosa extracts and phytopharmaceuticals.
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  • 87
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Enantiomers of furprofen ; Human plasma
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A sensitive and stereoselective liquid chromatographic (HPLC) assay for the S and R enantiomers of furprofen in human plasma has been developed. The assay is based on derivatization with S(−)-1-phenylethylamine with formation of two diastereoisomeric derivatives and on their separation and quantitation using HPLC with uv detection. The method is linear from 25 to 600 ng ml−1 of both enantiomers, with a variation coefficient below 10.8%, and a detection limit of 20 ng ml−1. This procedure is suitable for pharmacokinetic studies.
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  • 88
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Micelle-solute association constants ; Polynuclear aromatic hydrocarbons ; Octanol/water partition coefficients
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Sodium dodecyl sulphate, hexadecyltrimethylammonium bromide and polyoxyethylene(23) lauryl ether were investigated as mobile phases in the micellar liquid chromatography of polycyclic aromatic hydrocarbons of environmental concern. A wide range of surfactant concentrations were used and the retention parameters and distribution coefficients calculated. The trends in the retention data for the PAHs are discussed and several conclusions are presented concerning the partition coefficients when these surfactants are present in the mobile phase. Comparisons are made between the structural features of the compounds and their capacity factors, and the octanol/water partition coefficients are correlated with hydrophobicity for the PAHs studied.
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  • 89
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Normal phase separations ; Chloro-substituted polycyclic aromatic hydrocarbons ; Coupled column system ; Environmental samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention behaviour of chloro-substituted PAHs on several commercial normal bonded phase HPLC columns has been investigated. Chloro-substitution was shown to generally decrease the retention on stationary phases like amino-, diol- and nitrophenylpropyl-modified silica. Dimethylaminosilica exhibited more complex retention characteristics towards chloro-substituted PAHs. On this stationary phase, the position of the chlorine substituents on the aromatic solute seemed to be of greater importance for retention than on the amino-, nitro- and diolsilica. For some chloro-PAHs, the retention was shown to increase with the number of chloro-substitutions, probably due to the large affinity of the electron-rich nitrogen in the stationary phase for the electron deficient π-system of the chloro-PAHs. Chloro-substituted PAHs were strongly retarded on the electron donating 2-(1-pyrenyl)-ethylsilica (PYE) stationary phase. However, the molecular shape of the chloro-derivatives had a large influence on retention, which was considerably decreased for some nonplanar chloro-derivatives of chrysene and benz(a)anthracene. A two-dimensional back-flush HPLC method, consisting of a combination of a nitrophenylsilica column and a PYE column of matched lengths, was shown to be useful for clean-up of chloro-substituted PAHs in environmental samples.
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  • 90
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Column switching ; Lidocaine ; Horse urine analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A rapid method is described for the determination of lidocaine and its metabolites in horse urine using a column switching technique and HPLC analysis. This procedure offers a sensitive assay without the need for time consuming extractions.
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  • 91
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    Chromatographia 34 (1992), S. 132-136 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Cysteine, cystine ; Phenylthiocarbamyl derivatives ; Protein hydrolyzates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new approach is described, and a novel explanation presented, for the high performance liquid chromatographic analysis of cystine and cysteine as their phenylthiocarbamyl derivatives. PTC cystine and cysteine have been eluted with the same retention times and molar responses, most probably due to electrophilic attack of phenylisothiocyanate on cystine resulting in the scission of the disulfide bond yielding two moles of cysteine. Further, total PTC cystine and cysteine have been measured both in model solutions and in standard protein hydrolyzates (lysozyme, bovine albumin, ribonuclease) with the same linearity as the other ineteen amino acids. The reproducibility of the measurements, at the 250–750 pmole level, proved to be 4.1% (Relative Standard Deviation %) or less.
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  • 92
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    Chromatographia 34 (1992), S. 155-158 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Retention ; Crown ethers ; Actinomycin D ; Metal cation complexation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Retention of crown ethers in reverse-phase HPLC has been determined by their bonding ability with cations present in the eluent. The dependence of retention of crown ethers on cation concentration exhibits an inflection and makes it possible to calculate stability constant for the crown ether-cation complex. It is shown that in 75% MeOH retention of antitumor antibiotic, actinomycin D, depends on [Na+] and not on [K+] at concentrations of K+ from 5×10−7 to 10−1 mol l−1. Hence, actinomycin D may be classified as an ionophore-antibiotic.
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  • 93
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Phenolic compounds ; Optimisation of isocratic separations ; River water samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Isocratic column liquid chromatographic systems with UV absorbance detection at 280 nm have been developed for the separation of 29 phenolics and related compounds. The selectivity was investigated on silica-, carbon- and polymer-based separation columns for the separation of phenolic type of components. The effects of various acetonitrile/buffer mixtures, and pH of the mobile phase, and their impact on the retention of the phenols was assessed. Tables of retention times on the four columns for the 29 phenols with two different acetonitrile/buffer mixtures, together with the retention times at three pHs from 6.5 to 2.3 with varying levels of organic modifier on the LiChrospher RP 18 column are presented. As an application, the analysis of real river water samples from the Ebro river is described using a solid phase extraction step prior to injection into the chromatographic system.
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  • 94
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    Chromatographia 34 (1992), S. 173-176 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carbon packing materials ; Aromatic compound separation ; Eluent effect
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention volume dependences on the molar volume were found for aromatic compounds using liquid microcolumn chromatography. The contributions of the functional groups in molecules of these compounds to the total retention value were calculated from the capacity factor values. The comparison of capacity factor values for carbon sorbents and octadecyl-silicagel has shown that for several microcolumn separations the carbon sorbent column has a better selectivity and resolution than the octadecyl-silicagel column.
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  • 95
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    Chromatographia 34 (1992), S. 177-181 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Synthesis of bonded stationary phases ; Acceptor ligands ; Normal phases ; PAHs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The synthesis of several electron-acceptor stationary phases has been reviewed the materials evaluated for their capacity to separate polyaromatic hydrocarbons (PAHs). Chemically bonded phases were obtained by the same procedure; the organosilane moiety is monofunctional and the HPLC behaviour is compared under identical conditions. Examples of PAHs separations are given.
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  • 96
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    Chromatographia 34 (1992), S. 182-184 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; C18 bonded phase ; Residual silanol groups ; Metal 5-Br-PADAP complexes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary If any residual (free) silanol groups remain at the surface of silica gel after bonding treatment, they may affect the retention of solutes since the dissociated groups (≡SiO−) will attract cations. The silanol group effect on the retention of cationic solutes will increase with increasing pH of the mobile phase but the effect will decrease with increasing hydrophobic-ion concentration at the C18 surface because such ions can mask the residual silanol groups. A method for the separation of metal complexes with 2-(5-bromo-2-pyridylazo)-diethylaminephenol (5-Br-PADAP) has been developed. The hydrophobic ion in the MeOH/H2O mobile phase was tetrabutylammonium (TBA).
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  • 97
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    Chromatographia 34 (1992), S. 342-346 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; History of chromatography ; Calcium carbonate stationary phase ; Chlorophyll
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Although Michael Tswett is the originator of chromatography, little is known about the performance of his chromatographic systems. His descriptions of the separation of plant pigments are detailed but nevertheless difficult to interprete by today's chromatographic theory. By our own experiments with the system calcium carbonate/benzene it was found that the separation factor of chlorophyll a and b is approx. 1.6 which means that less than 100 theoretical plates are necessary for separation. Tswett's columns with 50 μm particles and 2–3 cm of bed height presumably exceeded this plate number. His separations could have been impaired by mass overload and by a volume flow rate which was two orders of magnitude faster than the optimum.
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  • 98
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Isomeric substituted alkylbenzenes ; Retention and resolution
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The retention data of isomeric xylenes, ethyltoluenes and diethylbenzenes, and of mesitylene, benzene, toluene and ethylbenzene were obtained on a reversedphase column using methanol-water and ethanol-water mobile phases at four different temperatures. This database was used to relate the dependence of solute retention and resolution on the polarity of the mobile phase, solute dipole moment, and column temperature. The additivity of the free energy of the transfer of solute molecules or solute segments from the stationary phase to the mobile phase, was examined for the isomeric compounds. For this, the logarithm of the net retention volume was substituted for the free energy. Deviations from the additivity of free energies indicate that the separation of isomeric substituted alkylbenzenes is governed by their differential interactions with both the polar mobile phase and nonpolar stationary phase. Among the disubstituted alkylbenzenes,ortho-isomers favor the mobile phase more andpara-isomers tend to prefer the stationary phase more. Themeta-isomers are found to follow the additivity rule closely. These trends are amplified as the polarity of the mobile phase is increased indicating that these isomers are resolved better in water-rich mobile phases. These findings are substantiated by analogous results from gas-liquid chromatographic retention data, estimation of dipole moment effects, and examination of the entropic and enthalpic contributions to the net retention volume.
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  • 99
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Column switching ; Polycyclic aromatics ; Oil distillates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A selective and sensitive HPLC method for the determination of Benzo[a]pyrene (B[a]p) in oil fractions by means of column switching is described. The diluted oil samples were injected directly onto a silica column with isooctane as eluent. After fast elution of the main part of the sample matrix, the B[a]p containing fraction was transferred on-line to a dinitro-aryl-modified silica column for final separation with isooctane/tetrahydrofuran. A detection limit of 50 ppt B[a]p was found when using fluorescence detection.
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  • 100
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Precipitation chromatography of polymers ; Block copolymers of styrene-butyl methacrylate ; Association phenomena
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Block copolymers of styrene andt-butyl methacrylate can be analysed by methanol/tetrahydrofuran gradients on C18 or phenyl bonded phase columns. On both of these columns, retention increases with styrene content of the samples. At 50°C, the retention of PS or a block copolymer containing 45% styrene was longer on the phenyl than the C18 columns. This indicates the contribution of adsorption to retention on phenyl bonded phase columns. Lowering the temperature from 50 to 30°C caused earlier elution of part of the sample from the phenyl phase. On a C18 phase the same drop in temperature improved the shape of the peak, which also started later than at 50°C. This effect of temperature is generally observed in polymer retention due to an adsorption mechanism, whereas increasing retention with decrease in temperature is characteristic of a precipitation mechanism. The block copolymer investigated contained 15% free polystyrene precursor which could not be separated from the block copolymer under the conditions employed. The addition of 20% PS homopolymer with a molecular weight similar to that of the styrene block in the copolymer showed that the polystyrene eluted together with the block copolymer, whereas the addition of PS homopolymer with a much higher molecular weight caused an extra peak at the expected elution time.
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