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  • Column liquid chromatography  (1.216)
  • Springer  (1.216)
  • Wiley
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  • 1
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Reversed-phase ; Codeine phosphate drug substance ; Opium alkaloids
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A rapid procedure for the evaluation of codeine phosphate drug substance derived from poppy straw or opium concentrate is described. The gradient HPLC procedure employs a pH 2.5 phosphate buffer, methanol and acetonitrile mobile phase at 40°C and a μBondapak C-18 column. Eight opium alkaloids, including the four major alkaloids, are separated from each other. The paper describes details of the assay procedure and presents data documenting the linearity, specificity, precision, and sensitivity of the method.
    Materialart: Digitale Medien
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  • 2
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 20 (1985), S. 335-342 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; External variance determinations ; Column and system compatibility ; Microbore and fast LC
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The demand for faster, more economic and convenient high-efficiency LC analyses has led to the development of microbore and fast columns. However, to utilize their benefits, the low column dispersions produced by these new technologies necessitate low external variances in the total system. This paper describes the determination of the external variance of microbore, fast and conventional LC systems by a column method. Compatibility with the relevant column technologies is evaluated by a method involving the comparison of the external and column dispersions. Direct comparison of chromatograms of an 8-component mixture, on a set of columns of various diameters and lengths, shows the relative speed, economy and sensitivity obtainable in practice. The problem of reduced sample loadability is considered and the practical solution of peak compression illustrated.
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  • 3
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Retention prediction system ; UV multichannel detector ; Polycyclic aromatic hydrocarbons
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The retention prediction system assisted by a micro-computer coupled with an UV multichannel detector has been investigated in the separation of polycyclic aromatic hydrocarbons. The method offered very precise identification of components in NBS-SRM-1647 sample without any standard reference substances. It has been proven that the system makes very precise, non-pollutive and convenient environmental analysis possible.
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  • 4
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 20 (1985), S. 313-322 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Tetracyclines antibiotics ; Quantitation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The use of high-performance liquid chromatography (HPLC) for the identification and determination of tetracycline antibiotics is reviewed. HPLC chromatograms provide fast identification by retention time, tR, and precise quantitation by measurement of peak height or peak area. For separation of tetracycline compounds, most HPLC methods use reversed-phase C18 or C8 columns and UV detection. The HPLC solvent system should have a pH of about 6 to prevent steric changes in the tetracycline molecule. For accurate quantitation it is necessary to avoid tailing and this is accomplished by adding a zwitter ion to the solvent system. Methanol and acetonitrile are frequently used as organic modifiers in these solvent systems. In a single analysis, HPLC methods can be used to separate as many as nine or ten commercially used tetracycline compounds and to determine four to five tetracyclines in commercial tetracycline preparations or in biological fluids.
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  • 5
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Resolution of optical isomers ; Chiral column ; Pyrethroids ; Fenvalerate
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The separation of the optical isomers of fenvalerate [cyano(3-phenoxyphenyl)methyl 2-(4-chlorophenyl)-3-methylbutyrate] has been carried out by high-performance liquid chromatography (HPLC) on a chiral column with (R)-N-3,5-dinitrobenzoyl-phenyl-glycine (DNBPG) covalently bonded on aminopropyl silica and eluted with mixtures of methanol, 2-propanol, and hexane. The system was applied to the analysis of Pydrin®, an emulsifiable concentrate formulation of fenvalerate, and to the residue analysis of fenvalerate in milk samples. For the analysis of Pydrin® the only requirement was the proper dilution of Pydrin® with hexane. For the analysis of residues in milk, fenvalerate was extracted with hexane after precipitating the milk proteins with acetonitrile and removing the precipitate by filtration; the hexane extract was concentrated to small volume and filtered before being analyzed by HPLC.
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  • 6
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 20 (1985), S. 487-494 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Size-exclusion chromatography ; Controlled-porosity glasses ; Boron-enriched glass surface ; Adsorptive properties
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Controlled-porosity glasses (CPG) are sieves for macromoleculars, very widely applied in chromatographic columns for the separation of polymers and biopolymers by means of size-exclusion chromatography (SEC) and affinity chromatography. This paper deals with the influence of the thermal treatment of CPG on the elution of polymers in SEC columns. The problem is examined for a few mobile phases and for glasses having different porosities. Additionally, the SEC results obtained are compared with the adsorption properties of the glases investigated.
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  • 7
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 21 (1986), S. 645-647 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Electrochemical detection ; Cysteinyldopamine ; Tyrosinase ; Autoxidation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary 5-S-Cysteinyldopamine, a new metabolite of dopamine, was determined in urine by high-performance liquid chromatography with electrochemical detection. The catechol was detected in 14 of 21 melanoma patients and 7 of 21 normal subjects; the highest values were 657 μg/day for melanoma patients and 44 μg/day for normal subjects. These results suggest that the cysteine conjugate may arise from autoxidation of dopamine but tyrosinase may also participate in the oxidation.
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  • 8
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 21 (1986), S. 136-142 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Chemical reaction detector ; Carbamate insecticides ; Quantitation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary For the determination of trace amounts of carbamate insecticides in vegetables the combination of liquid chromatography with post column chemical derivatization (chemical reaction detector) is used. In a two step reaction detector the carbamates are firstly saponified in 0.01 M sodium hydroxide at 80°C with a reaction time of 30sec. To this mixture OPA reagent is added to detect the methylamine generated in the saponification. Optimization strategies for this reaction are demonstrated. At a temperature of 80 °C a reaction time of 80 sec is sufficient for quantitative transformation of the methylamine. The peak dispersion can be reduced and hence the detection limit improved by decreasing the diameter of the tubes and by diminishing dilution through the addition of reagent. A 1∶24 ratio of reagent to column (reactor) effluent is possible with cyclone-type mixers. The quantitation of carbamates in different vegetables is demonstrated. The detection limit is 20ppb at a signal to noise ratio of 10∶1.
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  • 9
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 21 (1986), S. 205-213 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Chiral phases ; Optimization of separation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The preparation and properties of chiral bonded phases with amino acid groups are described. These phases were used in non-polar eluents and in aqueous systems in the presence of Cu2+ ions in the ligand-exchange mode. The optimization of chiral resolution is demonstrated for both cases. With non-polar eluents similarity between bonded groups and solutes is required. The elution could be accelerated by non-protonic moderators. Ligand-exchange separation is influenced by the copper content of the eluent and the stationary phase, the organic moderator concentration, the pH and ionic strength of the buffer and by the temperature. Structural requirements of both the bonded groups and of the solutes for chiral separation are discussed.
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  • 10
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Reversed-phase capacity factors ; Cavity term ; Molar volumes
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Reversed-phase liquid chromatographic capacity factors are well correlated by an equation of the form: $$logk' = (logk')_0 + mV/100 + s\pi ^* + b\beta + a\alpha $$ wheremV/100 measures the cavity term and π*, β, and α are the solvatochromic parameters that measure solute dipolarity/polarizability, hydrogen bond acceptor basicity, and hydrogen bond donor acidity respectively. Liquid molar volume (molecular weight divided by liquid density at 20°C) $$\bar V$$ , and computer-calculated intrinsic (van der Waals) molecular volume, $$\underset{\raise0.3em\hbox{$\smash{\scriptscriptstyle-}$}}{V} _I $$ , are compared as measures of the cavity term in a number of correlations. $$\underset{\raise0.3em\hbox{$\smash{\scriptscriptstyle-}$}}{V} _I $$ leads to more precise correlations as well as to a “cleaner” dissection of the multiple solute/solvent interactions. The opposing exoergic effect of solvent donor/solute acceptor hydrogen bonding, and endoergic cavity term are the main factors influencing HPLC capacity factors.
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  • 11
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 22 (1986), S. 40-42 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Pyridate ; CL-9673 ; Reversed phase
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The application of a simple reversed-phase, HPLC-UV method for the determination of the contact herbicide pyridate and its main metabolite 3-phenyl-4-hydroxy-6-chloropyridazine-known as CL-9673-in green cereals, grains and straw is described. The method is based on a simple extraction, separation of pyridate from its metabolite, hydrolysis of pyridate to CL-9673, high-performance liquid chromatographic separation of CL-9673 in both fractions using only one reversed phase column and UV-detection. The method is sensitive down to 3 ngg−1 CL-9673 in green plants and grain and 5ngg−1 in straw. In the range 0.05–1.0mgkg−1 recoveries are between 73.7% and 109% from green plants, between 77.7% and 102% from grains and between 77.3% and 87.5% from straw.
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  • 12
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Betablocker drugs ; Lipophilicity ; Capacity factors ; Distribution coefficients
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The reverse-phase, high-pressure liquid chromatographic capacity factors (k') of a series of 18 betablocking agents were determined in order to establish correlations with their distribution coefficient values (D), obtained from four bibliographic sources. Under the three pH conditions studied (3.5, 6.2 and 7.5) statistically significant linear correlations (p〈 0.002) between log k' and log D values were obtained for the four series studied. In this series it is concluded that the k' factor is a useful and reliable relative lipophilicity parameter.
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  • 13
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 22 (1986), S. 81-87 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Recycle chromatography ; Pressure dependence ; Capacity factor
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary It was found experimentally that the potential for routine, rapid high-efficiency separations by alternate column, recycle, reversed-phase chromatography is limited by the increase of capacity factors with pressure.
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  • 14
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 18 (1984), S. 633-636 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Aromatic acid isomers ; Low capacity ion-exchange resin ; Microbore packed columns
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A low-capacity, anion-exchange, porous-polymer resin was used as the packing material in a microbore column. Using a phosphate buffer containing various organic modifiers, retention behavior of substituted benzoic acid isomers with amino, chloro, methyl, nitro and carboxylic groups was investigated. The effect of ethanol, acetonitrile and sodium dodecylsulfate used as organic modifiers on the retention behavior at various eluent pH values was studies and optimum separations of the positional isomers reported.
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  • 15
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 18 (1984), S. 668-672 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Mixed eluents ; Preferential sorption of eluents ; Pressure effects
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Pronounced base line perturbations were repeatably observed in LC both in alternating recycling and in backflushing experiments when binary eluents and refractometric detectors were used. The perturbations which we call eigenzones appeared immediately after operating the recycling or the backflushing valve, and their size and shape depended on the nature of both the column filling and the mixed mobile phase as well as on the pressure drop across the column. Experimental results presented confirm that the primary causes of the eigenzones were the pressure changes in the columns which influenced the sorption equilibrium of mixed eluent components within the column packing. Some practical consequences of this effect are briefly discussed.
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  • 16
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 18 (1984), S. 677-679 
    ISSN: 1612-1112
    Schlagwort(e): Polycyclic aromatic hydrocarbons ; Column liquid chromatography ; Polyphenyl bonded phases ; Retention and carbon content
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The relationship between the retention of PAHs having various molecular sizes and the carbon contents (%) of bonded stationary phases with various types of ligands were investigated. The examined stationary phases were phenyl, diphenyl, triphenyl and benzyl-bonded silicas. The data indicated that sometimes it is not true that the retention of any solute relates linearly to the carbon content of the stationary phase. As the result, it is suggested that the pore size distribution of the silica support, the bulkiness of the ligand bonded to the silica and the molecular size of solute should also be considered before any precise statement can be made.
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  • 17
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Metalloporphyrins ; 5,10,15,20-Tetraphenylporphine
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The Co(II), Ni(II), Fe(III) and V(IV) complexes of tetraphenylporphine (TPP) can be eluted at short retention times from a LiChrosorb RP-18 column with pure ethanol. However, both Mn(III) and Co(III) complexes of metal TPP chloride type are so strongly retained on the column that they cannot be eluted. While the retention of other metal teraphenylporphine complexes was not affected, that of the metal(III) complexes of the TPP chloride type especially MnTPPCl and CoTPPCl, decreases dramatically with an increase in the concentration of NH4Cl added into the mobile phase; a linear relationship between logk' and log[NH4Cl], with the slope of about−1, has been observed for these two metal(III) complexes in the NH4Cl concentration range from 2.5×10−4 to 1.3×10−2 mol/l. Thus, the specific control of the retention of the metal(III) complexes is enabled by conditioning the NH4Cl content of the mobile phase, and the chromatographic separation is demonstrated.
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  • 18
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 22 (1986), S. 55-58 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; 1-Octanol/water partition coefficient ; Cellulose acetate ; Reverse osmosis
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The adsorption properties of esters, aldehydes, ethers and amides on cellulose acetate, which is commonly used as a reverse osmosis membrane material, in an aqueous solution system were measured by high-performance liquid chromatography. The adsorption property was characterized with the specific retention volume. For a noncyclic homologous series the logarithm of the specific retention volume was linearly correlated with the logarithm of the partition coefficient between 1-octanol and water. The fact that the slopes of these regression lines are almost identical confirms that the dominant effect on adsorption is the hydrophobic interaction between cellulose acetate and the solute molecule. The intercept represents the effect of the polar groups on adsorption. The effect of the polar group decreases as follows: ―C(O)O―, ―CO―, HCON〈 〉 CH3CON〈 〉 ―OH, ―O―.
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  • 19
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 22 (1986), S. 77-80 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Dihydroartemisine ; Interconversion equilibrium ; Multiple-peaks
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The interconversion between the α- and β-isomers and the multiple-peaks of dihydroartemisinine (dihydroqinghaosu) were investigated in reversed-phase, highperformance liquid chromatography. A convenient method using the Gaussian distribution function instead of the Schmidt graphical method for the theoretical calculation of the “diffuse” probability curves versus the fraction of the dead time on column as β form was introduced. Based on the theoretical probability curves and the experimental multiple-peak chomatograms, the effects of temperature and flow velocity on the accuracy and precision of analysis of dihydroartemisinine are indicated and the activation energy of the interconversion between α- and β-isomers of dihydroartemisinine is estimated.
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  • 20
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 22 (1986), S. 99-102 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Nucleotides ; Mytilus edulis ; Smooth muscle
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A method is described for the analysis of the 5′ mono-, di- and triphosphates of adenosine, guanosine, uridine and cytidine, as well as uridinediphosphate-glucose and cyclic AMP. Separation is achieved by reversed-phase ion-pair chromatography with linear gradient elution. Application of this method to the analysis of nucleotides in smooth molluscan muscles is described, including the determination of cAMP-levels and the calculation of energy charges for all of the four nucleotide systems.
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  • 21
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Porphyrin ; Metalloporphyrin ; Hematoporphyrin IX
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The feasibility of reversed-phase high-performance liquid chromatography for the separation of metal complexes of hematoporphyrin IX (Hp) is described. The retention order, Zn-complex〈Hp (free acid)〈 Ni-complex〈Cu-complex, is regular on an octadecylbonded stationary phase with different compositions of an aqueous methanol mobile phase. These four compounds can be successfully separated within about 8 min on a LiChrosorb RP-18 column (250×4-mm i.d.) with a 85:15 (vol/vol) mixture of methanol and phosphate buffer (pH 3) at a flow rate of 1 ml/min.
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  • 22
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 22 (1986), S. 157-159 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Flavonol aglycones ; Isocratic elution ; Wine phenolics
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An HPLC isocratic elution procedure which allows the separation of flavonol aglycones in wine without interference from other phenolics of low molecular weight is described. The method has been applied to the separation, identification and quantitative estimation of flavonol aglycones in ether extracts of different Spanish wines (red and white table wines and Sherry finos). The results suggest that these determinations, associated with other analyses, would permit the chemical characterization of wines.
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  • 23
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 23 (1987), S. 796-802 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Steroids ; Rat tissue ; Purification by extraction
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A high-performance liquid chromatographic method for analysis of steroids in the tissue of laboratory animals is described. A two-stage solid extraction procedure, utilizing Sep-pak C18 and graphitized carbon black, gives a purified product. Steroids in this extract were separated by multistep gradient elution with a reversedphase liquid chromatography system, using acetonitrilewater as solvent. Several columns with different geometry and phase loading were investigated. Optimum resolution was obtained with a medium covered and spherical particle. The applicability of this method was successfully demonstrated in the analysis of the testis and adrenal gland of rat.
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  • 24
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 23 (1987), S. 814-817 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Thin layer chromatography ; Ammonium tungstophosphate ; Aminoacids
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The chromatographic behaviour of aminoacids on columns of silica coated with different percentages of ammonium tungstophosphate at several buffer phosphate concentrations is reported. The stationary phase shows a high selectivity towards aminobutyric acids and methyl derivatives of tryptophan due to the distance between the carboxylic group and the −NH 3 + group involved in the cation-exchange process and/or to the steric hindrance by a methyl substituent. A relationship between HPLC and HPTLC data has been verified and applied to the prediction of the separation of six aminoacids.
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  • 25
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 23 (1987), S. 934-938 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Calibration ; Confidence interval ; Limit of determination ; Limit of calibration
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary In HPLC calibration the expressions lowest calibration limit and determination limit are defined in statistical terms. The lowest calibration limit is the minimum mass in the measured series of calibration points. It is calculated from the confidence interval of the inverse of the calibration function as the lowest mass limit that may be differentiated from zero mass with a preset probability of error. If the calculated lowest calibration limit is lower than the actual data, points at lower concentration may be measured. The determination limit is the smallest concentration of an analysis that is differentiated from the concentration zero or an apparent blind value in the calibration curve with a given probability of error. Using two different UV-detectors (variable wavelength and photodiode-array) the lowest calibration limit is experimentally evaluated and compared with specific data for the detectors.
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  • 26
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    Digitale Medien
    Springer
    Chromatographia 18 (1984), S. 175-182 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Fourier transform IR ; Polar compounds ; Coal products
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Fourier-transform infrared spectrometry (FTIR) was utilized as a detection system for high-performance liquid chromatography of polar compounds on a normal bonded-phase system. In addition to FTIR, UV (254 nm) and refractive index detection were employed in the separation of model compounds containing oxygen and nitrogen atoms in their molecules (phenols, alcohols, neutral and weakly basic nitrogen compounds). A polar amino-cyano (PAC) bonded-phase column was employed with a binary mobile phase (98:2 CDCl3:CH3CN). The separations and the information gained from each detector is discussed, including interactions between sample material and mobile phase. A polar fraction of a coal-derived product is also chromatographed under identical conditions. The results based on FTIR detection and chromatographic retention behavior suggest the exclusive presence of hindered and unhindered phenols.
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  • 27
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 18 (1984), S. 211-215 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Alkylbenzenes ; PAHs ; Retention prediction ; Microcomputer
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The microcomputer-assisted retention prediction system in C18 reversed-phase HPLC is described. The system is based on the use of the hydrophobic parameter and the correlation factor of alkylbenzenes and polycyclic aromatic hydrocarbons (PAHs) which are highly correlated to their retention in reversed-phase HPLC. The system is evaluated by comparing the retention data between measured and predicted values. One of the typical examples applied for PAH analysis in the extracts of diesel particulate matter shows the high potential of the system investigated.
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  • 28
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 18 (1984), S. 216-220 
    ISSN: 1612-1112
    Schlagwort(e): Cation exchangers ; Column liquid chromatography ; Exchange capacity, determination ; Organic peroxidation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Two oxidation procedures for the synthesis of silicabased aliphatic sulfonic acid cation-exchangers for HPLC are described. Several reaction conditions for oxidizing a terminal-bonded thiol with organic peroxides are provided along with their yields, capacities, reproducibility, and chromatographic behavior. Also, three methods for determining exchange capacity are discussed, and their relationship to the capacity factors of charged solutes is compared. The maximum capacity determined by the titration of the bonded silica was 0.34 meq/gram. The general problems of synthesizing cation-exchangers, measuring their efficiencies and exchange capacities, and evaluating their overall performances are outlined.
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  • 29
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Pre-column derivatization ; Ultraviolet detector sensitivity ; Dihydroartemisinin ; Diacetyldihydrofluorescein
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The use of diacetyldihydrofluorescein (DADF) for derivatization of dihydroartemisinin (dihydroqinghaosu, DHQHS) is proposed. The reaction between DHQHS and this reagent in the presence of 4-dimethylaminopyridine (DMAP) and N,N′-dicyclohexylcarbodiimide (DCC) was complete in 8 hours at room temperature giving about 80 per cent theoretical yield. The derivative showed intense UV absorption, thus providing a sensitivity of 0.1 nanogram by UV detection after column separation. The influences of the ratio of the reagents, reaction temperature, chromatographic conditions and the extent of detection linearity were investigated. The reaction gave consistent results and chromatographic separation was not affected by an excess of the reagent or side products.
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  • 30
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 18 (1984), S. 369-373 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Ion exchange ; dynamic ; Metal ions ; Equilibria effects
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Equilibria occurring during the dynamic ion exchange separation of metal ions were examined, and their effect on the chromatography of the metal ions was evaluated. Bonded reversed-phase silica, pure organic reversed phase, and silica columns were used to differentiate between the role of silica and the reverse phase. The results show that system peaks had the most important influence on the applicability of dynamic exchangers to quantitative metal ion determinations. The response of system peaks to sample composition (pH, ionic strength, matrix effects) was complicated and could not be predicted easily. Equilibria effects that can cause analytical errors were identified and recommendations for elimination of such errors are given.
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  • 31
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Amines ; Phenols ; Fourier transform I.R.
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Several chromatographic parameters have been examined as to their effect on detectability for microbore high-performance liquid chromatography coupled with Fourier-transform infrared spectrometry. Detection limits for several compound classes are presented as amount injected. Improvements in detectability for this technique are discussed.
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  • 32
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Polystyrene packings ; Pre-column derivatization ; Thiamine compounds ; UV and fluorescence detection
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The chromatography of thiochrome and related phosphate esters was studied on two different polystyrene packing materials. The adsorbents were compared with respect to capacity factors, plate heights and resolution factors measured with different mixtures of phosphate buffer (pH 8.5) and methanol. In contrast with derivatized silica, these phases were found to be stable using an alkaline mobile phase and sample. Fast separations were possible with good peak symmetry at all organic modifier concentrations.
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  • 33
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 18 (1984), S. 445-448 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Amino-bonded stationary phase ; Ion-exchange ; Fermentation solution ; Biomass
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary In this work the analytical separation of biomass hydrolysis and fermentation products is described. Aminobonded phase and ion exchange materials (HPX 87H, HPX 42A, μ Spherogel Carbohydrate) were used as HPLC stationary phases for the determination of monomeric and oligomeric carbohydrates, carbohydrate degradation and fermentation products. The HPX 42A and the amino-bonded phase columns are especially suitable for the analysis of the gluco oligomers. The HPX 87H column separates the monomeric sugars and their degradation and fermentation products (e.g. furfurals and ethanol) very well. Using the μ Spherogel Carbohydrate column the lower gluco-oligomers as well as the monomeric sugars and their degradation and fermentation products, can be determined within 35 minutes.
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  • 34
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Chiral bonded phase ; Racemate resolution
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A chiral stationary phase with an immobilized, optically active diamine was prepared for the separation of enantiomers. The synthesis of the phase was carried out by bonding (−)trans-1,2-cyclohexanediamine to microparticulate silica gel through the coupling agent 3-glycidoxypropylsilane. The resolution of the racemic compounds catechin, 2,2′-dihydroxy-1,1′binaphthyl and trans-1,2-cyclohexandiol, is reported.
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  • 35
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 18 (1984), S. 495-498 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; PAHs ; Molecular shape recognition
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The molecular-shape recognition of polycyclic aromatic hydrocarbons has been studied on various stationary phases in reversed-phase high-performance liquid chromatography. The examined stationary phases were phenyl-, diphenyl-, triphenyl- and benzyl-bonded silicas. The results of regression analysis inidcated that triphenylsilica is the best packing material to recognize the difference in the molecular-shape of structural isomers. This fact was confirmed by the separation of 4-ring isomers.
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  • 36
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Retention data ; Substituted benzene derivatives ; Correlations
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The capacity factors of substituted benzene derivatives on bonded phases of various chain lengths in the reversed-phase mode have been measured and correlation of retention data between four stationary phases has been investigated by linear regression analysis. As a result, a difference in the retention mechanism between phases of shorter chain length and octadecylsilica was observed. In addition, it is also apparent that the multicombination treatment between retention data and descriptors such as π, HA, HD and σ promises the possibility of predicting the retention of substituted benzene derivatives on various reversed-phase stationary phases.
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  • 37
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 18 (1984), S. 525-527 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Polyamines ; Dansyl derivatives ; Peak compression
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Analytical conditions for the high-speed, reversed-phase, liquid chromatographic of a diamine (putrescine) and polyamines (spermine and spermidine) were determined. Various elution modes were employed using the same mobile phase constituents: 20mM sodium heptane sulfonate and 20mM acetic acid as solvent A and, pure acetonitrile as solvent B. Samples were derivatized with dansyl chloride before injection. Under isocratic conditions, the separation of the three polyamines was achieved in 7 min. The use of a linear elution gradient led to the same analytical time but with a better resolution of the putrescine peak from non-polyamine frontal peaks. For these measurements, the sample size was 5μl. This volume was increased to 20μl and the use of a steep gradient combined with the peak-compression technique allowed a fast analysis in 2–3 minutes, which may be compared with a 30 min run time necessary when a conventional column is used.
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  • 38
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 23 (1987), S. 395-400 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Photokinetic data ; Reaction mechanism ; (E)-1-phenylpropene
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A combined method of high-performance liquid chromatography and UV-absorption spectroscopy is described for use in dynamic systems. It provides a way of obtaining detailed mechanistic information as well as quantitative data (rate constants, quantum yields), even though neither mechanism nor photoproducts are known. The kinetic treatment of the photoreaction of (E)-1-phenylpropene was successful, showing a photo-isomerization and a parallel step. Information on this additional step is obtained by using HPLC to observe the changes in the concentrations of the reactants' selectivity. The necessity of process control is demonstrated.
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  • 39
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 23 (1987), S. 419-422 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Fatty acid esters ; Particulate material in seawater
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A method for the determination of fatty acids of the molecular weight range of propionic to erucic acid is reported. The acids are converted to either p-bromophenacyl-or p-phenylphenacylesters and the esters are separated by HPLC and detected by UV-absorption. Twentytwo esters, including saturated, monoolefinic and polyunsaturated ones were separated within one HPLC-run. The detection limit is about 5 pmol per fatty acid. The application of the method to particulate material is described.
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  • 40
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Anion-exchange stationary phases ; Polymer coating ; Cross-linking
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary PHEB=POLY(2-hydroxy, 3N-ethylenediamino)butadiene has been synthesized. This unsaturated pre-polymer can be immobilized on different, preferably inorganic supports of suitable porosity such as silica or alumina by cross-linking. Weak anion-exchange phase are obtained. Such phases do not have the disadvantages of organic polymeric phases, regarding pressure stability and swelling by solvent influence. The ion-exchange capacity and the retentivity of IE-separations can deliberately be varied via the thickness of the cross-linked polymer layer. Alumina can also be coated with PHEB applying the same cross-linking procedure. Such phases exhibit an exceptional chemical stability even when operated with mobile phases at very high pH-values. Separations of excellent selectivity are achieved for inorganic anions, as well as with mixtures of aliphatic and aromatic free acids also including hydroxy- (mono- or poly)carboxylic acids.
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  • 41
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Reversed-phase systems ; Stationary phase-solute interactions ; Polycyclic aromatics
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Capacity factors of peropyrene-type polycyclic aromatic hydrocarbons were measured using 15 different liquid chromatographic reversed phase systems. On the basis of the retention data the electric interaction indices have been calculated. Application of these indices for structure-retention studies on peropyrene-type polycyclic aromatic hydrocarbons is demonstrated.
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  • 42
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 31-36 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Radioactivity detector ; Solid scintillator ; Fibre-packed flow cells
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A new type of flow-cell radiation detector for use in liquid chromatography which is packed with aligned scintillator fibers is described. A primary advantage of the fiber packed cell is that light generated by the scintillator is absorbed to a much less extent by the fibers than by the powder scintillator used in conventional flow cells. A detection efficiency of 55% has been obtained for carbon-14 using 0.1-mm diameter hand-pulled glass fibers. Computer modeling has shown that even better results can be obtained by using smaller and more uniform diameter fibers which will allow better packing. The fiber cell also demonstrates back pressures which are a factor of 50 less than the conventional cell and much less susceptibility to absorption of compounds because of its lower surface area.
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  • 43
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 854-860 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Polystyrene ; Gradient elution ; Turbidimetry
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Polystyrene samples of narrow molecular-weight distribution have been eluted according to their molecular weight from columns packed with bare silica Si50, phenyl, or C18 bonded phase by gradients of methanol and tetrahydrofuran (THF) or ofiso-octane and THF. Among the six combinations investigated,iso-octane/THF with a silica column formed a proper normal-phase system whereas methanol/THF with a C18 column formed a proper reversed-phase system. The combinations of C18 column andiso-octane/THF or of Si50 column and methanol/THF gradient did not correspond to the approved polarity rules in high-performance liquid chromatography but were nevertheless effective in separating polystyrene mixtures by molecular weight. Methanol andiso-octane are nonsolvents for polystyrene whereas THF is a solvent. The solubility of polystyrene as a function of molecular weight and concentration was determined by means of turbidimetric titration of solutions in THF with the nonsolvents used in the gradients. The solubility and elution characteristics were almost identical on C18 columns or in methanol/THF combinations. The elution from phenyl bonded phase and Si50 columns usingiso-octane/THF gradients required more THF than the solubility experiments. Information is also given on the occurrence of multimodal elution patterns.
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  • 44
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 25-30 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Polycyclic aromatic compounds ; Alkylated PAC ; Retention characteristics ; Normal phase
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Retention characteristics of series of polymethyl and mono-n-alkyl derivatives of benzene and pyrene, and also of parent polycyclic aromatic hydrocarbons (PAH), were studied using silica and aminopropyl- and cyanopropyl-modified silica. Differences in the selectivities for the studied compound groups were found between the three phases. Deviations from linear behaviour in plots of log (k′)vs. carbon number were observed for the methyl series. These are explained in terms of differences in π-electron delocalisation within the aromatic ring systems. Further, the effect of methyl substitution on selectivity decreased with an increasing number of aromatic rings. Results were obtained which indicated that the primary adsorption site in a cyano column used in normal phase mode, at least for PAH molecules, is the cyano group.
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  • 45
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 43-50 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Reversed phase ; Void volume ; Adsorption isotherms
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary In reversed-phase liquid chromatography with n-alkyl bonded silica, the dead volume (V0) of the column is theoretically indeterminate owing to adsorption of organic modifier on n-alkyl chains and of water on silanol groups. With binary mobile phases, retention volumes of the mobile phase components and of their deuterated species are relaeed to the adsorption isotherms and V0 by equations which can be solved with some assumptions on the adsorbed layer composition. Methanol-water and acetonitrile-water systems are studied. As the experimental excess isotherm shows a linear part in the concentration range 50–80% in organic modifier, the hypothesis of an adsorbed layer of constant composition in this range is possible. When increasing the water content of the mobile phase, adsorption of water occurs up to saturation of silanol groups. Then the assumption of a constant water content for a mobile phase having more than 50% of water is applied. With the hypothesis of a constant adsorbed content of organic modifier when the eluent has more than 80% of organic modifier, V0 and the absolute isotherms are calculated over the entire range of mobile phase composition. Experimental retention behavior of the mobile phase components are totally explained by these V0 determinations. The retention times of commonly used V0 markers are compared with V0 values. It is shown that, when buffering the eluent, no visible effect on the distribution equilibrium is observed, so that injection of concentrated potassium nitrate is a convenient method to measure V0. With a few solutes with are UV detectable it is possible to measure V0 whatever the mobile phase composition in methanol-water and acetonitrile-water systems.
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  • 46
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Stationary phase solubility parameters ; Cyano-silica ; Amino-silica ; Diol-silica
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Extended solubility parameters have been determined for aminopropyl, cyanopropyl and 1,2-dihydroxypropyl propyl ether (diol) normal bonded-phase HPLC columns. Parameters were calculated from both the retention data of solutes (partition model) and empirically determined solvent strengths (adsorption-displacement model). The use of solvent strengths to calculate solubility parameters for these silica-based bonded stationary phases appears to be superior, since this technique avoids many of the problems that arise from their inherent heterogeneity. Normalized solubility parameters were also used to position these columns on a stationary phase selectivity triangle. The amino and cyano phases appear in regions of the tringle expected based on the properties of the pure liquids, but an ether linkage in the diol apparently neutralizes some of the acidity expected from this phase.
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  • 47
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 999-1003 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Macrolide antibiotic azithromycin ; Intermediates of azithromycin ; Optimization of separation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary HPLC is the most convenient method for the assay of the azithromycin (10-dihydro-10-deoxo-11-methyl-11-azaerythromycin A), a semisynthetic macrolide antibiotic and its reaction intermediates. Data concerning the effects of pH, temperature and column type are presented. The analytical procedures enabling the reliable assay of azithromycin and its intermediates, as well as other impurities are defined. Use of a reversed-phase octadecyl column, a pH of 9.3–9.5, and isocratic mode at ambient temperature are the best conditions of analysis.
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  • 48
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Metabolic disorders ; Xanthine and 2,8-dihydroxyadenine ; Urine analysis
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary 2,8-Dihydroxyadeninuria and xanthinuria are inborn enzyme disorders which must be under lifelong therapeutic control. Quantitative determination of 2,8-DHA and xanthine using reversed phase HPLC was performed. A new application for the separation of purines shortens analysis-time. Examples of the determination of 2,8-DHA and xanthine before and under certain therapies are shown. Long term monitoring of the patients offers the possibility of a reliable prophylaxis against stone recurrence.
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  • 49
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Indirect detection of non-electrolytes ; Simulation of induced peaks ; RP systems
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Induced peaks observed in indirect detection of nonelectrolytes in high-performance liquid chromatography are simulated. The equation representing the signal intensity of the induced peaks is derived, and it is verified by the experimental results. The peak area is proportional to (K b ′ +1) k a ′ /| a ′ —k b ′ |, where k a ′ ad k b ′ are the capacity factors of the visualization agent and the analyte, respectively.
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  • 50
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 162-166 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Ion chromatography ; Analysis of metal ions ; Post column derivatisation ; Amperometric detection
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A method for determination of metal ions subsequent to separation by ion chromatography has previously been developed. The method is based on Indirect Amperometric Detection whereby the decrease in the oxidation current, due to a dithiocarbamate ligand added post column, is monitored. Upon elution from the chromatographic column the metal ions are complexed by the ligand. As the complexes formed are electroinactive at the applied potential, the background current decreases according to the metal ion concentration. The method developed in this work involves addition to the reagent of Zn(II) as a auxiliary metal ion to displace the analyte metals from the chromatographic eluent ligand complexes after separation. Sodium bis(2-hydroxy-ethyl) dithiocarbamate was used as the postcolumn derivatising reagent. The addition of Zn(II) to the reagent causes some unforeseen behaviour in the chromatographic system.
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  • 51
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 199-204 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Column switching ; Catecholamines ; Urine ; Serum
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary We developed an automated, two-column HPLC-method that can be used routinely to quantify the catecholamines norepinephrine and epinephrine in body fluids. The method is based on a new, laboratory-prepared SEC-HPAC column material, on the application of a microprocessor-controlled column-switching technique, and on the use of an integrated reaction system for postcolumn derivatization and trihydroxyindol-fluorescence monitoring. It allows the direct injection (upto 500 μl) of an appropriate biological fluid and distinguishes on its integrated sample-processing mode, its practicability, its chemoselectivity and-specivity, its detection limit (2 pg), its within- and between-run precision and its speed of analysis.
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  • 52
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 319-323 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Pheophytinatonicke(II) ; Chlorophyll ; Pheophytin
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary HPLC determination of pheophytinatonicke(II) (Pheo-Ni) prepared by the replacement of magnesium(II) in chlorophyll with nicke(II) is described. The good separation of PheoNi was obtained by using chemically bonded C18 as the stationary phase and acetone-methanol (50∶50, vol/vol) as the mobile phase. Conventional spectrophotometric method was also used for the determination of PheoNi. For the synthetic samples prepared by mixing (pheophytinato a) nicke(II) [(Pheo-a) Ni] and (pheophytinato b) nicke(II) [(Pheo-b) Ni], analytical values obtained by the spectrophotometric method were very high compared to those obtained by HPLC. In the proposed HPLC method, (Pheo-a) Ni and (Pheo-b). Ni could be determined in the concentration range of 0.028–30μg/ml and 0.038–30μg/ml with relative standard deviations (n=10) of 3.1% and 0.8%, respectively.
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  • 53
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Flavonoid compounds ; Structure-retention relationships ; Reversed-phase systems
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Reversed-phase HPLC retention behaviour of different flavonoid compounds in different columns and with a range of methanol-buffer eluents was examined. Repeatibility and reproducibility of logk′ and Δlogk′ values were analyzed. Sharp group contributions, expressed as Δlogk′, were observed. These did not depend significantly on acid modifier type, column packing characteristics (C8 and C18) and dimensions (5,7 and 10μm) or the percentage of methanol in the mobile phase. A list of twelve group contributions is presented which is in agreement with literature data.
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  • 54
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 443-446 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Large scale separations ; Dissolution of silica ; Metallic contaminants
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Possible contamination of purified product by the silica matrix is of considerable importance when considering process scale high-performance liquid chromatography (HPLC) as a separation methodology. The stability of silica supports in normal phase, reversed phase and affinity chromatography modes has been examined with organic solvents and water. Both inorganic and organic components were found, contributed by the support, and the chromatographic and distillation equipment. In all cases, based on assumed values of production, they were found to contribute less than 0.01% of impurities. In critical cases crystallisation or dialysis may be considered as a last stage of purification, with re-chromatography to maximise yields.
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  • 55
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 523-525 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Fast atom bombardment mass spectrometry ; Nonionic detergents
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Microcolumn liquid chromatography (LC) combined with fast-atom-bombardment mass spectrometry (FABMS) was applied to the analysis of nonionic detergents. The porous silver filter attached to the top of the capillary fused-silica tubing worked as the interface for coupling of micro LC and FABMS.
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  • 56
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 577-581 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Process scale ; Examples of separations
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The flexibility of process scale high performance liquid chromatography is demonstrated by three examples of reversed-phase separations (a) a standard purification (b) isolation of trace compounds, and (c) recovery from crystallisation mother liquors. It was shown that a material, thought to be acceptably pure, contained a toxic impurity, and a remaining impurity, a previously unseen component of potential therapeutic interest. Favourable cost data were indicated for example (3).
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  • 57
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Benzidine+diaminodiphenyl methane derivatives ; Preconcentration from urine ; UV and electrochemical detection
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary For the title compounds 4,4′-DADPM, MOCA, 3,3′-DCB, 4-ADP and 4-ADPA listing on the EPA priority pollutant list, an analytical practicable, reliable, reproducible and sensitive procedure is required. Therefore a new method has been developed for the routine determination of these toxic aromatic amines in urine at the ppb level. The quantitative determination of amines is a suitable procedure of occupationally exposed persons. Urine sample preparation is done using simple liquid-liquid extraction followed by a precolumn enrichment (PRP1-material; Hamilton). Breakthrough measurements were done using an enrichment column packed with PRP1 material. The capacities of the studied amines ranged from 21.9mg/g to 96.6mg/g, while influent concentrations differed from 28.3mg/l to 332.0mg/l. The advantages of electrochemical detection regarding to selectivity and sensitivity are clearly indicated in this paper. Separation has been achieved applying reversed-phase-high-performance-liquid chromatography (LiChrosorb RP 18/5μm) followed by electrochemical or UV-detection. The detection limits employing an electrochemical detector at a potential of 1 V range from 2.2ng to 12.1ng. UV detection at 254 nm and 280 nm is about 10–100 times less sensitive. Recoveries from spiked water samples at the 5ppb levels were 75% to 96% respectively. The standard deviation of the developed procedure varies from 5.3% to 14%. Day-to-day repeatability is good.
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  • 58
    ISSN: 1612-1112
    Schlagwort(e): Thin layer chromatography ; Column liquid chromatography ; 21H, 23H-Porphine ; Metalloporphyrin complexes
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The chromatographic mobility of 21H, 23H-porphine and its Ni(II), Cu(II), Zn(II) and Pd(II) complexes were investigated by high-performance thin-layer chromatography on an octadecyl-bonded, silica gel plate with various polar organic solvents including alcohols, acetonitrile, dimethylsulfoxide and propylenecarbonate. The mobility generally decreases according to the central metal ion of the complex as follows: Zn(II)〉(free porphine)〉Ni(II)〉Pd(II)〉Cu(II). Methanol is a good choice of solvent for the separation of these metal porphine complexes. Successful separation of porphine and the four metal complexes is accomplished within 13 min on a LiChrosorb RP-18 column with methanol eluent.
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  • 59
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 717-720 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Reversed-phase chromtography ; Antifungla agent ; Pharmacokinetics
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A high-performance liqid chromatographic method is reported for the measurement of miconazole in systemic, fungal infectious patients. Pharmacokinetic data are presented for a single patient receiving miconazole therapy. Sample preparation involves protein precipitation by acetonitrile (1:1, vol/vol). Analyses are carried out on a reversed-phae chromatographic system using octadecylsilane stationary phase: a mobile phase consisting of 0.05 M acetate buffer (pH 7.4)acetonitrile (20:80, vol/vol) is used to elaute miconazole is quantified on the basis of ultraviolet absorption at 220 nm. The precision of the method ranged from 3.21% at 0.5 mg/L to 0.85% at 2.0 mg/L. The limit of quantification was established as 0.1 mg/L. Interference from other drugs that are co-adimistered such as amphotericin B, 5-fluorocytosine of ketoconazole and most other comonly encountered drugs was not observed.
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  • 60
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Mobile phase composition and column temperature ; Retention prediction ; Polycyclic aromatic hydrocarbons
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The relationship between the logarithmic capacity factor measured in reversed-phase liquid chromatography and the operating conditions including the mobile phase composition and the column temperature is investigated. The strategy described herein can offer the possibility to predict the retention of polycyclic aromatic hydrocarbons without any experiments and standard materials, by utilizing equations describing the relationships between retention, temperature, mobile phase composition and physicochemical properties of the solutes previously stored in the program of the microcomputer-assisted retention prediction system. This concept is one of the most promising techniques for the optimization of the separation conditions in reversed-phase liquid chromatography.
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  • 61
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Fractional factorial experimental designs ; Ruggedness test ; Method validation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Recently much attention has been directed to the validation of analytical methods. The level of validation will depend on the method application. If a method is developed for general use, for instance by different analysts, instruments or laboratories, then the effect of these changes need evaluation. This is normally referred to as ruggedness testing, where the limitations of the method to changes in the specified conditions are examined. This paper examines the use of Plackett-Burman fractional factorial experiment designs for ruggedness testing in high performance liquid chromatography (HPLC). The ability of these designs to identify confounding effects is applied to the stability indicating analysis of Salbutamol and its major degradation product, AH4045. The results show that confounding effects, proving extremely pertinent to HPLC, can be identified. The assay proved rugged to most tested changes although not to the use of column packing material from different manufacturers.
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  • 62
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 22 (1986), S. 231-234 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Post-column reactor ; Crosheted PTFE construction ; Photochemical reaction detection
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Construction of crocheted photochemical reactors for use in high performance liquid chromatography is described. The design of these reactors is optimal for low intensity light sources because of their cylindrical configuration. Band broadening is minimized by the use of tightly crocheted narrow bore tubing and fittings modified to reduce dead volume. These reactors are suitable for most post-column photochemical reactions with the additional possibility of serving as mixing/delay coils, deoxygenation devices for electrochemical detectors, and as low dispersion detector cells for chemiluminesckent reactions.
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  • 63
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 23 (1987), S. 31-32 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Gonadal steroids ; Epimers
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Chromatographic separation of biologically active epimeric steroids was carried out using a combination of normal and reversed phases. Testosterone (17β-OH) was separated from its 17α-OH epimer epitestosterone using a normal phase silica column whereas their reduced 5α-metabolites were separated on a reversed phase system. The separation of other gonadal steroids including the epimers 20α- and 20β-hydroxypregn-4-en-3-one is also discussed. The technique is particularly useful for separating mixtures of naturally occurring steroid epimers prior to radioimmunoassay.
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  • 64
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Ammonium acetate buffer eluent ; Chlorophylls and degradation products ; Marine phytoplankton
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An RP-HPLC procedure which separates chlorophylls and their degradation products is described. By employing an amonium acetate buffered mobile phase and a linear gradient elution, complex mixtures of chloroand phaeopigments are separated in less than 30 minutes. The method has been applied to the control of chlorophyll enzymatic degradation in cultures of two algal species, and has also been successfully used in the analysis of algal xanthophylls.
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  • 65
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Alkyl-bonded phases ; Retention behaviour ; Ligand density ; n-alkyl chain length
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Two series of bonded phases were synthesized employing LiChrospher Si 100, 10 μm and n-alkyldimethylmonochlorosilanes as silanizing reagents. In series A the n-alkyl chain length, n, of the bonded phase was varied between 1 and 20 at a constant ligand density of 3.5±0.2μmol·m−2. In series B the ligand density, d, was gradually changed from 0 to 4.1μmol·m−2 on the C1, C4, C6, C8 and C18 bonded phases, respectively. The capacity factors of benzoic acid esters and anilines as solutes were found to increase linearly with the n-alkyl chain length of packings at constant eluent composition (series A) up to a so-called critical chain length, ncrit, where the capacity factor remained constant. ncrit was in the range from 11 to 14. The same pattern was observed when plotting the solute capacity factor against the ligand density of the packing at constant n and constant eluent composition (series B). The critical ligand density, αcrit, varied between 2.3 and 3.2 μmol·m−2 depending on n and the solute. Furthermore, solute retention was slightly higher on RP packings with an even number of carbon atoms in the alkyl chain than on those with an odd number. These findings are consistent with the results of Berendsen and de Galan (J. Chromatogr., 196, 21 (1980)), Dill (J. Phys. Chem., 91, 1980 (1987)) and Simpson and Lau (to be published). The observed phenomena reflect the dynamic structure of RP silicas which are related to the mobility of solvated n-alkyl chains. Due to the lack of a precise conformational analysis of the surface of RP silicas, a semiquantitative model was applied to interprete the described dependencies.
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  • 66
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Behaviour of metal complexes ; Solvophobic theory
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The chromatographic behaviour of Cu(II), Fe(II), Ni(II) and Co(II) complexes with 4-(2-pyridylazo)resorcinol was studied. The experimental results were very sensitive even to less obvious operational parameters like the kind of the cation (sodium or ammonium) of the phosphate salt used as buffer. The puzzling pattern of the data obtained was interpreted in terms of the equations formulated by Horvath's ‘olvophobic” theory which correlates the capacity factors of the solutes with the surface tension of the mobile phase. A satisfactory rationalization of the data was obtained together with qualitative information on the stoichiometry and charge state of metal complexes. Useful suggestions about the direction to address the experimental work in order to obtain the best results was also obtained.
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  • 67
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Ligand Exchange ; Diethylenetriaminepentaacetic acid ; Transition metal ion separation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Basic alumina-bonded diethylenetriaminepentaacetic acid (DTPA) has been utilized for the separation and preconcentration of some transition metal ions on the basis of ligand exchange. Breakthrough capacity and rate of sorption have been studied. The distribution coefficients of 16 transition metal ions have been determined in demineralized water, 0.01 M sodium citrate and in four different pH systems. On the basis of differences in Kd values some quantitative separations of metal ions have been achieved. The greater selectivity behaviour (higher Kd values) of the adsorbent for Pt(IV)and Cr(III) has been utilized for their preconcentration in the presence of other metal ions. The method has been employed for the recovery of Pt(IV) and Cr(III) from tapwater and sea-water samples.
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  • 68
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Gel permeation chromatography ; Cheese peptides ; Amino acids
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The nitrogen fraction from cheese, soluble in phosphotungstic acid has been analyzed by gel permeation and high performance liquid chromatography. Elution profiles of this fraction on Sephadex G-10 show that there are no peptides of molecular weight higher than 700 daltons. Six fractions have been obtained. The first one has the peptides and some amino acids. Fractions II to VI contains mostly free amino acids. Fraction I has been separated into many peaks by HPLC. Six or seven of these peaks are presumed to correspond to peptides.
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  • 69
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Small-bore packed columns ; Air pollutants ; PAH, nitro and oxy-PAH ; Aldehydes
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The preparation of small bore columns (1 mm i.d.) packed with reversed-phase materials is described. High efficiency (Hmin=2 dp), coupled with a small C term (0.005 sec) have been obtained so that high speed can be combined with sufficient resolution for the separation of complex organic mixtures. These columns have been used for the separation of air pollutants dispersed in different matrices (air, particulate matter and rain water). Practical applications include the determination of aldehydes in air and emission samples, PAHs, nitrated and oxygenated PAHs in dust sampled from the stack of an industrial emission or collected in a urban area and the analysis of organic components dissolved in rain water collected at a rural site. Specific detection of these pollutants has been achieved by connecting small bore columns to UV absorbance, voltammetric and fluorimetric detectors. Mass spectra of some specific components have been recorded using the off-line technique.
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  • 70
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 23 (1987), S. 825-828 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Gasoline ; Single-ring aromatic hydrocarbons ; Polycyclic aromatic hydrocarbons
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary This work reports a rapid and easy procedure for the analysis of the aromatic fraction in gasoline. No sample pretreatment is required, since the gasoline is diluted in methanol and directly injected into a liquid chromatograph. A spectrophotometer detector and a spectrofluorimeter detector are used in series. The procedure has been applied to a large number of Italian and European refined gasoline samples.
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  • 71
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 27 (1989), S. 27-30 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; 1,ω-Di(alkoxy)-polysulphides ; Retention contributions
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The reaction of S2Cl2 with alcohols yields products, the reversed-phase liquid chromatograms of which are similar to those of dialkyl-polysulphides RSnR, i.e., they represent homologous series. Four of the products were identified via GC-MS as 1,ω-di(alkoxy)-polysulphides having the general structure ROSnOR. Retention contributions of alkyl groups R and sulphur atoms in the −Sn — chain are not much different from values observed with polysulphides. The effect of oxygen, however, is only about −100 index units per O atom, while in dialkyl ethers values of −500 units have been reported.
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  • 72
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 27 (1989), S. 5-14 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Retention behaviour ; Column parameters
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Retention of small molecules on reversed phase or other hydrophobic stationary phases can be represented by k′ values of members of a homologous series at varying solvent compositions. The evaluation of simple linear relationships leads to the introduction of a set of four parameters that contain all the information about retention behaviour of this homologous series in the binary solvent system chosen. It is possible to extrapolate to a hypothetical non-hydrophobic molecule and a solvent, the polarity of which equals that of the stationary phase, to characterize the properties of the stationary phase — eluent system. In addition, a chromatographic method for determination of the phase ratio of the column is proposed.
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  • 73
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 23 (1987), S. 109-111 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Normal and reverse phase ; Aldicarb ; Aldicarb sulfoxide ; Aldicarb sulfone
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Aldicarb, aldicarb sulfoxide, and aldicarb sulfone were chromatographed on an octyl-silica bonded-phase column and on an unmodified silica column using acetonitrile/water mobile phases. The elution order of the analytes from the silica column was different from that using the octyl-silica bonded phase and allowed confirmation of residues of aldicarb sulfoxide in citrus nectar. Isocratic elution of the unmodified silica column allowed rapid sample throughput.
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  • 74
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 23 (1987), S. 118-120 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Ligand-exchange chromatography ; Chiral bonded phase ; Racemate resolution ; Amino acids
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The resolution of racemates on chiral chemically bonded silica gel by high-performance ligand-exchange chromatography is described. The stationary phase was prepared by bonding (−) trans 1,2 cyclohexanediamine to silica gel through the coupling agent 3-glycidoxypropyl silane. The resolution of several α-amino acids and of compounds of pharmaceutical interest is reported.
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  • 75
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Anion exchange separation ; Preparative separations ; Human chorionic gonadotropin hormone
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A high-performance liquid chromatography (HPLC) method was developed for the purification of 50mg crude human chorionic gonadotropin (HCG) hormone sample in one chromatographic run on a 250×10 mm SERVA DEAE Poliol-Si-500 column. During the 60-minute linear gradient of 0.05 M sodium sulfate, 0.05 M sodium hydrogen sulfate and 0.05% (v/v) acetonitrile in buffer “B” complete separation was accomplished in 40 min. Identity and purity of the fractions were checked by SDS electrophoretic method. The eluted HCG fractions were dialyzed for 24 hours to remove the buffer salts and liophilized. The activity of the hormone did not decreased significantly during the purification procedure.
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  • 76
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Bovine milk ; Multivariate optimization ; Glycerophospholipids ; Molecular species separation ; Chemometrics
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The molecular species profile, representing the fatty acid combinations on the glycerol backbone, is the most fundamental description of an intact glycerophospholipid class and provides a key to understanding its functional characteristics. We have developed a powerful RP-HPLC method for the separation of molecular species, including so-called “critical pairs”, of natural mixtures of 1,2-diacyl-sn-glycero-3-phosphocholine 1,2-diacyl-sn-glycero-3-phosphoethanolamine from bovine milk and other natural sources. We have used a novel multivariate development and optimization strategy to locate the region of optimum separation conditions within a prechosen domain of the chromatographic parameter space.
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  • 77
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Open tubular columns ; Cross-linked polyacrylate stationary phase ; Photopolymerization ; Antracene derivatives
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Polyacrylate films containing a lauryl moiety were fabricated on about 12 μm I.D. fused silica capillaries by in-situ photopolymerization of acrylates. Relatively thick films up to 1 μm were obtained by the technique. The films were tested as retentive layers for reversed phase open tubular liquid chromatography (OTLC). Due to the presence of the incorporated lauryl moiety in the layer considerable retention could be achieved for polar compounds with aqueous mobile phases. The efficiency of the prepared columns approximates to the theoretical value. The polyacrylate films appear to be extremely stable even under strong basic conditions. The films swell considerably in the presence of nonpolar solvents resulting in more favourable retention and a significant improvement of the chromatographic performance.
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  • 78
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 35 (1993), S. 627-630 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Fatty acid analysis ; Fish oils
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A chromatographic method has been developed for the determination of eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) in fish oil dietary supplements containing triglycerides rich in (n−3) polyunsaturated fatty acids (PUFAs). Following the ester saponification, free fatty acids were resolved by TLC into two fractions: i) a more mobile group of saturated and monounsaturated fatty acids and ii) a less mobile group containing PUFAs. The PUFA fraction was further analyzed by HPLC to determine the levels of EPA and DHA in the fish oil sample.
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  • 79
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Carbidopa and levodopa in plasma ; Electrochemical detection
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A validated reversed-phase high-performance liquid chromatographic procedure employing electrochemical detection (LCEC) for the analysis of carbidopa and levodopa in human plasma is reported. The method is sensitive and specific with amperometric detection at a glassy carbon working electrode with Eapp=0.75 V vs. Ag/AgCl. The retention times of levodopa, internal standard, and carbidopa are 3.3, 4.5, and 9.7 minutes, respectively, with an overall chromatographic run time of 12.0 minutes. The peak height ratio versus plasma concentration is linear over the range of 5.0 to 500 ng/mL for each analyte and exhibits correlation coefficients of 0.9957 or better (n=9). The mean absolute recovery of carbidopa and levodopa using the described assay is 36.6 and 66.0%, respectively. The inter- and intra-day accuracy and precision are within 11.8% of the actual values for all concentrations. Also, due to the demonstrated instability of carbidopa and levodopa in plasma a procedure is provided to circumvent this. Blood collected in pre-treated Vacutainer tubes can be stored in an ice bath for up to 4 hours without any significant degradation, thereby providing a practical means for processing several clinical samples simultaneously.
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  • 80
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Fullerenes ; FullereneSep® ; Separation factor ; HPLC-particle beam mass spectrometry
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary High-performance liquid chromatographic separation of fullerene mixtures in the range C60 to C100 can be achieved using a novel stationary phase which rivals the performance of the more expensive ‘Pirkle-type’ columns currently employed.
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  • 81
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 35 (1993), S. 675-678 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Ion chromatography ; Trace metal determination ; Sample contamination ; Human hair
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The dynamic ion-exchange chromatographic analysis of bivalent ions, such as Cu, Pb, Zn, Ni, Co and Mn in resistant organic matrices needs preliminary wet ashing with oxidizing acids (HNO3 and HClO4). Such treatment may lead to an increase in the amounts of metals present in the sample due to their release from containers or equipment used in an acidic environment and to metal impurities contained in the acids. The effect of these interferences in the determination of trace metals in human hair was studied.
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  • 82
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 32 (1991), S. 334-340 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Normal phase separations ; Cyanopropyldimethyl silica ; Chloro-added polycyclic aromatic hydrocarbons ; Environmental samples
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Retention characteristics in normal phase HPLC of highly biologically active chloro-added polycyclic aromatic hydrocarbons (PAHs) were studied. Silica, cyanopropyldimethylsilyl- and aminopropylsilyl- modified stationary phases were investigated. Retention properties of chloroadded PAHs on these phases were shown to be strongly influenced by the number of chloro-additions. This is due to the strong polarity of the methylene carbon at the chloro-addition site. Active silica had a strongly degrading effect on the unstable chloro-added PAHs during separation. Aminopropylsilica did not exhibit sufficient selectivity towards chloro-added PAHs when compared to chlorosubstituted PAHs. Cyanopropyldimethylsilica was shown to be applicable to a group separation of chloro-added and chloro-substituted PAHs. A fast clean-up procedure for chloro-added PAHs in complex samplesis outlined. It involves an initial elimination of more polar substances on a short open column with strongly deactivated silica and a subsequent separation on a cyanopropyldimethylsilyl HPLC column in normal phase mode.
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  • 83
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 32 (1991), S. 345-349 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Column packings ; Pore size distribution ; Diffusion and adsorption ; Band broadening
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The complex intraparticle structure typical of chromatographic column packings has been analyzed by use of an equivalent network model which emphasizes pore size distribution and connectivity. Special attention is given as to the way in which diffusion and adsorption interact and display modified peak spreading characteristics according to the morphology of the pore space. This study reveals a very significant increase in the column band broadening over that expected from physical adsorption which can arise from particular distributions of pore sizes. This has implications for designing packings which take advantage of the separating power due to adsorption but do not compromise the resolution of the chromatographic system.
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  • 84
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; GC/ECD detection ; PCBs, ortho and non-ortho ; Chromatographic separation ; Congener determination ; FTIR identification
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An analytical procedure for the individual determination of ortho and non-ortho PCB congeners in sediments, using high performance liquid chromatography (HPLC) preseparation and gas chromatography/ECD detection, is described. Gas chromatography/FTIR spectrometry (GC/FTIR) and gas chromatography/mass spectrometry (GC/MS) were employed for individual congener identification and determination. Sample extraction, clean-up of extract and selective elution procedures were optimized by using reference certified marine sediment samples. Recovery and precision were typically 83% and 16% respectively at 2 ng/g of total PCB content. The proposed procedure, tested by analyzing real sediment samples, showed a reproducibility better than 20% at 13 ng/g PCB level.
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  • 85
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Glutamine ; Pyroglutamic acid ; Amino acids formulations
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The aminoacid glutamine in aqueous solution and in conditions of high temperature and long term storage is partly transformed into pyroglutamic acid which exhibits potential neurotoxic effects. Commercially available aminoacid mixtures supplemented with glutamine are heat-sterilized and some losses of glutamine and formation of pyroglutamic acid may occur. The aim of the work was to set up an easy and reliable HPLC method which allows the determination of pyroglutamic acid as a degradation product of glutamine. The column was a 5 μm Hypersil ODS (100×4.6 mm) and the mobile phase 100% 0.007 M phosphate buffer pH 3.5. Stability studies in different conditions of temperature and time of storage were performed on aminoacid mixture available in the commerce.
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  • 86
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Carbonyl compounds ; Luminarin hydrazides ; Fluorescence detection
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Fluorogenic reagents (luminarin 3, luminarin 11 and luminarin 12), having a quinolizinocoumarin moiety as fluorophore and a carboxylic acid hydrazide function as reacting group, have been developed. These reagents were found to be highly sensitive fluorescence derivatization reagents for aldehydes and ketones in high-performance liquid chromatography. The reagents readily react with carbonyl compounds in aqueous sulphuric acid solution (0.1 M) at room temperature to produce the corresponding hydrazone derivatives, which can be separated on both reversed or normal-phase column. The structures of the derivatives were studied, together with their properties in reversed and normalphase chromatographic systems. UV absorbance, corrected fluorescence spectral data and quantum yields of luminarin 3, luminarin 11 and luminarin 12 are presented. The detection limits (signal to noise ratio=3) for aldehydes and ketones were in the sub-pmol range. Luminarin 3 was also applied to the determination of hydroxymethylfurfural (HMF) in orange juices and concentrates. The method for HMF involves the solid-liquid extraction of the juice by using a C-18 cartridge prior to derivatization and normal-phase separation of the derivative with fluorimetric detection at 387 nmex., 444 nm em. The calibration curve was linear for amounts of HMF ranging from 0.1 to 10 nmol. Intrarun relative standard deviation was 12.8% for 0.1 nmol and 2.6% for 1 nmol. Recovery studies indicated an average of 98.7±1.9% for juice concentrate and 99.8±3.2% for pasteurized juice.
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  • 87
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Method development ; Chemometrics ; Response criteria ; Analysis of drug purity
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Optimization procedures require adequate response criteria to assess the quality of each chromatogram obtained during the process. The objective of this paper is to evaluate the possibility of using different resolution functions, in the chromatographic separation of a drug and its impurities (particularly the impurity just eluted after the drug). This study shows the limits of some resolution expressions. The interest of the simple Δt criterion, the difference between retention times, is presented in this paper.
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  • 88
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 36 (1993), S. 147-151 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Polarity ; Retinoids
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The retention of retinoids in reversed-phase liquid chromatography was studied using aqueous mobile phases of different composition (methanol 94–86% and acetonityrile 92–82%) at five temperatures (40–60 °C). With both organic modifiers the effect of the molecular structure increased as the water content and the polarity of the mobile phase increased. The temperature-dependence increased in the same manner with aqueous acetonitrile mobile phases. The π-π interactions between the retinoids and acetonitrile diminish when the water content of the mobile phase is increased, as happens also to the hydrophobic interactions with both organic modifiers. The net effect of these changes depends on the composition of the mobile phase. There was excellent correlation of retention with all polarity parameters studied(ϕ, P′, xe, xd, xn, E T N , δT, δ, δo and δd), when the calculations were made separately with methanol and acetonitrile. The volume fraction of the organic modifier, ϕ, was the only parameter describing the retention well in both organic modifiers simultaneously.
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  • 89
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Aromatic amines ; Arylbenzylamide methylthioether derivative ; SL 85.1016 ; Pharmacokinetics
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An HPLC method has been developed for the determination of SL 85.1016, a new calcium antagonist arylbenzylamide methylthioether derivative. SL 85.1016 and the internal standard, SL 87.0210, are extracted from alkaline human plasma withn-hexane and back extracted into 0.05 M phosphate buffer (pH 2.5; 0.2 ml). Acetonitrile (50 μl) is added to the final aqueous extract in order to prevent absorption of the compounds of interest onto the walls of the glass tube; this solution then is partially processed by HPLC on a C18 column with UV detection (254 nm). The determination limit of the method is 2 ng.ml−1 of SL 85.1016 in human plasma; the response to the drug is linear in the range 2–200 ng.mg−1.
    Materialart: Digitale Medien
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  • 90
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 36 (1993), S. 347-350 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Allium ; Derivatization ; S-alk(en)yl-L-cysteine sulfoxides ; Sulfur amino acids
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Two pre-column derivatization procedures coupled with reversed phase HPLC have been compared for the analysis ofS-Alk(en)yl0L-cysteine sulfoxides in variousAllium species. In order to establish external standards some (+/-) sulfoxides were synthesized, using a new method to enhance asymmetric synthesis of the diastereoisomers. The first derivatization method is the formation ofo-phthaldialdehyde/tert.-butylthiol derivatives which can be analyzed using UV detection. The second, presently used for amino acid analysis, is the Waters Pico-Tag method, which employs phenylisothiocyanate as derivatization reagent. As the Pico-Tag method was found to be the most efficient for determination ofS-alk(en)yl-L-cysteine sulfoxides it was used to determine the alliin content of various samples of garlic.
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  • 91
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 33 (1992), S. 13-18 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Fatty acids and bile acids ; Fluorogenic precolumn derivatization ; 2-Bromoacetyl-6-methoxynaphthalene
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The use of 2-bromoacetyl-6-methoxynaphthalene as a fluorogenic labelling reagent in pre-column derivatization for the HPLC separation of biologically active carboxylic acids (fatty acids and bile acids) has been investigated. The compound reacts (30 min. at 70°C) with carboxylic acids to give fluorescent esters that can be separated by reversedphase HPLC and detected at λ ex. 300 nm, λ em. 460 nm. The experimental conditions for the derivatization and chromatographic separation are discussed. Applications to the determination of valproic acid and chenodeoxycholic acid in pharmaceutical formulations are described.
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  • 92
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Valproic acid ; Simultaneous determination of anticonvulsants
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The derivatizing procedure of Moody et al. [20] for valproic acid has been simplified and applied to the simultaneous HPLC determination of valproic acid (VPA), barbital (B), primidone (PRM), phenobarbital (PB) and carbamazepine (CBZ) in serum or plasma of epileptic patients. The sample is deproteinized with acetonitrile containing esterification agents and an aliquot of the supernatant is heated to 70°C for 15 min with 4-bromophenacyl bromide. The reaction mixture is analysed on a C18 column at ambient temperature, with gradient elution and with detection at 205 nm. The time required for the chromatographic analysis is 13 min; identification is based on retention time and quantification is by peak area determination with an internal standard. The calibration curves show good linearity in the range 6.25 to 100 mg/L. The detection limits at a signal: noise ratio ≥3, ranged from 1 mg/L for B and CBZ to 2–3 mg/L for PRM, PB and VPA. The method described for the simultaneous determination of the five drugs in the same plasma pool, correlated well with isocratic HPLC methods specific for each drug. The simultaneous procedure described allows a reproducible (CVs≤6.5% within run) and rapid (25 min for sample preparation: 13 min for chromatographic run) therapeutic monitoring of patients treated with VPA and two or more antiepileptic drugs.
    Materialart: Digitale Medien
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  • 93
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 33 (1992), S. 19-24 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Porous polymer spherical packings ; Vinyl ether ; Alkali resistance ; No abnormal adsorption
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Spherical, porous-polymer particles for column packing in high-performance liquid chromatography were prepared by suspension copolymerization of alkylvinyl ether with triethyleneglycol divinyl ether. The hydrophobicity of the packings was easily adjusted by changing the monomer ratio. The packings showed the usual reversed-phase liquid chromatographic properties, but did not sho abnormal retention, tailing and broadening of peaks and irreversible adsorption of ionic and aromatic substances, owing to the lack of ionic or aromatic groups. In addition, the packings were stable in alkaline solutions because of the relative alkali stability of C−O−C bonds as compared with CO−O and Si−O−C bonds in conventional packings.
    Materialart: Digitale Medien
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  • 94
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Anion exchange ; Indirect photometric and direct conductivity detection ; Naphthalenesulfonate ; Inorganic anions
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Indirect photometric and unsuppressed direct conductivity detection modes are examined using naphthalene mono-, di-, and tri-sulfonate as mobile phases for the separation of several anions such as F−, Cl−, NO2 −, Br−, NO3 −, SO4=,I−, and SCN− using a commercial anion exchange column. With all three mobile phases, conductivity detection shows better sensitivities and detection limits than indirect photometry. Conductivity detection is 5 to 16 times more sensitive than indirect photometry for all analytes. Detection limits achieved using these mobile phases are, for example, 0.04 ng and 0.1 ng for chloride ion with conductivity and indirect photometry, respectively. Both detection modes give wide linear ranges extending from at least 100 ppm to the detection limit of each anion which is generally about 0.02 ppm. Sulfur oxide anions such as dithionate and tetrathionate are separated using flow programming with naphthalenetrisulfonate as the mobile phase in less than 20 minutes. With both detection modes, desired chromatographic performance of these three eluents is achieved without pH adjustment of the mobile phase.
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  • 95
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 33 (1992), S. 45-48 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Heat-treated milk ; Milk quality indicators ; 5-Hydroxymethyl-2-furfuraldehyde
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An enhanced method of HPLC for the determination of 5-Hydroxymethyl-2-furfuraldehyde (HMF) in fluid milk was perfected. Its resolving capacity permitted the specific separation of this compound. The real concentration (μmol/l) of HMF was determined and not the HMF value, as in the colorimetric analysis, where an intermediary coloured compound (HMF-TBA) is utilised. The optimum pH condition (pH=4.0–4.2) for the mobile phase to prevent overlapping between the HMF peak and the peaks of the other compound (α and β) that coeluted with the HMF and also the optimum organic solvent content (3% or 7%) were established. This is a sensitive, quick and safe method for the determination of HMF in fluid milk.
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  • 96
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Chlortetracycline ; Reversed-phase silical gel ; C8 bonded phase ; Collaborative study
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An established method for the analysis of chlortetracycline by liquid chromatography using octylsilylated silica gel as the stationary phase was examined in a multicentre study involving five laboratories and a total of six columns. Three chlortetracycline hydrochloride samples were analysed. The main component and the impurities were determined. An analysis of variance, treating each column as a different laboratory, showed an absence of consistent between-laboratory bias and the presence of a significant laboratory-sample interaction. The repeatability and the reproducibility of the method, expressed as relative standard deviations of the result of the determination of chlortetracycline hydrochloride, were calculated to be 0.9% and 1.1% respectively.
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  • 97
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 37 (1993), S. 627-634 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; ODS phases ; NMR and FTIR characterization ; Stationary phase functionality
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Two spectroscopic methods, solid state NMR and diffuse reflectance FTIR, have been used in conjunction with liquid chromatographicretention data to identify and distinguish the functionality of octadecylsilica (ODS) stationary phases. NMR and FTIR spectra are indicative of various features of the different functionalities of the phases and this information can be used to elucidate the configuration of the organosilyl moiety in the ODS on the silica surface and explain why DSS phases have different molecular shape (mainly planarity) recognition capability.
    Materialart: Digitale Medien
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  • 98
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 37 (1993), S. 423-428 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Polymer-modified silica ; Polypyrrole cloride ; Polypyrrole dodecylsulfate ; Small molecules ; Polyaromatic hydrocarbons
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Polypyrrole chloride and polypyrrole dodecylsulfate coated-silica packing materials have been synthesized. Reverse-phase chromtographuy was employed to characterise both packings. A series of test compounds with known properties was used as molecular probes. They included benzene and derivatives, basic drugs, and polyaromatic hydrocarbons. A commericial C18 column was also used for the purpose of comparison in some cases.
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  • 99
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Arsenic compounds ; Polymeric styrene divinylbenzene phase ; Ion-pairing
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The resolving power of an ion-pair reversed-phase liquid chromatography method, on a polymeric stationary phase (PRP-1) with an alkaline aqueous mobile phase (pH=9) containing tetrabutylammonium cation as ion-pairing agent, is compared with a traditional ion-pairing system using an octadecyl-modified silica column and a neutral aqueous mobile phase (pH=7.3). This chromatographic system (PRP-1 column) provides a rapid means for the determination of two of the most important arsenic species, arsenobetaine and arsenite. Addition of methanol (5%) to the aqueous mobile phase allows the differentation of arsenobetaine from the system peak when using UV detection.
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  • 100
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Gravity-flow column chromatography ; Provitamin A determination
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The provitamin A content of some food samples was determined by methods involving MgO: Hyflosupercel gravityflow column chromatography (GFCC) and reversed phase high performance liquid chromatography (HPLC), the quantitation being done by external standardization (HPLC-ES) or internal standardization (HPLC-IS) with Sudan. The results obtained with α- and β-carotene in carrots, β-carotene and β-cryptoxanthin in papaya and β-carotene in tomato and kale agreed well, showing that any of the these techniques can be used, provided the analysis is done under optimum conditions. Good separation of the different provitamins using GFCC depends on the analyst's skill and visual acuity. HPLC-ES required a constant supply of provitamin standards, thus the varying purity of commercially available standards and the high instability of these compounds could pose grave problems. Due to the stability of Sudan, HPLC-IS appeared to be the method of choice although passage of the extract through a MgO: Hyflosupercel minicolumn was required prior to injection to separate chlorophylls, dihydroxy- and polyoxycarotenoids which would otherwise elute with Sudan. Nonconformity of the Sudan structure to those of the provitamins did not effect the quantitative results. The chromatographic separation, identity and quantification of the provitamins could be more easily established by using HPLC-IS, complemented with GFCC.
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