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21.
This paper describes the screening for metabolites of butoprozine, a new anti-anginal drug, in dog bile by means of reverse-phase HPLC. Although it does involve a simple clean-up step to remove a substantial amount of endogenous bile compounds, this screening method nevertheless avoids extraction of metabolites and thus allows all metabolites to be introduced into the chromatographic system. A single run of 100 minutes from 100% water to 100% methanol in a linear gradient effects adequate separation of the great majority of metabolites without interference from remaining endogenous compounds. Two methods of differentiating between metabolite peaks and endogenous peaks have been worked out. The first one makes use of 14C-labeled butoprozine by measuring the amount of radioactivity in the column effluent while simultaneously recording the UV absorbance. The second method compares continuous gradient chromatograms of bile recorded before and after butoprozine administration under very similar conditions. The latter method can be applied to both radioactive and non-radioactive materials. 相似文献
22.
M. R. Gregg 《Chromatographia》1985,20(2):129-133
Summary Electrode surface modification by electrochemical pretreatment of glassy carbon electrodes was shown to enhance significantly the sensitivity of the electrodes for the detection of timolol and oxprenolol, but reduce slightly the sensitivity to prenalterol. This method may permit the detection of exprenolol and timolol with increased sensitivity, or may allow their detection at lower applied potentials than is presently possible. Electrode surface modification may prove to be a valuable aid to the detection of compounds that are considered to be outside the practical limits of electrochemical detection. 相似文献
23.
Summary Clenbuterol has been determined in urine by solidphase extraction on a C18 cartridge, diazotization of the eluate with nitrite, coupling of the diazonium ion with 1-(naphthyl)ethylenediamine, and
separation of the azo dye formed by HPLC with a C18 column and a micellar mobile phase containing 0.1 M sodium dodecyl sulphate, 12%n-butanol and 0.05 M citrate buffer, pH 3. Recoveries higher than 90% were obtained by mixing the samples with a 20% 0.2 M
NaOH before extraction. Limits of detection of 51 and 6.7 ng L−1 were obtained with spectrophotometric and thermal lens spectrometric detection, respectively; respective repeatabilities
were 3.1% (5 μg mL−1) and 5.6% (0.16 μg mL−1). 相似文献
24.
Roger M. Smith 《Chromatographia》1982,16(1):155-157
Summary The pungent principles of ginger and grains of paradise are examined using a reversed-phase HPLC column. An electrochemical detector is used to selectively detect the phenolic gingerols and shogaols. The retention indices of the compounds are compared using methanowater and acetonitrile-water as eluents.Presented at the 14th International Symposium on Chromatography London, September, 1982 相似文献
25.
Summary The use of non-segmented flow, post-column reaction detection is evaluated for use with miniaturized HPLC. Non-segmented open-tubular reactors with internal diameters 0.1 mm to 0.25 mm and packed-bed reactors with internal diameters of 1 mm, filled with 5 and 10 m particles are evaluated theoretically and experimentally with respect to band broadening and pressure drop characteristics. An integrated system consisting of miniaturized HPLC (1 mm i. d.) columns and compatible hardware is described. An example of the separation of catecholamines is given. 相似文献
26.
Summary A method is described for the determination of the enantiomeric purity (enantiomeric excess) of the anticholinergic drug oxyphenonium. The method for this quaternary ammonium compound is based on the direct HPLC analysis with a chiral stationary phase. Two kinds of 1-acid glycoprotein-bonded phases were used.For the detection a post-column extraction with fluorescence detection of the ion-pair counter ion dimethoxyantracene sulphonate was used. 相似文献
27.
Three different types of SCD combustion source have been evaluated for use in the chromatographic analysis of atmospheric sulfur compounds. The conventional FID source and the newer inverted burner source were found to be less sensitive and less stable than the flameless design. Overall, the flameless source was superior for use with HRGC-SCD. 相似文献
28.
Thermal lens detection with a 325.0 nm He-Cd excitation laser is used for thermooptical indirect detection in combination with the capillary electrophoretic separation of organic anions. The optimization of indirect thermooptical detection is discussed. With Mordant Yellow 7 (an azo dye) chosen as a probe ion limits of detection for 1-heptane-, 1-pentane-, 1-butane-, 1-propanesulfonic, and acetic acid at a level of n × 10−7 M were achieved with a separation electrolyte containing 50 μM of the probe ion and 5 mM Tris pH 9.90. A further increase in the detection sensitivity (twofold decrease in the limit of detection ) was obtained with a separation electrolyte containing a volume fraction of 20% acetonitrile. 相似文献
29.
Norbert V. Fehringer Dalia M. Gilvydis Stephen M. Walters Colin F. Poole 《Journal of separation science》1992,15(2):124-127
The combination of open tubular column gas chromatography with electrolytic conductivity detection has been evaluated for the determination of nitrogen-containing pesticide residues in food extracts. Optimization of the column position at the column-detector interface was crucial to the successful operation of the detector. The signal-to-noise ratio and response stability of the detector are greatly influenced by the composition of the electrolyte solvent. Large volume splitless injections using retention gaps and optimized detector operating conditions enabled pesticide residues in food extracts to be determined at sub parts-per-million levels. Although the electrolytic conductivity detector is less sensitive than the thermionic ionization detector, its greater nitrogen selectivity can he crucial to the determination of nitrogen-containing contaminants in food extracts, particularly in complex mixtures where phosphorus-containing contaminants or matrix compounds are also present. 相似文献
30.
A multidimensional GC-system containing two capillary columns of different polarities, operated within a double oven instrument, was used for the optimized separation of complex isomeric mixtures of various types of chlorinated aromatic compounds such as PCB, PCDD, or PCDF. Electron capture was applied parallel to flame ionization detection to obtain sensitive signals of the PCB or PCDD and the n-alkane standards required for identification by Kovats indices, respectively. Electron capture detection within a valvelessly operated MDGC system forced changes in the usual instrumental set-up, the live-switching coupling piece being located within the second oven of the double oven instrument. This oven is operated isothermally to ensure optimal and interference-free detection, for stable flow conditions within the coupling piece and for the determination of the isothermal retention indices (Kovats), which are much more suitable for identification by retention than the so-called “linear” indices. 相似文献