Journal of chromatography最新文献

{"title":"Separation and characterization of rat kidney isometallothioneins induced by exposure to inorganic mercury.","authors":"M A Morcillo,&nbsp;J Santamaría","doi":"10.1016/0021-9673(93)87013-c","DOIUrl":"https://doi.org/10.1016/0021-9673(93)87013-c","url":null,"abstract":"<p><p>High-performance liquid chromatography (HPLC) was applied to the separation of metallothionein (MT) isoforms from different tissues from a variety of eukaryotic species. Recently we reported an analytical method for 203Hg-metallothionein, which detects the radioisotope bound to each iso-MT after separation by HPLC on a size-exclusion column coupled with on-line radioactivity flow detection. The MTs can be separated as distinct isoprotein peaks by elution with alkaline buffer solution owing to cation-exchange chromatographic action. In the present work, renal MT from rats exposed to inorganic mercury was separated into four peaks by UV and 203Hg detection. Moreover, it was resolved into four components by non-denaturing polyacrylamide gel electrophoresis. The two major components correspond to MT-1 and MT-2, which were characterized by amino acid analysis. Finally, Hg induces and binds to both iso-MTs.</p>","PeriodicalId":15508,"journal":{"name":"Journal of chromatography","volume":"655 1","pages":"77-83"},"PeriodicalIF":0.0,"publicationDate":"1993-11-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/0021-9673(93)87013-c","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"19295382","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Liquid chromatography and radioimmunoassay method for the determination of prostaglandins E1 and E2 in rat embryo incubates.","authors":"G Hotter,&nbsp;J Roselló-Catafau,&nbsp;D Closa,&nbsp;G Bioque,&nbsp;E Gelpí,&nbsp;A Javerbaum,&nbsp;E González,&nbsp;M A Gimeno","doi":"10.1016/0021-9673(93)87014-d","DOIUrl":"https://doi.org/10.1016/0021-9673(93)87014-d","url":null,"abstract":"<p><p>This paper describes the application of a combined high-performance liquid chromatography and radioimmunological assay method for the measurement of prostaglandins E1(PGE1) and E2(PGE2). Samples were acidified to pH 3.15, extracted twice with ethyl acetate and further processed through C18 solid-phase extraction cartridges. After HPLC purification, PGE1 and PGE2 were measured by radioimmunological techniques. The limit of detection for PGE1 was 3.9 pg/ml and the intra-assay relative standard deviation was 7.8% for n = 5. The accuracy of the assay procedure was also verified. The method has been applied to the determination of PGE1 and PGE2 in embryo incubates from 10-day pregnant rats.</p>","PeriodicalId":15508,"journal":{"name":"Journal of chromatography","volume":"655 1","pages":"85-8"},"PeriodicalIF":0.0,"publicationDate":"1993-11-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/0021-9673(93)87014-d","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"19295383","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of chlorinated insecticides in blood samples of agricultural workers.","authors":"M G Rosell,&nbsp;J Obiols,&nbsp;M J Berenguer,&nbsp;X Guardino,&nbsp;F López,&nbsp;J Brosa","doi":"10.1016/0021-9673(93)87023-f","DOIUrl":"https://doi.org/10.1016/0021-9673(93)87023-f","url":null,"abstract":"<p><p>Lindane, aldrin and p,p'-DDT were determined in blood samples from 71 farmers by means of an analytical method which combines a direct whole-blood extraction with n-hexane and gas chromatography (GC)-electron-capture detection (ECD), using a capillary column, applied to the organic extract. This technique allowed the determination of pesticides at levels varying from 0.1 to 180 micrograms per l of blood, the detection limit for every pesticide being 0.1 microgram/l. GC-mass spectrometry was used to confirm the identity of each pesticide. The advantage of capillary column GC-ECD for pesticide determination is its sensitivity and high resolution, which makes it possible to separate pesticides from a complex n-hexane extract obtained in a very simple pretreatment of the blood sample, which is itself a very complex matrix.</p>","PeriodicalId":15508,"journal":{"name":"Journal of chromatography","volume":"655 1","pages":"151-4"},"PeriodicalIF":0.0,"publicationDate":"1993-11-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/0021-9673(93)87023-f","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"19295380","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of clenbuterol and salbutamol in urine by capillary gas chromatography with capillary columns of 100 microns.","authors":"J A García Regueiro,&nbsp;B Pérez,&nbsp;G Casademont","doi":"10.1016/0021-9673(93)87012-b","DOIUrl":"https://doi.org/10.1016/0021-9673(93)87012-b","url":null,"abstract":"<p><p>A method to determine clenbuterol and salbutamol in calf urine is described. Two independent extraction procedures using Extrelut (clenbuterol) and octadecylsilica (salbutamol) were used; the extracts obtained were mixed and purified over a cyanopropyl minicolumn. Trimethylsilyl derivatives were prepared and analysed by GC-MS in selected-ion monitoring mode using a fused-silica open tubular capillary column, 10 m x 100 microns coated with 5% phenylmethylsilicone. Splitless injection was optimized to achieve low percentage residual standard deviation of absolute areas. The best conditions were: injection volume 0.5 microliter, column head pressure 22 p.s.i. (1 p.s.i. = 6894.76 Pa), inlet temperature 250 degrees C and glass liner volume 250 microliters. The recoveries of the complete procedure were in the range 50-60% for both compounds.</p>","PeriodicalId":15508,"journal":{"name":"Journal of chromatography","volume":"655 1","pages":"73-6"},"PeriodicalIF":0.0,"publicationDate":"1993-11-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/0021-9673(93)87012-b","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"19295381","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"High-performance liquid chromatographic determination of plasma triglyceride type composition in a normal population of Barcelona. Relationship with age, sex and other plasma lipid parameters.","authors":"M Parreño,&nbsp;A I Castellote,&nbsp;R Codony","doi":"10.1016/0021-9673(93)87015-e","DOIUrl":"https://doi.org/10.1016/0021-9673(93)87015-e","url":null,"abstract":"<p><p>A coupled TLC-HPLC procedure is proposed for the separation and determination of plasma triglycerides. The method was tested by application to plasma samples corresponding to a normal population of Barcelona (Spain). Eighteen different triglyceride types were identified and their relative proportions were established, in order to give a \"normal profile\" for men and women. Sex-related differences (p < 0.05) were only found for dioleostearin and palmitodilinolein + linoleooleopalmitolein (LLP+LOPa). A correlation study showed that palmitodiolein and total cholesterol levels increase with age, whereas LLP-LOPa decreases in men and palmitolinoleoolein + palmitooleopalmitolein in women.</p>","PeriodicalId":15508,"journal":{"name":"Journal of chromatography","volume":"655 1","pages":"89-94"},"PeriodicalIF":0.0,"publicationDate":"1993-11-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/0021-9673(93)87015-e","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"19294589","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Identification of radiolabeled metabolites of nicotine in rat bile. Synthesis of S-(-)-nicotine N-glucuronide and direct separation of nicotine-derived conjugates using high-performance liquid chromatography.","authors":"M J Seaton,&nbsp;E S Vesell,&nbsp;H Luo,&nbsp;E M Hawes","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>Four metabolites of nicotine, including two glucuronides, have been separated by high-performance liquid chromatography. This separation was applied to identification of biliary metabolites of radiolabeled nicotine by radiometric detection. S-(-)-Nicotine N-glucuronide was synthesized and used as a standard in method development.</p>","PeriodicalId":15508,"journal":{"name":"Journal of chromatography","volume":"621 1","pages":"49-53"},"PeriodicalIF":0.0,"publicationDate":"1993-11-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"19294783","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Automated sample preparation by on-line dialysis and trace enrichment. Analysis of morphine, 6-monoacetylmorphine, codeine, ethylmorphine and pholcodine in plasma and whole blood by capillary gas chromatography and capillary gas chromatography-mass spectrometry.","authors":"M Krogh,&nbsp;A S Christophersen,&nbsp;K E Rasmussen","doi":"","DOIUrl":"","url":null,"abstract":"<p><p>A fully automated sample preparation method for the determination of five opiates in human plasma and whole blood is described. The technique combines dialysis and trace enrichment prior to gas chromatography and gas chromatography-mass spectrometry. Dialysis and trace enrichment on a polymer column was shown to be a highly reliable method for sample preparation. The method can be used, after minor modification, to determine other basic drugs in plasma and whole blood. The method demonstrates the potential of the automated sequential trace enrichment of dialysate (ASTED) system for automated sample preparation.</p>","PeriodicalId":15508,"journal":{"name":"Journal of chromatography","volume":"621 1","pages":"41-8"},"PeriodicalIF":0.0,"publicationDate":"1993-11-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"19294782","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Characterization of metallothionein isoforms. Comparison of capillary zone electrophoresis with reversed-phase high-performance liquid chromatography.","authors":"M P Richards,&nbsp;J H Beattie","doi":"10.1016/0021-9673(93)80429-c","DOIUrl":"https://doi.org/10.1016/0021-9673(93)80429-c","url":null,"abstract":"<p><p>The purpose of this study was to compare and contrast the separation of metallothionein (MT) isoforms by reversed-phase high-performance liquid chromatography (RP-HPLC) with capillary zone electrophoresis (CZE). RP-HPLC was performed on a Vydac C8 column eluted with a linear acetonitrile gradient. CZE was performed in a 57 cm x 75 microns I.D. fused-silica tube at an operating voltage of 30 kV. Phosphate buffer (10 mM) at pH 2.5, 7.0 and 11.0 was used for both separations. CZE at pH 2.5 resolved three distinct peaks of rabbit liver MT which were incompletely resolved at pH 7.0 or 11.0. RP-HPLC at pH 2.5 gave two peaks and the resolution was not as good as with CZE at the same pH. At pH 7.0 or 11.0, RP-HPLC of rabbit liver MT gave a single predominant peak of unresolved MT-1 and MT-2. Purified rabbit liver MT-1 and MT-2 were used to verify the identity of these peaks. In contrast, MT from horse kidney demonstrated three predominant peaks which were best resolved by CZE at pH 11.0, whereas RP-HPLC resolved only two peaks at pH 11.0 and 7.0. At pH 2.5, RP-HPLC of horse kidney MT gave three peaks, though two of the peaks were incompletely separated. We conclude that pH has a considerable impact on the resolution of MT isoforms by CZE and RP-HPLC and that it is possible to exploit changes in pH to optimize the separation of isoforms for a particular species of MT. When samples of human and sheep liver MT-1, both of which exhibit microheterogeneity, were subjected to CZE, a single predominant peak was observed at each pH value. RP-HPLC of human liver MT-1 at pH 2.5 yielded two peaks that were incompletely resolved. Purified chick liver MT and rat liver MT-1 and MT-2 gave a single predominant peak at all pH values on CZE. In contrast, pig liver MT-1 and MT-2 each exhibited multiple peaks when subjected to CZE, the number of which depended on the pH used to separate the MT. In conclusion, CZE, with its orthogonal selectivity, and RP-HPLC make an excellent combination for the separation and characterization of MT isoforms. Because CZE is rapid (run times typically < 10 min) and requires little sample (< 100 nl), MT samples can readily be analyzed by CZE in conjunction with RP-HPLC or other techniques in order to maximize the information obtained about the individual isoforms.</p>","PeriodicalId":15508,"journal":{"name":"Journal of chromatography","volume":"648 2","pages":"459-68"},"PeriodicalIF":0.0,"publicationDate":"1993-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/0021-9673(93)80429-c","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"19216227","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Simple high-performance liquid chromatographic method for assessing the deterioration of atropine-oxime mixtures employed as antidotes in the treatment of nerve agent poisoning.","authors":"B M Paddle,&nbsp;M H Dowling","doi":"10.1016/0021-9673(93)80419-9","DOIUrl":"https://doi.org/10.1016/0021-9673(93)80419-9","url":null,"abstract":"<p><p>A set of reversed-phase HPLC conditions for determining the degradation of atropine and the oxime (pralidoxime, obidoxime, or HI-6) in autoinjectors designed for use against nerve agent poisoning is described. The assay conditions for atropine do not require its prior separation from the large molar excess of oxime since both the atropine and tropic acid peaks elute well clear of the oxime and its degradation products and the phenolic preservatives. Further dilution of the sample and simple changes to the mobile phase then provide conditions for the oxime and its major degradation products to be quantitated.</p>","PeriodicalId":15508,"journal":{"name":"Journal of chromatography","volume":"648 2","pages":"373-80"},"PeriodicalIF":0.0,"publicationDate":"1993-10-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/0021-9673(93)80419-9","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"19216226","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Identification and determination of individual sophorolipids in fermentation products by gradient elution high-performance liquid chromatography with evaporative light-scattering detection.","authors":"A M Davila,&nbsp;R Marchal,&nbsp;N Monin,&nbsp;J P Vandecasteele","doi":"10.1016/0021-9673(93)83295-4","DOIUrl":"https://doi.org/10.1016/0021-9673(93)83295-4","url":null,"abstract":"<p><p>High-performance liquid chromatography (HPLC) was used for the characterization of sophorolipids, one of the most important types of glycolipid biosurfactants. By using gradient elution with a water-acetonitrile mixture on a reversed-phase (C18) column and evaporative light-scattering detection, resolution of all the important individual sophorolipids present in fermentation products was achieved. In addition to HPLC, a combination of techniques involving selective production by fermentation of sophorolipids, chemical conversions of the products, separation methods and, for identification of lipidic chains of sophorolipids, gas chromatography and mass spectrometry was used. This led to the identification of almost all significant compounds observed in HPLC, including several previously unreported sophorolipids. As a result, a rapid method is now available for investigations of the influence of fermentation conditions on the nature and quantitative distribution of the sophorolipid products obtained.</p>","PeriodicalId":15508,"journal":{"name":"Journal of chromatography","volume":"648 1","pages":"139-49"},"PeriodicalIF":0.0,"publicationDate":"1993-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/0021-9673(93)83295-4","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"19233749","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}