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  • Biochemistry and Biotechnology  (670)
  • Life and Medical Sciences  (629)
  • Analytical Chemistry and Spectroscopy
  • 1995-1999  (1,525)
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  • 1
    Electronic Resource
    Electronic Resource
    New York, NY [u.a.] : Wiley-Blackwell
    Biotechnology and Bioengineering 49 (1996), S. 204-216 
    ISSN: 0006-3592
    Keywords: expanded bed adsorption ; bakers' yeast ; G6PDH ; STREAMLINE ion exchange adsorbents ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The use of expanded beds of STREAMLINE ion exchange adsorbents for the direct extraction of an intracellular enzyme glucose-6-phosphate dehydrogenase (G6PDH) from unclarified yeast cell homogenates has been investigated. It has been demonstrated that such crude feedstocks can be applied to the bed without prior clarification steps. The purification of G6PDH from an unclarified yeast homogenate was chosen as a model system containing the typical features of a direct extraction technique. Optimal conditions for the purification were determined in small scale, packed bed experiments conducted with clarified homogenates. Results from these experiments were used to develop a preparative scale separation of G6PDH in a STREAMLINE 50 EBA apparatus. The use of an on-line rotameter for measuring and controlling the height of the expanded bed when operated in highly turbid feedstocks was demonstrated. STREAMLINE DEAE has been shown to be successful in achieving isolation of G6PDH from an unclarified homogenate with a purification factor of 12 and yield of 98% in a single step process. This ion exchange adsorbent is readily cleaned using simple cleaning-in-place procedures without affecting either adsorption or the bed expansion properties of the adsorbent after many cycles of operation. The ability of combining clarification, capture, and purification in a single step will greatly simplify downstream processing flowsheets and reduce the costs of protein purification. © 1996 John Wiley & Sons, Inc.
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  • 2
    Electronic Resource
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    New York, NY [u.a.] : Wiley-Blackwell
    Biotechnology and Bioengineering 49 (1996), S. 259-265 
    ISSN: 0006-3592
    Keywords: hepatocytes ; lactose-derivatized polystyrene ; polystyrene ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Hepatocytes isolated from male Fisher 344VF rats were cultured on two substrates, collagen I and a lactose-derivatized polystyrene (PS-lactose), to compare morphological and functional differences. Hepatocyte morphology changed dramatically depending upon the substrate, shown through actin cytoskeletal staining and scanning electron microscopy. Functional assays performed included albumin secretion, reduced glutathione content, UDP-glucuronosyl transferase, and cytochrome P4501A1 activity. The presence of dexamethasone and dimethylsulfoxide (DMSO) in the media was required for the maintenance of several differentiated functions for cells cultured on collagen. In general, cells cultured on the PS-lactose substrate showed a much slower loss of function over the same period of time. The maintenance of differentiated function of cells on PS-lactose was enhanced with the addition of dexamethasone and DMSO. This is the first report of a culture system in which hepatocytes, cultured on a polymer substrate without additional protein coatings or media additives, have been able to maintain differentiated functions for up to 1 week. © 1996 John Wiley & Sons, Inc.
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  • 3
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    New York, NY [u.a.] : Wiley-Blackwell
    Biotechnology and Bioengineering 49 (1996), S. 290-299 
    ISSN: 0006-3592
    Keywords: proteins, modified ; partitioning in aqueous system ; thaumatin ; β-lactoglobulin ; BSA ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Relatively conservative modifications of three proteins were carried out to alter their surface properties. The protein properties modified were hydrophobicity and charge. This was done by acylation of amino groups with anhydrides. For the hydrophobic modification experiments, two proteins (β-lactoglobulin and bovine serum albumin [BSA]) and four anhydrides (hexanoic, butyric, succinic, acetic) were used. For the modification of surface charge the protein thaumatin was selected and various proportions of the free amino groups were blocked with acetic anhydride to give a series of proteins with differing isoelectric points. Detailed characterization and purification of selected modified proteins was carried out including molecular weight measurements and conformational analysis. The criteria used for selecting the modified proteins for subsequent investigation of their partitioning in aqueous two-phase systems (ATPS) is described. With a judicious choice of starting material it was found that limited chemical modifications to proteins could effectively alter surface hydrophobicity or charge almost independently, with little effect on other molecular properties. It appears, however, that the method for chemical modification and the reaction conditions must also be carefully controlled. © 1996 John Wiley & Sons, Inc.
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  • 4
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    New York, NY [u.a.] : Wiley-Blackwell
    Biotechnology and Bioengineering 49 (1996), S. 309-315 
    ISSN: 0006-3592
    Keywords: surface charge ; proteins, modified ; partitioning in aqueous system ; thaumatin ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A series of charge-modified thaumatins with different values of surface charge were partitioned in aqueous two-phase systems (ATPS) to study the effect of surface charge as a single property on partitioning. Electrophoretic mobility of the proteins in titration curves was used as a measure of surface charge. Four modified proteins derived from thaumatin with the following values of isoelectric point: 8.70, 8.15, 5.60, and 4.50 were used for partitioning. The resolution of the systems in terms of protein surface charge was calculated. Partitioning of modified thaumatins in PEG 4000/dextran systems with phosphate buffer, Tris buffer, NaCl, KCl, and sulfate salts was carried out. Among the sulfate salts tested, the addition of 50 mM Li2SO4 to the system buffered with phosphate gave the highest value of resolution for differences in surface protein charge (RSPC). It shows a decrease in the value of K (partition coefficient) with an increase in the protein's charge. The addition of 100 mM KCl to the system promoted the opposite effect on the RSPC value. Charge-modified proteins were partitioned in PEG/salt systems to investigate the ability of these systems for resolving differences in surface charge. The PEG/citrate system seemed to have almost no ability for resolving proteins on the basis of surface charge differences; PEG/phosphate systems had some capability for resolving differently charged proteins. The more negative proteins tended to have higher values of K than the more positively charged fractions. The use of charge-modified proteins allowed the investigation of the effect of protein surface charge on partitioning in aqueous two-phase systems independently from other protein parameters as they were prepared from a common parent protein thaumatin. This technique provides an interesting novel tool to investigate the effect of protein surface charge on partitioning in ATPS taking protein charge as an independent parameter. © 1996 John Wiley & Sons, Inc.
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  • 5
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    New York, NY [u.a.] : Wiley-Blackwell
    Biotechnology and Bioengineering 49 (1996), S. 348-354 
    ISSN: 0006-3592
    Keywords: oxygenator ; NMR spectroscopy ; organ perfusion ; mammalian cell culture ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A compact, reusable membrane oxygenator has been constructed for the perfusion of cultured cells and isolated organs. While the oxygenator was designed to be compatible with nuclear magnetic resonance (NMR) spectroscopy studies, it can also be used for any experiment which requires warming and oxygenation of perfusates. For the NMR studies, the oxygenator can be positioned at the opening of the magnet bore which allows oxygenation and warming of the perfusate immediately prior to delivery to the tissue, therefore eliminating problems with heat or oxygen loss which may occur with the long perfusion lines. © 1996 John Wiley & Sons, Inc.
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  • 6
    ISSN: 0006-3592
    Keywords: c-fos protein ; endothelium ; hemodynamics ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The c-fos protein belongs to a family of transcriptional cofactors that can complex with proteins of the Jun family and activate mRNA transcription from gene promoters containing an activator protein 1 (AP-1) binding element. The shear stress inducibility of the c-fos protein was studied in human and animal cell lines of vastly different origins. Primary human umbilical vein endothelial cells (HUVEC), bovine aortic endothelial cells (BAEC, passage 2-14), HeLa cells, and Chinese hamster ovary (CHO) cells were subjected to steady laminar shear stress using a parallel plate flow apparatus. After 1 h of flow exposure at 25 dyn/cm2, the c-fos levels in nuclei of shear stress HUVEC, BAEC, HeLa, and CHO were 5.4 ± 2.0 (n = 3), 2.25 ± 1.38 (n = 6), 2.14 ± 0.07 (n = 8), 1.92 ± 0.58 (n = 2) times higher, respectively, than in matched stationary controls. Flow exposure at 4 dyn/cm2 caused no enhancement of c-fos levels in any of the cell lines tested, but caused significant reduction in c-fos expression in the HeLa cells. The c-fos induction by shear stress could be blocked by pharmacological agents. For example, the flow induction of the c-fos protein levels was blocked by 50% with the preincubation of HUVEC with a protein kinase C inhibitor, H7 (10 μM) and blocked completely in HeLa cells preincubated with the phospholipase C inhibitor, neomycin (5 mM). The minimum time of shear stress exposure required to induce the c-fos protein expression in HeLa cells was found to be as low as 1 min. By Northern analysis, the c-fos mRNA levels were found to be elevated in BAEC, CHO, and HeLa cells exposed to 25 dyn/cm2 for 30 min. These studies indicate that c-fos induction is a consistent genetic response in a variety of mammalian cells that may alter cellular phenotype in mechanical environments. © 1996 John Wiley & Sons, Inc.
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  • 7
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    New York, NY [u.a.] : Wiley-Blackwell
    Biotechnology and Bioengineering 49 (1996), S. 412-420 
    ISSN: 0006-3592
    Keywords: Amycolatopsis orientalis ; vancomycin production ; chemostat culture ; phosphate inhibition ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Production of the glycopeptide antibiotic vancomycin by two Amycolatopsis orientalis strains was examined in batch shake flask culture in a semidefined medium with peptone as the nitrogen source. Different growth and production profiles were observed with the two strains; specific production (Yp/x) was threefold higher with strain ATCC 19795 than with strain NCIMB 12945. A defined medium with amino acids as the nitrogen source was developed by use of the Plackett-Burman statistical screening method. This technique identified certain amino acids (glycine, phenylalanine, tyrosine, and arginine) that gave significant increased specific production, whereas phosphate was identified as inhibitory for high specific vancomycin production. Experiments made with the improved medium and strain ATCC 19795 showed that vancomycin production kinetics were either growth dissociated or growth associated, depending on the amino acid concentration. In chemostat culture at a constant dilution rate (0.087 h-1), specific vancomycin production rate (qvancomycin) decreased linearly as the medium phosphate concentration was increased from 2 to 8 mM. In both phosphate and glucose limited chemostats, qvancomycin was a function of specific growth rate; the maximum value was observed at D = 0.087 h-1 (52% of the maximum specific growth rate). Under phosphate limited growth conditions, qvancomycin was threefold higher (0.37 mg/g dry weight/h) than under glucose limitation (0.12 mg/g dry weight/h). © 1996 John Wiley & Sons, Inc.
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  • 8
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    Biotechnology and Bioengineering 50 (1996), S. 36-48 
    ISSN: 0006-3592
    Keywords: insect cell culture ; Sf-9 cells ; respiration ; bioreactor ; on-line monitoring ; baculovirus expression vector system ; recombinant proteins ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Respiration rates in Spodoptera frugiperda (Sf-9) cell bioreactor cultures were successfully measured on-line using two methods: The O2 uptake rate (OUR) was determined using gas phase pO2 values imposed by a dissolved oxygen controller and the CO2 evolution rate (CER) was measured using an infrared detector. The measurement methods were accurate, reliable, and relatively inexpensive. The CER was routinely determined in bioreactor cultures used for the production of several recombinant proteins. Simple linear relationships between viable cell densities and both OUR and CER in exponentially growing cultures were used to predict viable cell density. Respiration measurements were also used to follow the progress of baculoviral infections in Sf-9 cultures. Infection led to increases in volumetric and per-cell respiration rates. The relationships between respiration and several other culture parameters, including viable cell density, cell protein, cell volume, glucose consumption, lactate production, viral titer, and recombinant β-galactosidase accumulation, were examined. The extent of the increase in CER following infection and the time postinfection at which maximum CER was attained were negatively correlated with the multiplicity of infection (MOI) at multiplicities below the level required to infect all the cells in a culture. Delays in the respiration peak related to the MOI employed were correlated with delays in the peak in recombinant protein accumulation. DO levels in the range 5-100% did not exert any major effects on viable cell densities, CER, or product titer in cultures infected with a baculovirus expressing recombinant β-galactosidase. © 1996 John Wiley & Sons, Inc.
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  • 9
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    New York, NY [u.a.] : Wiley-Blackwell
    Biotechnology and Bioengineering 50 (1996) 
    ISSN: 0006-3592
    Keywords: Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
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  • 10
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    Biotechnology and Bioengineering 50 (1996), S. 169-183 
    ISSN: 0006-3592
    Keywords: liposomes ; biotin ; aggregation kinetics ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The aggregation of biotinylated phospholipid vesicles (liposomes) cross-linked by antibiotin IgG was studied experimentally and theoretically. The liposomes were either low density liposomes that contained 0.4 mol% biotinylated phospholipid (≈100 exposed biotin molecules per liposome), or high density liposomes that contained 2.7 mol% biotinylated phospholipid (≈1000 exposed biotin molecules per liposome). The solution turbidity and mean particle size measured by quasi-elastic light scattering (QLS) were monitored throughout the aggregation. Three different lots of antibiotin antibodies, each with different association constants and binding heterogeneities, were used. The antibody binding characteristics affected the aggregation rates. The aggregation kinetics were analyzed using a model based on the Smoluchowski theory of aggregation, fractal concepts of aggregate microstructure, and Rayleigh and Mie light scattering theory. The experimental conditions of liposome concentration, protein concentration, and ligand density under which aggregation occurred correlated well with calculated sticking probabilities based on isotherms describing the adsorption of antibiotin antibody to the liposomes. These results are compared with prior observations made when avidin was used as the cross-linking protein. © 1996 John Wiley & Sons, Inc.
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  • 11
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    New York, NY [u.a.] : Wiley-Blackwell
    Biotechnology and Bioengineering 50 (1996) 
    ISSN: 0006-3592
    Keywords: Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
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  • 12
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    New York, NY [u.a.] : Wiley-Blackwell
    Biotechnology and Bioengineering 50 (1996), S. 211-216 
    ISSN: 0006-3592
    Keywords: microgravity ; bioprocessing ; sedimentation ; turbulence ; collagenase ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The effect of a quiescent microgravity fluid environment on the activity of collagenase directed at demineralized bone fragments was investigated over a period of 10 days. Enzyme treatment resulted in greater mass loss in microgravity, with nearly three times the loss of mass during Space Shuttle mission STS-62 compared to the stationary ground control. Clinorotation enhanced the loss of mass relative to a stationary control, but this increase was still significantly less than the increase with exposure to microgravity. This suggests the detrimental influence of turbulence on the enzyme function and the benefit of using microgravity to provide both low turbulence and uniformity of unequally dense materials within the reaction chamber. The results are considered for their general applicability to a variety of bioprocessing applications that may be enhanced in microgravity. © 1996 John Wiley & Sons, Inc.
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  • 13
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    Biotechnology and Bioengineering 50 (1996), S. 430-437 
    ISSN: 0006-3592
    Keywords: cartilage ; tissue regeneration ; chondrocytes ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: In the last 5 to 10 years, tissue engineering has revolutionized the way in which medical researchers and clinicians are thinking of and, in some cases, actually treating diseases involving tissue damage and destruction. One such disease, osteoarthritis, results from progressive degeneration of articular cartilage, which has a limited ability to repair itself. With tissue engineering, scientists are now able to regenerate cartilage in vitro from isolated mature chondrocytes. While the regeneration process is still not fully understood, enough has been learned that physicians are already implanting cultured chondrocytes into humans and other animals in the hopes of effecting joint repair. One aspect which has not been fully explored is the effect of mechanical stress on developing and implanted cartilage, especially over the long term. This article will review in brief what is now known about the mechanical factors affecting cartilage regeneration in vitro and what still remains to be determined for optimum tissue engineering of cartilage constructs. © 1996 John Wiley & Sons, Inc.
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  • 14
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    Biotechnology and Bioengineering 50 (1996), S. 443-451 
    ISSN: 0006-3592
    Keywords: osteoblast ; migration ; poly(αhydroxy esters) ; poly(DL-lactic-co-glycolic acid) ; PLGA ; biodegradable polymers ; tissue engineering ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: We investigated the migration of rat calvaria osteoblast populations on poly(α-hydroxy ester) films for up to 14 days to determine effects of substrate composition and culture conditions on the migratory characteristics of osteoblasts. Initial osteoblast culture conditions included cell colonies formed by seeding a high (84,000 cells/cm2) or low (42,000 cells/cm2) density of isolated osteoblasts on the polymer films, and bone tissue cultures formed by plating bone chips directly on the substrates. High density osteoblast colonies cultured and allowed to migrate and proliferate radially on 85:15 poly(DL-lactic-co-glycolic acid) (PLGA) films, 75:25 PLGA films, and tissue culture polystyrene controls demonstrated that the copolymer ratio in the polymer films did not affect the rate of increase in substrate surface area (or culture area) covered by the growing cell colony. However, the rate of increase in culture area was dependent on the initial osteoblast seeding density. Initial cell colonies formed with a lower osteoblast seeding density on 75:25 PLGA resulted in a lower rate of increase in culture area, specifically 4.9 ± 0.3 mm2/day, versus 14.1 ± 0.7 mm2/day for colonies seeded with a higher density of cells on the same polymer films. The proliferation rate for osteoblasts in the high and low density seeded osteoblast colonies did not differ, whereas the proliferation rate for the osteoblasts arising from the bone chips was lower than either of these isolated cell colonies. Confocal and light microscopy revealed that the osteoblast migration occurred as a monolayer of individual osteoblasts and not a calcified tissue front. These results demonstrated that cell seeding conditions strongly affect the rates of osteoblast migration and proliferation on biodegradable poly(α-hydroxy esters). © 1996 John Wiley & Sons, Inc.
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  • 15
    ISSN: 0006-3592
    Keywords: bone marrow ; hematopoiesis ; perfusion ; culture optimization ; stroma ; stem cells ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Hematopoiesis, the formation of mature blood cells from stem (LTC-IC) and progenitor (CFU-GM) cells in the bone marrow, is a complex tissue-forming process that leads to many important physiological functionalities. Consequently, a functioning ex vivo hematopoietic system has a variety of basic scientific and clinical uses. The design and operation of such a system presents the tissue engineer with challenges and choices. In this study, three culture variables were used to control ex vivo human hematopoiesis. Systematic variation of inoculum density (ID), medium exchange interval (MEI), and the use of preformed stroma (PFS) showed that (1) all three variables significantly influenced culture performance, (2) the three variables interacted strongly, and (3) the variables could be manipulated to achieve the optimization of different performance criteria. Donor-to-donor variability in culture performance was great at low ID but was minimized at higher ID. PFS had a large positive effect on cell and CFU-GM output at low ID, but had minimal effect at higher ID. In fact, PFS caused a decrease in LTC-IC output at high ID. The effects of PFS indicated that stromal cell elements became more limiting than proliferative cell elements as ID was reduced.In cultures without PFS, maximum cell output was obtained with high ID using a short MEI, whereas the greatest cell expansion ratio was obtained at low ID with an intermediate MEI. Maximum CFU-GM output was obtained from cultures with high ID using a short to intermediate MEI, whereas the greatest CFU-GM expansion ratio was obtained at intermediate ID with an intermediate MEI. The addition of PFS altered the locations of these maxima. In general, PFS moved the maxima to lower ID, and culture output became more sensitive to MEI. Therefore, the optimization of one performance criterion always resulted in a decline of the others. This study demonstrates that ex vivo tissue function is sensitive to many culture variables in an interactive fashion and that systematic multivariable studies are required to characterize tissue function. Once the effects of individual variables and their interactions are known, this knowledge can be used to optimize tissue performance with respect to desired criteria. © 1996 John Wiley & Sons, Inc.
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  • 16
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    Biotechnology and Bioengineering 50 (1996) 
    ISSN: 0006-3592
    Keywords: Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
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  • 17
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    Biotechnology and Bioengineering 51 (1996), S. 410-421 
    ISSN: 0006-3592
    Keywords: lysozyme ; thermal stability ; 1H NMR ; conformational flexibility ; melting temperature ; PEG ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The reversible folding destabilization of hen lysozyme has been confirmed by a melting temperature (Tm) decrease in aqueous poly(ethylene glycol) (PEG). The percent denatured, extracted from the histidine 15 C2H (H15 C2H) native and denatured peak areas from 500-MHz one-dimensional proton nuclear magnetic resonance (1D 1H NMR) spectra in D2O, was analyzed through denaturation temperatures at 0% and 20% (w/w) PEG 1000. The lysozyme (3.5 mM) Tm decreased by 4.2°C and 7.1°C in 20% (w/w) PEG 1000 at pH 3.8 and 3.0, respectively. The Tm decreased with increasing lysozyme concentration. Additionally, the temperature-induced resonance migrations of 17 protons from 8 residues indicate that the native lysozyme structure undergoes temperature-induced conformational changes. The changes were essentially identical in both 0% and 20% (w/w) PEG 1000 at both pH 3.0 and 3.8. This small, local restructuring of the hydrophobic box region may be a manifestation of temperature-dependent solution hydrophobicity, whereas active-site cleft fluctuations may be due to the inherent active-site flexibility. The lysozyme structure in PEG at 35°C was determined to be essentially native from the 1H nuclear Overhauser effect spectroscopy (NOESY) fingerprint regions. Additionally, lysozyme chemical shifts, from 1D spectra, in PEG 200, 300, and 1000 at 35°C and various concentrations were essentially identical, further confirming that the conformation remains native in various PEG solutions. © 1996 John Wiley & Sons, Inc.
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  • 18
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    Biotechnology and Bioengineering 51 (1996), S. 375-383 
    ISSN: 0006-3592
    Keywords: cellulase ; enzyme recycling ; enzyme adsorption ; lignocellulosic hydrolysis ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Past technoeconomic modeling work has identified the relatively large contribution that enzymatic hydrolysis adds to the total cost of producing ethanol from lignocellulosic substrates. This cost was primarily due to the high concentration of enzyme and long incubation time that was required to obtain complete hydrolysis. Although enzyme and substrate concentration and end-product inhibition influenced the rate of hydrolysis, the effect was less pronounced during the initial stages of hydrolysis. During this time most of the cellulases were adsorbed onto the unhydrolyzed residue. By recycling the cellulases adsorbed to the residual substrate remaining after an initial 24 h, a high rate of hydrolysis, with low overall residence time and minimal cellulase input, could be achieved for several rounds of enzyme recycle. A comparison of the front end (pretreatment, fractionation, and hydrolysis) of a softwood/hardwood to ethanol process indicated that the lignin associated with the softwood-derived cellulose stream limited the number of times the cellulose containing residue could be recycled. © 1996 John Wiley & Sons, Inc.
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  • 19
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    Biotechnology and Bioengineering 51 (1996), S. 399-409 
    ISSN: 0006-3592
    Keywords: cell damage ; cell culture ; bubble aeration ; agitation ; bubble coalescence and breakup ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: It has been established that the forces resulting from bubbles rupturing at the free air (gas)/liquid surface injure animal cells in agitated and/or sparged bioreactors. Although it has been suggested that bubble coalescence and breakup within agitated and sparged bioreactors (i.e., away from the free liquid surface) can be a source of cell injury as well, the evidence has been indirect. We have carried out experiments to examine this issue. The free air/liquid surface in a sparged and agitated bioractor was eliminated by completely filling the 2-L reactor and allowing sparged bubbles to escape through an outlet tube. Two identical bioreactors were run in parallel to make comparisons between cultures that were oxygenated via direct air sparging and the control culture in which silicone tubing was used for bubble-free oxygenation. Thus, cell damage from cell-to-bubble interactions due to processes (bubble coalescence and breakup) occurring in the bulk liquid could be isolated by eliminating damage due to bubbles rupturing at the free air/liquid surface of the bioreactor. We found that Chinese hamster ovary (CHO) cells grown in medium that does not contain shear-protecting additives can be agitated at rates up to 600 rpm without being damaged extensively by cell-to bubble interactions in the bulk of the bioreactor. We verified this using both batch and high-density perfusion cultures. We tested two impeller designs (pitched blade and Rushton) and found them not to affect cell damage under similar operational conditions. Sparger location (above vs. below the impeller) had no effect on cell damage at higher agitation rates but may affect the injury process at lower agitation intensities (here, below 250 rpm). In the absence of a headspace, we found less cell damage at higher agitation intensities (400 and 600 rpm), and we suggest that this nonintuitive finding derives from the important effect of bubble size and foam stability on the cell damage process. © 1996 John Wiley & Sons, Inc.
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  • 20
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    Biotechnology and Bioengineering 51 (1996), S. 434-438 
    ISSN: 0006-3592
    Keywords: polyphosphate ; Escherichia coli ; phosphate starvation ; gene expression ; heterologous ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The effect of intracellular polyphosphate on the phosphate-starvation response in Escherichia coli was studied by genetically manipulating the intracellular polyphosphate levels and by performing phosphate shifts on the genetically engineered strains. Strains that produced large quantities of polyphosphate and were able to degrade it induced the phosphate-starvation response to a lesser extent than wild-type strains, whereas strains that were unable to degrade a large intracellular polyphosphate pool induced the phosphate-starvation response to a greater extent than wild-type strains. These results have important implications for expression of heterologous genes under control of the phoA promoter. © 1996 John Wiley & Sons, Inc.
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  • 21
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    Biotechnology and Bioengineering 51 (1996), S. 458-465 
    ISSN: 0006-3592
    Keywords: concentric-cylinder shear device ; rotor/stator homogenization ; shear ; shear rate ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Shear is present in almost all bioprocesses and high shear is associated with processes involving agitation and emulsification. The purpose of this study is to investigate the effect of high shear and high shear rate on proteins. Two concentric cylinder-based shear systems were used. One was a closed concentric-cylinder shear device (CCSD) and the other was a homogenizer with a rotor/stator assembly. Mathematical modeling of these systems allowed calculation of the shear rate and shear. The CCSD generated low shear rates (a few hundred s-1), whereas the homogenizer could generate very high shear rates (〉 105 s-1). High shear could be achieved in both systems by increasing the processing time. Recombinant human growth hormone (rhGH) and recombinant human deoxyribonuclease (rhDNase) were used as the model proteins in this study. It was found that neither high shear nor high shear rate had a significant effect on protein aggregation. However, a lower melting temperature and enthalpy were detected for highly sheared rhGH by using scanning microcalorimetry, presumably due to some changes in protein's conformation. Also, SDS-PAGE indicated the presence of low molecular-weight fragments, suggesting that peptide bond breakage occurred due to high shear. rhDNase was relatively more stable than rhGH under high shear. No conformational changes and protein fragments were observed. © 1996 John Wiley & Sons, Inc.
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  • 22
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    Biotechnology and Bioengineering 51 (1996), S. 494-499 
    ISSN: 0006-3592
    Keywords: cell metabolism ; baculovirus ; insect cells ; recombinant protein OSF-2 ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The properties of Sf9 and Tn5 insect cells were analyzed comparatively under serum-free culture conditions. Sf9 cells in SF900II medium apparently utilized sucrose as a primary nutrient both before and after virus infection, yielding small amounts of lactate and ammonia. Tn5 cells in Excell 401 medium consumed all the nutrients examined, including sucrose. The productivity of a recombinant glycoprotein, OSF-2, by Tn5 cells, was moderate in both monolayer and spinner cultures, but the ability to secrete it was compromised in the former case. Relative to the Tn5 cultures, Sf9 produced 30-fold more OSF-2 in either culture mode. © 1996 John Wiley & Sons, Inc.
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  • 23
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    Biotechnology and Bioengineering 51 (1996), S. 538-543 
    ISSN: 0006-3592
    Keywords: NMR imaging ; biosorption ; alginate ; shrinking core model ; Laminaria ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: In this contribution, an NMR imaging study of heavy metal absorption in alginate, immobilized-cell biosorbents, and kombu (Laminaria japonica) algal biomass is presented. This method provides the good possibility of directly monitoring the time evolution of the spatial distribution of the ions in the materials. From these results, we demonstrate that rare earth ions are absorbed with a steep reaction front that can be described very well with a modified shrinking core model, while copper ions are absorbed with a more diffuse front.
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  • 24
    ISSN: 0006-3592
    Keywords: oxidoreductase ; chiral alcohol ; racemic resolution ; membrane reactor ; continuous extraction ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Oxidations of alcohols by alcohol dehydrogenases often suffer from low conversions and slow reaction rates due to severe product inhibition. This can be overcome by continuous product extraction, because only the concentrations, but not the kinetic parameters, can be changed. As a consequence, it is favorable to apply a differential circulation reactor with continuous product extraction, where only a small amount of product is formed per cycle. The product is then directly extracted using a microporous hydrophobic hollow fiber membrane. This results in an increase of the relative activity of the dehydrogenase at a given conversion. The reaction investigated is the kinetic resolution of racemic 1-phenyl-1,2-ethanediol by glycerol dehydrogenase (GDH). The resulting oxidation product, 2-hydroxyacetophenone, causes a strong product inhibition. Additionally, it reacts in a chemical reaction with the cofactor lowering its active concentration. Because the GDH needs β-nicotinamide adenine dinucleotide (NAD+) as a cofactor, lactate dehydrogenase is used to regenerate NAD+ from NADH by reducing pyruvate to (L)-lactate. A conversion of 50% with respect to the racemate and an enantiomeric excess 〉99% of the (S)-enantiomer was reached.
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  • 25
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    Biotechnology and Bioengineering 51 (1996), S. 581-590 
    ISSN: 0006-3592
    Keywords: microfiber ; graft polymerization ; DNA immobilization ; immunoadsorbent ; DNA ; anti-DNA antibody ; systemic lupus erythematosus ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Immobilization of DNA to the surface of poly(ethylene terephthalate) (PET) microfibers with a high specific surface area of 0.83 m2/g was carried out to give the fiber surface an affinity for anti-DNA antibody. Following ozone oxidation, the microfibers were subjected to graft polymerization of monomers including acrylic acid, methacryloyloxyethyl phosphate, N,N-dimethylaminoethyl methacrylate, N-vinylformamide, and glycidyl methacrylate. Calf thymus DNA was immobilized to the grafted fiber surface through either covalent binding or polyion complexation with the grafted polymer chains. The highest surface density of DNA immobilized (0.6 μg/cm2) was obtained when DNA was immobilized through formation of phosphodiester linkage between the hydroxyl group of DNA and the phosphate group in grafted poly(methacryloyloxyethyl phosphate) using 1,1-carbonyldiimidazole, or through polyion complexation between the anionic DNA and the cationic grafted poly(N,N-dimethylaminoethyl methacrylate) chains. Batch adsorption of anti-DNA antibody to the grafted PET fibers with and without DNA immobilized on their surface was conducted with serum obtained from systemic lupus erythematosus model mice. The DNA-immobilized PET fibers exhibited a higher adsorption capacity and specificity than the others. In addition, the DNA-immobilized fibers effectively adsorbed human anti-DNA antibody.
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  • 26
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    Journal of High Resolution Chromatography 19 (1996), S. 111-116 
    ISSN: 0935-6304
    Keywords: Polynuclear aromatic hydrocarbons ; Liquid chromatography ; Alcohols ; Micelles ; Enviromental samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method for the separation of polycyclic aromatic hydrocarbons (PAHs) by high-performance liquid chromatography using a hybrid micellar mobile phase is described. The detection of PAHs was carried out using the fluorescence method with programmable excitation and emission wavelength. The method is applied to the analysis of several environmental samples (sea water, sediments, limpets, sea worms) and several of these compounds are quantitated at concentration below 70 ng L-1(kg-1) in the original samples.
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  • 27
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    Journal of High Resolution Chromatography 19 (1996), S. 99-104 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Micellear electrokinetic chromatography ; Organic modifiers ; Naphthalene sulfonates ; Surface water ; Thermostatting ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The production and use of naphthalene sulfonates can easily cause pollution of surface and other types of waters. In the present study, capillary electrophoresis in combination with UV absorption detection was used to separate 21 amino- and hydroxy-substituted naphthalene sulfonates which included multiple isomeric compounds. The influence of various parameters such as pH (which turned out to be extremely important), temperature of the surrounding air flow, and the use of buffer additives (micelles, cyclodextrins, organic modifiers) was studied. Complete separation of all analytes including the isomers, was achieved in two runs with a 50 mM boric acid/borate buffer, containing either 100 mM sodium dodecylsulfonate or 15% acetonitrile. The limits of detection obtained for the individual compounds typically were 20μgI-1. River water samples spiked at this concentration level could be analysed using a simple three-step sample clean-up procedure.
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  • 28
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    Journal of High Resolution Chromatography 19 (1996), S. 403-408 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Cryogenic trapping ; Capillary ; Focusing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cryogenic trapping of solutes leads to narrowing of the chromatographic band. By placing the trap at the end of a capillary column, it is possible to study the effectiveness of the trap in terms of producing a sharpened elution profile. The trap may be heated by supplementary heating, but here convective heating from the GC oven is employed simply by turning off the cryogenic coolant. It is estimated that it takes about 50 s for the trap to heat up sufficiently to allow trapped solute to be remobilized, although this depends upon the oven temperature and thermal mass of the trap. It can also be shown that the more volatile solutes mobilize faster from the trap in this particular mode of operation. The recovery of trapped components shows that there is essentially quantitative trapping, and the solutes are trapped just at the leading edge of the trap.
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  • 29
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    Journal of High Resolution Chromatography 19 (1996), S. 409-412 
    ISSN: 0935-6304
    Keywords: Micellar electrokinetic chromatography ; Rhei Rhizoma ; Scutellariae Radix ; Coptidis Rhizoma ; Bioactive constituents determination ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A capillary electrophoretic method for simultaneous determination of six bioactive ingredients (berberine, palmatine, baicalin, sennoside B, emodin, and sennoside A) in the Chinse herbal formula San-huang-hsieh-hsin-tang was established. A carrier composed of aqueous buffer solution (50 mM sodium cholate, 15 mM sodium dihydrogen phosphate, and 4.25 mM sodium borate)-acetonitrile (3:2) was found to be the most suitable electrolyte for this separation. Contents of these constituents in a non-pretreated methanol-water extract of San-huang-hsieh-hsin-tang sample could be easily determined within 20 min. The effects of borate, cholate, and organic modifier (acetonitrile) concentration of the carrier on the migration behavior of the solutes were also studied.
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    Journal of High Resolution Chromatography 19 (1996), S. 418-418 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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  • 31
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    Journal of High Resolution Chromatography 19 (1996), S. 485-491 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Qualitative analysis ; Quantitative analysis ; Retention indices ; Retention times ; Solvent effect ; Sulfur Chemiluminescence Detection (SCD) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Gas chromatrography (GC) with sulfur chemiluminescence detection (SCD) is an outstanding combination for selectively determining trace concentrations of sulfur compounds in hydrocarbon samples. GC peaks can be identified by retention times when reproducible, automated injection techniques are used. However, as described in this work, analysts should be on the look out for retention shifting due to solvent effects from sample components. Three examples of retention shifting are presented: (1) thiophene by benzene; (2) methylthiophenes by toluene; and (3) dibenzothiophene by gas oil. Depending on samples and analysis conditions, retention shifts from a few hundredths to 1.5 min have been observed. Such retention shifts are likely to cause errors in peak identifications. Therefore, when using SCD, simultaneous FID monitoring is recommended as an aid in evaluating chromatograms for possible retention shifting due to solvent effects.
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    Journal of High Resolution Chromatography 19 (1996), S. 497-502 
    ISSN: 0935-6304
    Keywords: α-Monoacetotriacylglycerides ; Celastraceae ; Fatty acids ; GLC ; GLC-(NCI)MS ; Maytenus seed oils ; OV-225-OH, OH-terminated ; SOP-50, methoxy-terminated ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The seed oils of three Maytenus species have been examined by high temperature GLC using SOP-50 (methoxy-terminated) and OV-225-OH (OH-terminated) glasscapillary columns. The main compounds (71-76%) could be identified as α-mono-acetotriacylglycerols by a combination of high temperature GLC-MS in negative chemical ionization mode with a CH4/N2O mixture as reactant gas and other spectroscopical methods (infrared, 1H- and 13C-nuclear magnetic resonance spectroscopy). The OV-225-OH phase demonstrated better separation properties that the SOP-50 phase for this substance class and up to eight species of α-monoacetotriacylglycerols could be separated. The content of usual triacyclglycerols was below 1%. The results of the analysis of the individual fatty acids as their methyl esters by GC and GC-MS are also presented.
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    Journal of High Resolution Chromatography 19 (1996), S. 521-526 
    ISSN: 0935-6304
    Keywords: LSS model ; Whey proteins ; HIC of proteins ; Circular dichroism ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 19 (1996), S. 527-529 
    ISSN: 0935-6304
    Keywords: High pressure gas chromatography ; Stationary phases ; Hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 19 (1996) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
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  • 36
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Enantiomeric separations ; Acidic compounds ; Neutral β-cyclodextrins ; Sulfobutyl ether β-cyclodextrin ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High resolution could be achieved for the enantiomers of acidic drugs, namely, sulindac, fenoprofen, ketoprofen, warfarin, and hexobarbital, in a buffer of pH 3 by the simultaneous addition of uncharged and charged β-cyclodextrin derivatives. The interaction of the analytes with the anionic sulfobutyl ether β-cyclodextrin provides the analytes with an adequate electrophoretic mobility whereas the interaction with various neutral β-cyclodextrins generates high enantioselectivity. Five neutral cyclodextrins, the native β-cyclodextrin, as well as methyl-, dimethyl-, trimethyl- and hydroxypropyl-β-cyclodextrin, were tested to enhance the enantioselectivity of the electrophoretic system. High resolution values and the shortest analysis times for the five drugs tested were achieved in a buffer made of 100 mM phosphoric acid adjusted to pH 3 with triethanolamine and containing dimethyl- or trimethyl-β-cyclodextrin in addition to sulfobutyl ether β-cyclodextrin.
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  • 37
    ISSN: 0935-6304
    Keywords: Chlorobiphenyl congeners ; Aroclors ; DB-XLB phase ; HP-5/HT-5 serial coupled phases ; GC-ECD ; GC-MS-SIM ; GC-Ion Trap MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Three HRGC systems (1: 30m DB-XLB capillary with MS-SIM detection; 2: 60m DB-XLB capillary with full-scan, ion-trap MS detection; and 3: Parallel dual-column DB-17 and series-coupled HP5/HT5 with ECD detection) were used to completely characterize multiple lots of 8 different-numbered Aroclor mixtures by quantitative calibration against 9 solutions containing primary standards of all 209 PCB congeners. Despite lower absolute sensitivity and more Aroclor congener coelutions than the dual-column ECD system, the MS systems enabled measurement of more congeners per Aroclor since their greater linear response range did not require dilution of samples and standards. Pairs of different lots of Aroclors 1248 and 1254 displayed markedly different proportions of congeners, and the 1254 pair displayed strong differences in the extent of ortho-chlorine substitution. The tables of congener weight percent distributions among Aroclors are more comprehensive and quantitatively precise than those of prior publications. However, the limitations of single-level calibration precluded measurement of all congeners to the ±10% accuracy desirable for establishing these Aroclors as secondary standards for comprehensive, quantitative congener-specific PCB analysis.
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  • 38
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Mass spectrometry ; Electrospray ionization ; Fourier transform ion cyclotron ; Resonance ; Biomolecule analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: We describe the current state of the on-line combination of capillary electrophoresis (CE) electrospray ionization (ESI) Fourier transform ion cyclotron resonance (FTICR) mass spectrometry (MS), and discuss aspects of the FTICR technique relevant to its use as a detection scheme for on-line separations. Aspects including sensitivity, mass resolution, duty cycle, and tandem mass spectrometric capabilities are discussed in the context of online separations with examples from the authors' laboratory.
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  • 39
    ISSN: 0935-6304
    Keywords: HPLC of phenols ; Dianthus caryophyllus ; Carnation vascular wilt ; Fusarium oxysporum f. sp. dianthi ; Root phenolic compounds ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 40
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    Journal of High Resolution Chromatography 19 (1996), S. 43-48 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Mass spectrometry ; Wax esters ; Festuca arundinacea ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The ester portion of epicuticular waxes of tall fescue (Festuca arundinacea Schreb.) is composed of mixtures of homologous series of fatty acids esterfied with fatty alcohols. GC analyses of natural esters gave rise to the separation of several compounds of different chain length. To identify and quantify individual components in the mixture, GC/MS analyses were carried out, and the mass spectra of each peak were recorded and analyzed for characteristic ions. This approach permitted a comparison with data obtained from classical methods using GC analysis of acid and alcohol moieties obtained by hydrolysis.
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  • 41
    ISSN: 0935-6304
    Keywords: Optimization of GC conditions ; Sugar analysis ; Acid analysis ; Chlorogenic acid ; Raffinose ; Pectin decomposition products ; Galacturonic acid ; Arabinose ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Our GC-MS method for the simultaneous quantitation of sugars and acids as their silyl(oxime) derivatives, from one solution by one injection, has been extended to the reproducible determination of high molecular weight compounds sensitive to decomposition yet requiring a high evaporation temperature (e.g. chlorogenic acid and rffinose) and for the quantitation of the decomposition products of pectin (i.e., for the determination of galacturonic acid at low ng levels in the presence of a 10-100 fold excess of glucose eluting just before the acid). The optimized GC procedure has been used for quantitation of the sugar and acid (including chlorogenic acid) composition of potato samples, and for the determination of the increasing amount of the decomposition products of pectin substances in apple pulp after different storage times.
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    Journal of High Resolution Chromatography 19 (1996), S. 66-66 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 19 (1996) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 19 (1996), S. 180-182 
    ISSN: 0935-6304
    Keywords: trans-Fatty acids ; Semi-industrial frying ; Capillary GC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 45
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    Journal of High Resolution Chromatography 19 (1996), S. 183-188 
    ISSN: 0935-6304
    Keywords: Chelating agents ; Complexation ; Capillary zone electrophoresis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A capillary electrophoretic method has been developed which achieves rapid quantitative separation and determination of ethylenediaminetetraacetic acid, N-(2-hydroxyethyl)ethylenediaminetriacetic acid, diethylenetriaminepentaacetic acid, ethylenediaminediacetic acid, and nitrilotriacetic acid in Hanford tank waste simulant (TWS). Direct UV detection of Cu2+/chelator complexes is used to achieve enhanced sensitivity. The qualitative and quantitative reliability of the method and the quality of separations, as given by efficiency and resolution, is presented. In addition, the limits of detection and linearity of detector response with concentration are given for each chelator. The selection of Cu as the UV-absorbing species over other transition metals present in the waste is discussed.
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  • 46
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    Journal of High Resolution Chromatography 19 (1996), S. 49-53 
    ISSN: 0935-6304
    Keywords: Polycyclic aromatic sulfur heterocycles ; Crude oil ; Oil maturity ; Fingerprinting ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method is presented for the identification and quantification of C2-substituted benzothiophenes in crude oil. The method will enable analysis of the pattern of these compounds, for example as a basis for differentiating crude oils from one another (fingerprinting) and for investigation of their suitability as indicators of oil maturity. Here results are reported for five crudes from Iraq, Venezuela, Saudi Arabia, the former Soviet Union, and the North Sea. The aromatic fraction of the crudes was oxidized and the dioxides of the heterocycles separated according to the number of carbon atoms in the side chains. The final separation was by capillary GC with atomic emission or flame ionization detection. A fluorinated analog was synthesized and used as internal standard. The concentrations of 2,3-, 2,4-, 2,7-, and 3,7-dimethylbenzothiophene ranged between 11 and 272 ppm. Three other dimethylated benzothiophenes present in lower amounts were also identified.
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  • 47
    ISSN: 0935-6304
    Keywords: Capillary Supercritical Fluid Chromatography ; Mass Spectrometry ; SFC-MS ; On-line combination ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An interface for coupling supercritical fluid chromatography to a magnetic sector mass spectrometer was developed and evaluated. The interface is based on direct introduction of the mobile phase, carbon dioxide, into the ion-source of the mass spectrometer. The SFC-MS system was optimized with respect to the signal-to-noise ratio. Under optimized conditions, the estimated detection limit for n-pentadecane is approximately 30 ppm. Spectra obtained in the electron-impact ionization mode show a very good similarity with library spectra. The performance of the SFC-MS system was evaluated by the analysis of a number of test mixtures. A sample containing several low molecular mass, thermally unstable compounds, which could neither be analyzed by GC-MS nor by LC-MS, was analyzed. Also for the analysis of high molecular mass compounds, the coupled system showed a good performance.
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  • 48
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    Journal of High Resolution Chromatography 19 (1996), S. 37-42 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The headspace gas in static headspace gas chromatography contains mostly saturated water vapor. In the case of the cryofocusing enrichment technique this may cause baseline distortion in the early part of the chromatogram or may even lead to ice-plugging of the capillary column. A water-trap is described in which the water vapor is removed from the headspace gas before entering the cryo-trap. The water trap is packed with lithium chloride on a porous support and is regenerated after each analysis by heating under backflush conditions. It therefore can be used for automatic operation. Data are given for the precision and accuracy, and some practical examples, for environmental and flavor analysis are shown.
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  • 49
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    Journal of High Resolution Chromatography 19 (1996), S. 59-61 
    ISSN: 0935-6304
    Keywords: Steam chromatography ; Salt-water stationary phases ; Retention of alcohols ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 50
    ISSN: 0935-6304
    Keywords: Gas Chromatography ; Ion-Trap Mass Spectrometry ; Pesticide residue analysis ; Eggs ; Ardea cinera ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 19 (1996), S. 65-65 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 19 (1996), S. iii 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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  • 53
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    Journal of High Resolution Chromatography 19 (1996), S. 80-84 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Specific detectors ; ECD/FPD response ratios ; Retention indices ; Identification on real samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A previous paper reported the possibility of using the ratio between the responses of two different specific detectors to a single compound (detector response ratio, DRR) as an identification criterion for that compound, in combination with its retention index.This article gives some applications of DRR in the identification of some pesticides in four different fruits (apples, apricots, strawberries, and peaches) in a range varying from 0.02 to 1.3 ppm, by means of their ECD/FPD DRRs. After clean-up GC analyses were performed on a single column with dual parallel detection; a personal computer system was used for data analysis.
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    Journal of High Resolution Chromatography 19 (1996), S. 91-94 
    ISSN: 0935-6304
    Keywords: Chiral selector anchored to polysiloxane ; Chiral phase capillary GC ; Immobilization ; Thermal treatment ; High enantioselectivity ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The chiral selector L-t-leucine-t-butylamide has been anchored to a polysiloxane by nucleophilic displacement of 2,2,2-trifluoroethyl ester-functionalized block polysiloxanes with L-t-leucine-t-butylamide. Attempts were made to immobilize the chiral polysiloxanes inside the capillaries by thermal treatment at 300°C for 30-90 min. The polysiloxanes were found to be more resistant than Chirasil-Val to the racemization caused by such high temperature treatment. Capillary columns coated with this type of immobilized polysiloxane have shown very high enantioselectivity and thermal stability.
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    Journal of High Resolution Chromatography 19 (1996), S. 284-284 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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  • 56
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    Journal of High Resolution Chromatography 19 (1996), S. 277-283 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Coupled columns ; Four factor optimization ; Simplex method ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Optimization of a gas chromatographic system with two capillary columns coupled in series in a single oven for the linear temperature programmed separation of a mixture of C1—C10 hydrocarbons has been carried out using the simplex optimization method. The following four selectivity parameters were optimized: the initial temperature of the oven; the initial hold time; the temperature programmed rate; and the pressure at the mid-point of the system. The optimization procedure was monitored by the Cp criterion.
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  • 57
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    Keywords: Capillary electrophoresis-mass spectrometry ; Membrane preconcentration ; Capillary electrophoresis ; Sulfonated membrane ; Polar drug metabolites ; Toxic oil syndrome ; Eosinophilia-myalgia syndrome ; 3-Phenylamino-1,2-propanediol ; 3-Phenylamino-L-alanine ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 19 (1996), S. VII 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 19 (1996), S. 298-300 
    ISSN: 0935-6304
    Keywords: Dynamic head space ; Coffee berry ; Identification ; Hypothenemus hampei ; Plant-insect relationship ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 60
    ISSN: 0935-6304
    Keywords: Capillary GC ; Drug screening ; Retention index ; Reporting ; Mean list length ; Blood analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A dual-column gas chromatographic retention index method was evaluated for the toxicological screening for basic drugs in autopsy blood samples. The dual-column approach with DB-5 and DB-1701 capillary columns doubles the Identification Power of the corresponding single column methods. The long-term intralaboratory variation of the dialkylfluoroaniline series based retention indices of drugs in blood ranged from 0.03% to 0.2% which was generally better than that obtained using the relative retention time. Novel software is described for the processing and reporting of the dual-column chromatographic data in analytically useful form. Besides retention data, the response factors served as an additional identification factor.
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    Journal of High Resolution Chromatography 19 (1996), S. 327-332 
    ISSN: 0935-6304
    Keywords: Capillary GC ; Separation performance ; Fourier analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A simple procedure is presented for determining separation performance of HRGC analysis of multicomponent mixtures. The procedure is based on the computation of Autocovariance Function (EACVF) from the digitized experimental chromatogram. Graphic inspection of the EACVF plot permits easy computation of the width value of the single component peak, σ; from the EACVF value at t=O the number of component in the mixture, m, can be simply derived. From these two basic quantities all the other chromatographic performance attributes can be calculated. The consistency of the procedure is tested for different chromatograms and compared with the more complex EACVF fitting method. Several features of the multicomponent chromatogram, overloading effects included, are directly detected.
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    Journal of High Resolution Chromatography 19 (1996), S. 339-344 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Trace gas analysis ; Multichannel thick film silicone rubber traps ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Established standard methods for analyzing semi-volatile pollutants by capillary gas chromatography are cumbersome, time-consuming, and expensive. With the longer term aim of replacing the sample preparation procedures with convenient concertrating and thermal desorption steps, thick film silicone rubber traps were constructed in a novel multi-channel configuration. Tests were performed to determine breakthrough volumes and thermal desorption characteristics for total transfer of the trap contents to a capillary column. Initial results are very promising.
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    Journal of High Resolution Chromatography 19 (1996), S. 333-338 
    ISSN: 0935-6304
    Keywords: Adsorptive enrichment/thermal desorption ; Microtrap ; VOC and PVOC analysis ; Humid air sample analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An instrument has been developed and tested for the continuous measurement of volatile organic compounds (VOC) in air. The system consists of a gas chromatograph equipped with a dedicated sampling device that allows the sample to be transferred to a cooled microtrap via sampling loops (10, 100, 250 ml) or via a direct pump transfer to the trap. The microtrap is placed in the chromatographic oven just below a modified split-splitless injector, allowing direct liquid injection for calibration of the system; the injector is in communication with the sampling valve equipped with the loop and the sampling pump. The system allows 24-hour sampling and analysis of a large number of VOC (up to 25 individual hydrocarbons ranging from C2—C9) and also polar volatile organic compounds PVOC. Thanks to the particular trap geometry, a minimum consumption of liquid nitrogen (between 150—300 ml) is needed for each analytical run and no water managing system is normally required for humid air samples.
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    Journal of High Resolution Chromatography 19 (1996), S. 353-358 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Gas chromatography-mass spectrometry ; Essential oil analysis ; Ylang-ylang oil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Steam distillation (SD), simultaneous distillation-solvent extraction (SDE), and supercritical (CO2) extraction (SFE) were used to isolate volatile secondary metabolites from fresh, totally mature flowers of Colombian ylang-ylang (Cananga odorata). The various extracts were analyzed by capillary chromatography (DB-1, DBWAX, 60 m columns) using FID, NPD or MSD (EI, 70 eV). Kováts indexes, mass spectra, or standard substances were employed for compound identification. 51, 70, and 73 compounds at concentrations above 100 ppb were detected in the SD, SDE, and SFE extracts, respectively. The main constituents of these extracts were linalool (20.7, 28.0, and 16.5%), germacrene-D (10.1, 3.1, and 20.3%) benzyl benzoate (14.1, 2.9, and 3.9%), benzyl acetate (9.6, 17.0, and 6.2%), caryophyllene (3.1, 2.9, and 3.9%), and p-methylanisole (6.8, 6.1, and 2.7%). 85% of the composition of SDE extracts was represented by oxygenated compounds. Heavy hydrocarbons (Cn 〉20) and fatty acids were found only in the SFE extracts, which also had a higher content of nitrogenated compounds (phenylacetonitrile, 4-methylbenzaldoxime, indole, 2-phenyl-nitroethane, and methyl anthranilate) and sesquiterpenes (43% vs 19.5% in SD and 8.1% in SDE) and 1.5 - 2 times lower concentration of monoterpenes and light oxygenated compounds than the SD (49.7%) and SDE (64.5%) extracts.
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    Journal of High Resolution Chromatography 19 (1996), S. 359-361 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Atomic emission detection ; Triclosan ; Dental plaque ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A validated gas chromatographic method for the determination of triclosan in human dental plaque is described. Based on plaque sample weights of 10 mg, the limit of detection (2 × S/N) is 0.5 μg/g. The method is linear (r = 0.9986) from the limit of detection to 50 μg/g. Recoveries from placebos spiked with 2.0, 25, and 50 μg/g of triclosan were 105.6%±7.5%, 107.2%±3.1%, and 99.1%±1.1%, respectively (n = 3 at each level). Twenty replicate preparations and analyses of a homogenized sample, conducted by two operators over the course of 4 days, showed agreement to within 9% RSD. Analyses of dental plaque collected from patients after brushing with dental cream containing triclosan, shows triclosan to be retained in dental plaque at concentrations above the minimum inhibitory concentration (1 μg/g) after 12 h.
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    Journal of High Resolution Chromatography 19 (1996) 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 19 (1996), S. 371-371 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 19 (1996), S. 377-382 
    ISSN: 0935-6304
    Keywords: Capillary chromatography ; Boiling points prediction ; Identification ; Chlorobenzenes ; Phenols ; Programmed temperature ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Quantitative correlations between physicochemical parameters and structure of various solutes and their gas chromatographic behavior were investigated in order to predict the retention values. The identification of unknown samples in gas chromatographic routine analysis of environmental samples is enhanced by the use of these correlations in conjuction with other chromatographic methods and with mass spectrometry. The boiling points of many compounds are easily found in literature and therefore their correlation with retention values obtained in isothermal or programmed temperature analysis permit restriction of the choice of names of unknown compound to within a narrow range. The correlation between the boiling points and the retention times of chloro- and bromo-benzenes and of some chloro- and nitro- substituted phenols was investigated on non-polar capillary columns and permitted the tentative identification of many compounds belonging to these homologous series.
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  • 69
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; FID, O-FID, and MS detection ; Glycol ethers and glycol ether acetates ; Heptafluorobutyryl derivatives ; Mass spectra ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Twelve compounds, commonly used as industrial solvents and belonging to the chemical class of glycol ethers and glycol ether acetates, were investigated. Several analytical conditions, applied to single or connected capillary columns of different length and polarity coating and connected to FID, O-FID and MS detection systems, were assayed. Tests on heptafluorobutyryl derivatives were also attempted to improve the analytical sensitivity. The aims were to establish gas chromatographic methods suitable for analysis of reference standard compounds and to verify their applicability to biological matrix analysis for pharmacokinetic and toxicological studies, since these chemicals have been shown to be hazardous in laboratory animals and are presumed to be dangerous in man.
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    Journal of High Resolution Chromatography 19 (1996), S. 444-448 
    ISSN: 0935-6304
    Keywords: LC-GC coupling ; Loop-type interface ; Alcohols ; Sterols ; Olive oil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A modified loop-type interface is decribed which uses two 6-way valves and concurrent eluent evaporation to perform an on-line transfer and simultaneous gas chromatographic analysis of two different fractions pre-separated by liquid chromatography. The interface is used to simultaneously analyze aliphatic alcohols and sterols present in olive oil. LC pre-separation is carried out using a normal phase column (20 cm × 0.21 cm i.d.) and hexane-isopropanol (99:1) as a mobile phase at a flow of 0.2 ml/min; for the GC analysis a 5 % phenyl, 95 % dimethyl siloxane (25 m × 0.32 mm i.d., 0.4 μm film thickness) column is used.
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    Journal of High Resolution Chromatography 19 (1996), S. 462-462 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 19 (1996), S. 463-463 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 19 (1996), S. 449-456 
    ISSN: 0935-6304
    Keywords: Supercritical fluid chromatography (SFC) ; Packed columns ; Pressure drop ; Selectivity ; Resolution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The influence of pressure drop on retention, selectivity, plate height and resolution was investigated systematically in packed supercritical fluid chromatography (SFC) using pure carbon dioxide as the mobile phase. Numerical methods developed previously which enabled the prediction of pressure gradients, diffusivities, capacity factors, plate heights and resolutions along the length of the column were used for the model calculations. The effects of inlet pressure and supercritical fluid flow rate on selectivity and resolution are studied. In packed column SFC with pure carbon dioxide as the mobile phase, the pressure drop can have a significant effect on resolution. The flow rate is shown to have a larger effect than generally realized. The calculated data are shown to be in good agreement with the experimental results. Finally, the variation of the chromatographic parameters along a 5.5 meter long model SFC column is illustrated. The possibilities and limitations of using long packed columns in SFC are discussed. It is demonstrated that long columns with large plate numbers do not necessarily yield better separations.
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    Journal of High Resolution Chromatography 19 (1996), S. 464-464 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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  • 75
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Purge and trap extraction ; 1,2,4-TCB ; Environmental analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High resolution gas chromatography (HRGC) coupled to a “purge and trap” extraction-injection technique is described as a method of determining 1,2,4-trichlorobenzene in water at levels as low as parts-per-trillion (ppt). In order to investigate the interference from other volatile organic compounds (VOCs) several detection systems were compared: flame ionization, electron capture, and mass spectrometry-multiple ion detection. Concentrations ranging from 15 to 600 ng/L were analyzed in 20 ml standard aqueous solutions. The mean accuracy of the method varied from 89 to 103%, and its mean precision varied from ± 0.85 to ± 7.5 % for all detectors. The detection limits were 20 ng/L for FID, 2 ng/L for ECD and 0.5 ng/L for MID-MS detectors. The procedure was successfully applied to the analysis of industrial waste waters. The necessity of an appropriate internal standard to improve the quantitative determination and to determine possible losses or degradation of 1,2,4-trichlorobenzene during handling or storage is discussed.
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    Journal of High Resolution Chromatography 19 (1996), S. 469-471 
    ISSN: 0935-6304
    Keywords: Microextration ; GC/MS ; Chlorobenzenes ; Water samples ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 19 (1996), S. 465-469 
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction (SFE) ; Beef ; Anabolic steroids, synthetic ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 19 (1996), S. vii 
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    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
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    Journal of High Resolution Chromatography 19 (1996), S. 478-480 
    ISSN: 0935-6304
    Keywords: Capillary zone electrophoresis ; Chiral separation ; Cyclodextrins ; Methoxamine ; Lobeline ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 19 (1996), S. 492-496 
    ISSN: 0935-6304
    Keywords: High - speed capillary GC ; Carbon dioxide cryotrap ; Deactivated metal tubing ; Thermal decomposition ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ten different metal tubings were investigated for thermal decomposition of analytes when used as the trap tube in a cryotrap/thermodesorption inlet system. No noticeable sample decomposition of hydrocarbons, chlorinated hydrocarbons and a brominated hydrocarbon was observed for six of the tubings with hydrogen as the carrier gas. This observation may be partly attributed to the developed deactivation techniques that produce inert metal tubings that are being widely adopted by many column manufacturers, the different trap materials used in comparison to previous studies and the decreased sample residence time in the hot trap tube. A cryotrap using carbon dioxide was constructed and tested as a alternative to the previously used liquid nitrogen based systems. This cryotrap was able to trap compounds with a boiling point of 80°C.
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    Journal of High Resolution Chromatography 19 (1996), S. 511-514 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Enantiomer separation ; Amino acids ; N-Alkyloxycarbonyl alkylamide derivatives ; Nucleophilic substitution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The enantiomers of amino acids were first converted into N-alkyloxycarbonyl 2,2,2-trifluoroethyl esters, and then into N-alkyloxycarbonyl alkylamides by nucleophilic substitution of the ester group with amines. The first reaction proceeds instantaneously, while the second substitution occurs smoothly with n-propylamine and isobutylamine. The final derivatives were produced for separation on a capillary column coated with Chirasil-Val by GC. Pro, which is difficult to separate completely as its N-perfluoroacyl alkyl ester derivative, showed complete separation of the enantiomeric pair. All amino acids examined in this study showed an increased separation factor.
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    Journal of High Resolution Chromatography 19 (1996), S. 530-533 
    ISSN: 0935-6304
    Keywords: High-performance liquid chromatography ; Paeoniae Radix ; Peony constituent separation ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 19 (1996), S. 543-548 
    ISSN: 0935-6304
    Keywords: Gas chromatography ; High temperature ; Dead time ; Constants of the n-alkane retention time curve ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In gas liquid chromatography, the column dead time and the constants of the n-alkane retention time curve are calculated by the multiparametric least-squares regression iterative method at high temperature between 180 and 270°C. The method was applied to two types of columns. The first group includes eight packed columns (seven OV polymethylphenylsiloxane and Apolane-87), while the second includes five glass capillary columns (four methylsilicone with different film thicknesses and Apolane-87). The calculated tM and b values were compared with those obtained by Guardino's, Grobler's, and Kaiser's methods. The influences of coating thickness and temperature thereon were investigated.
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    Journal of High Resolution Chromatography 19 (1996), S. 569-570 
    ISSN: 0935-6304
    Keywords: Microbore SFC ; Chiral separation ; 3,5-Dimethylphenyl carbamate derivative of cellulose ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    Journal of High Resolution Chromatography 19 (1996), S. 559-563 
    ISSN: 0935-6304
    Keywords: Pesticide residue analysis ; Solid phase extraction ; Ground water ; Surface water ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A critical study of a solid phase extraction method using C18 SPE columns for the determination of 23 halogenated pesticides is presented. Type of sorbent, sorbent mass, flow rate in the extraction process, sample concentration of the different compounds, sample volume, pH, ionic strength and type of water were evaluated. Recoveries of pesticides under study yield a linear relationship, except for conazole fungicides and captan. Losses can be expected for heptachlor, aldrin, and captan. Sample volume and flow rate of extraction affect recoveries. Matrix effects from surface and groundwaters were observed. Recoveries for vinelozolin and dieldrin from groundwater were lower than those obtained from nanopure water. In river water losses of these compounds are higher. Captan and penconazole were not present and high losses were obtained for trifluralin, α-BHC, γ-BHC, tri-allate and chlorpyriphos. Impurities arising from the sorbent materials of cartridges have been detected.
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  • 86
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 549-558 
    ISSN: 0935-6304
    Keywords: Size exclusion chromatography ; Petroleum waxes ; Flame ionization detector ; Refractive index detector ; Molecular weight distribution ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Molecular weight distribution of solid petroleum waxes is a key parameter for the general characterization of these materials. Particular interest concerns extremely large components, typically present in oil distillation residua, and solid deposits found in oil production facilities. Molecular weight distributions of oil waxes were determined in this work by high temperature size exclusion chromatography. Separations were carried out with two different eluents, namely toluene and ortho-dichlorobenzene and two detection systems, these being a differential refractive index and a flame ionization detector. Toluene proved to be the best choice when combined with flame ionization detection. Better uniformity of response was the greatest advantage achieved by this approach. The experimental set up permitted analysis of samples containing molecules with up to 138 carbon atoms. Burning properties of very large molecules, isomerism affecting calibration, and signal asymmetry when flame ionization detection was adopted were three issues still requiring additional efforts to understand and to improve analysis accuracy.
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  • 87
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 577-580 
    ISSN: 0935-6304
    Keywords: Phenolic compounds ; Solid phase extraction ; Coal gasification ; GC/MS ; XAD-4 ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 88
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 588-590 
    ISSN: 0935-6304
    Keywords: Supercritical fluid extraction ; Water samples ; Polycyclic aromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 5 Ill.
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  • 89
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 585-587 
    ISSN: 0935-6304
    Keywords: Enantioselective gas chromatography ; Volatiles ; 2-Heptanol ; Ethyl benzoate ; (E)-Hex-2-enal ; 1-Terpinen-4-oI ; Rubus glaucus ; Rosaceae ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 1 Tab.
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  • 90
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 596-596 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 91
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 92
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 597-607 
    ISSN: 0935-6304
    Keywords: Capillary gas chromatography ; Atomic emission detection ; Environmental applications ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Environmental applications of capillary gas chromatography coupled with atomic emission derection (GC-AED) have been reviewed with emphasis on both the commercial and laboratory-built systems. Attention was focused on (1) element-selective detection of non-metallic as well as metallic pollutants, (2) identification of contaminants, and (3) sample preparation considerations.
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  • 93
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 613-616 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Electrochemical detection ; End column detection ; Nickel electrode ; Carbohydrates ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Carbohydrates were separated by capillary electrophoresis (CE) and detected electrochemically using a nickel microelectrode which was operated at a constant applied potential (∼0.6 V vs. Ag/AgCI). A simple capillary electrode holder design facilitated alignment between the separation capillary and the working microelectrode without the use of micro-positioning equipment. The separations were performed under alkaline conditions (pH 〉 11), matching the high pH requirements for amperometric detection at the nickel electrode. The analytical procedure developed showed detection limits for the carbohydrates studied in the micromolar range, showing a linear response in the range tested (micromolar to millimolar). The procedure was used to identify sugars in two real samples (i.e., urine and in a common beverage). The potential use of the system for the determination of amino acids was also demonstrated.
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  • 94
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 691-695 
    ISSN: 0935-6304
    Keywords: HPLC ; Molecular sieve ; Cis-trans isomers ; Phenols ; Selectivity ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A molecular sieve known as Silicalite was used as the column packing for HPLC. Silicalite contains channels (or cavities) approximately 6 Å in diameter but, unlike most other molecular sieves, Silicalite is hydrophobic. The retention times of methyl ketones and substituted phenols containing n-alkyl groups increase with increasing chain length of the substituent. However, phenols with very bulky substituents appear to be excluded from the Silicalite channels and elute very quickly. Excellent separations were obtained for a number of compounds with only slight differences in chemical structure. These include phenol isomers with a primary- or secondary alkyl group, position isomers of substituted phenols, and aliphatic cis-trans isomers.
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  • 95
    ISSN: 0935-6304
    Keywords: Capillary zone electrophoresis ; Chiral separation ; Cyclodextrin ; Anisodamine ; Glycopyrronium ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
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  • 96
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 622-626 
    ISSN: 0935-6304
    Keywords: Multidimensional capillary chromatography ; Polychlorinated biphenyls ; PCBs ; Congener ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Multidimensional chromatography was used to resolve the specific chlorobiphenyl (CB) congeners 28, 52, 101, 118, 138, 153, and 180 in technical aroclor standards. Single column analysis of polychlorinated biphenyls (PCBs) results in co-elution of key congeners with other components in the mixture; therefore using two columns of different selectivity was necessary to enhance the resolution achievable on just one column. The HT8 column (8% phenylpolycarborane-siloxane phase) has been reported to have specific selectivity characteristics for improved PCB separation. When coupled with a BPX5 column (5% phenylpolysiloxane-silphenylene phase), it has been shown here to provide unambiguous identification of 7 marker compounds which are used to monitor PCB occurrence and distribution. All seven marker CBs are present in aroclor 1254, and by adjusting the size of the heartcut window, it was possible to obtain resolution of the marker congeners from other congeners. Single column analysis is unable to achieve this result. This offers an alternative to GC-MS analysis.
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  • 97
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 647-650 
    ISSN: 0935-6304
    Keywords: Capillary zone electrophoresis (CZE) ; Separation of herbicides ; Chlorophenoxy acid ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 98
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996) 
    ISSN: 0935-6304
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 99
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 69-79 
    ISSN: 0935-6304
    Keywords: Large volume injection ; PTV injector ; Water analysis ; River sediment ; Pesticides ; Polycyclic aromatic hydrocarbons (PAHs) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Temperature programmable (PTV) injectors with packed widebore (ca. 3.5 mm i.d.) liners are used for large volume injection in capillary gas chromatography with the aim to simplify and/or improve off-line sample pretreatment proecdures. A simple procedure for optimization of large volume PTV injection is described. The system performance, i.e. linearity and repeatability, is evaluated for polar nitrogen/phosphorus containing pesticides (PTV-GC-NPD) and organochlorine pesticides (PTV-GC-ECD) in river water extracts as well as for polycyclic aromatic hydrocarbons (PAHs) in river sediment (PTV-GC-MS).
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  • 100
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    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 124-126 
    ISSN: 0935-6304
    Keywords: Reversed-phase HPLC ; Propionic antiinflammatory drugs ; Barbituric sedatives and hypnotics ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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