Journal of Chromatography B: Biomedical Sciences and Applications最新文献_第8页

Fluorometric determination of dl-fenfluramine, dl-norfenfluramine and phentermine in plasma by achiral and chiral high-performance liquid chromatography 非手性和手性高效液相色谱法测定血浆中dl-芬氟拉明、dl-诺芬氟拉明和芬特明

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00368-1

Amal Kaddoumi, Mihoko N Nakashima, Kenichiro Nakashima

{"title":"Fluorometric determination of dl-fenfluramine, dl-norfenfluramine and phentermine in plasma by achiral and chiral high-performance liquid chromatography","authors":"Amal Kaddoumi, Mihoko N Nakashima, Kenichiro Nakashima","doi":"10.1016/S0378-4347(01)00368-1","DOIUrl":"10.1016/S0378-4347(01)00368-1","url":null,"abstract":"<div><p>High-performance liquid chromatography (HPLC) with fluorescence detection has been developed for the simultaneous determination of sympathomimetic amines including ephedrine, norephedrine, 2-phenylethylamine, 4-bromo-2,5-dimethoxyphenylethylamine, phentermine (Phen) and <span>dl</span>-fenfluramine (Fen) in spiked human plasma. Furthermore, an enantioselective HPLC method for the separation of <span>d</span>-Fen (dexfenfluramine) and <span>l</span>-Fen (levofenfluramine) in addition to their active metabolites <span>d</span>- and <span>l</span>-norfenfluramine (Norf) is described. The detection was achieved at emission wavelength of 430 nm with excitation wavelength of 325 nm for both methods. The analytes were extracted from plasma (100 μl) at pH 10.6 with ethyl acetate using fluoxetine as the internal standard. The extracts were evaporated and derivatized with the fluorescence reagent 4-(4,5-diphenyl-1<em>H</em>-imidazole-2-yl)benzoyl chloride in the presence of carbonate buffer (pH 9.0). A gradient separation was achieved on a C<sub>18</sub> column for the achiral separation or on a Chiralcel OD-R column for the chiral separation. The methods were fully validated, and shown to have excellent linearity, sensitivity and precision. The chiral method has been applied for the determination of <span>d</span>- and <span>l</span>-enantiomers of Fen and Norf, in addition to Phen in rat plasma after an intraperitoneal administration of <span>dl</span>-Fen and Phen, simultaneously.</p></div>","PeriodicalId":15463,"journal":{"name":"Journal of Chromatography B: Biomedical Sciences and Applications","volume":"763 1","pages":"Pages 79-90"},"PeriodicalIF":0.0,"publicationDate":"2001-11-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0378-4347(01)00368-1","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82601714","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}

引用次数: 25

Determination of mycophenolic acid and its phenol glucuronide metabolite in human plasma and urine by high-performance liquid chromatography 高效液相色谱法测定人血浆和尿液中霉酚酸及其酚葡萄糖醛酸代谢物

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00354-1

Kamonthip Wiwattanawongsa , Erin L Heinzen, Daniel C Kemp, Robert E Dupuis, Philip C Smith

引用次数: 45

Comparison of the capabilities of liquid isoelectric focusing–one-dimensional nonporous silica reversed-phase liquid chromatography–electrospray ionization time-of-flight mass spectrometry and liquid isoelectric focusing–one-dimensional sodium dodecyl sulfate polyacrylamide gel electrophoresis mass mapping for the analysis of intact protein molecular masses 液体等电聚焦-一维无孔二氧化硅反相液相色谱-电喷雾电离飞行时间质谱法与液体等电聚焦-一维十二烷基硫酸钠聚丙烯酰胺凝胶电泳质谱图分析完整蛋白质分子质量的能力比较

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00382-6

Daniel B Wall, Stephen J Parus, David M Lubman

{"title":"Comparison of the capabilities of liquid isoelectric focusing–one-dimensional nonporous silica reversed-phase liquid chromatography–electrospray ionization time-of-flight mass spectrometry and liquid isoelectric focusing–one-dimensional sodium dodecyl sulfate polyacrylamide gel electrophoresis mass mapping for the analysis of intact protein molecular masses","authors":"Daniel B Wall, Stephen J Parus, David M Lubman","doi":"10.1016/S0378-4347(01)00382-6","DOIUrl":"10.1016/S0378-4347(01)00382-6","url":null,"abstract":"<div><p>Nonporous silica reversed-phase HPLC coupled to electrospray ionization with on-line time-of-flight mass spectrometric detection (NPS-RP-HPLC–ESI-TOF-MS) is shown to be an effective liquid phase method for obtaining the molecular masses of proteins from pH fractionated cellular lysates where the method is capable of generating the same banding patterns typically observed using gel phase one-dimensional sodium dodecyl sulfate–polyacrylamide gel electrophoresis. The liquid-phase mass spectrometry-based method provides a mass accuracy of at least 150 ppm, with 4000 mass resolution and provides improved sensitivity as the protein molecular mass (MW) decreases. The liquid and gel phase methods are shown to be complementary in terms of their mass range but the liquid phase method has the advantage over the gel method in that the analysis times are 50 times shorter, the mass accuracy is 70 times better and the resolution is 130 times higher. The liquid phase method is shown to be more effective for detection of proteins below 40 kDa, while the gel phase separation can access many more proteins, including more hydrophobic proteins, at increasing MW.</p></div>","PeriodicalId":15463,"journal":{"name":"Journal of Chromatography B: Biomedical Sciences and Applications","volume":"763 1","pages":"Pages 139-148"},"PeriodicalIF":0.0,"publicationDate":"2001-11-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0378-4347(01)00382-6","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84899541","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}

引用次数: 11

Automated chromatographic system for the simultaneous measurement of plasma pregnenolone and 17-hydroxypregnenolone by radioimmunoassay 用放射免疫法同时测定血浆孕烯醇酮和17-羟基孕烯醇酮的自动色谱系统

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00373-5

F.G Riepe, S Wonka, C.-J Partsch, W.G Sippell

引用次数: 15

High-performance liquid chromatographic analysis for the determination of a novel polymer-bound camptothecin derivative (MAG-camptothecin) and free camptothecin in human plasma 高效液相色谱法测定人血浆中新型聚合物结合喜树碱衍生物(mag -喜树碱)和游离喜树碱

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00391-7

Nadja E Schoemaker , Enrico Frigerio , Daniela Fraier , Jan H.M Schellens , Hilde Rosing , Sindy Jansen , Jos H Beijnen

{"title":"High-performance liquid chromatographic analysis for the determination of a novel polymer-bound camptothecin derivative (MAG-camptothecin) and free camptothecin in human plasma","authors":"Nadja E Schoemaker , Enrico Frigerio , Daniela Fraier , Jan H.M Schellens , Hilde Rosing , Sindy Jansen , Jos H Beijnen","doi":"10.1016/S0378-4347(01)00391-7","DOIUrl":"10.1016/S0378-4347(01)00391-7","url":null,"abstract":"<div><p>A selective HPLC assay is described for the determination of free and total (free plus polymer-bound) camptothecin (CPT) in human plasma after administration of the anti-tumor drug MAG-CPT (polymer bound camptothecin). Total CPT levels were determined after hydrolysis and free CPT was extracted from acidified plasma using Oasis solid-phase extraction material. Extracts were analyzed on a Zorbax SB-C<sub>8</sub> analytical column, using a mixture of acetonitrile–25 m<em>M</em> phosphate buffer (pH 4.0) as the eluent. Detection was performed fluorimetrically. Concentrations of polymer-bound CPT were calculated by subtraction of free from total CPT. The lower limits of quantitation of the methods were 100 ng/ml for total and 1.0 ng/ml for free CPT using 50 μl and 250 μl plasma, respectively. Special attention was paid to the stability of the analytes. The presented method was successfully applied in a clinical pharmacokinetic study in our institute.</p></div>","PeriodicalId":15463,"journal":{"name":"Journal of Chromatography B: Biomedical Sciences and Applications","volume":"763 1","pages":"Pages 173-183"},"PeriodicalIF":0.0,"publicationDate":"2001-11-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0378-4347(01)00391-7","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74766304","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}

引用次数: 12

Simultaneous determination of retinol, β-carotene and α-tocopherol in adipose tissue by high-performance liquid chromatography 高效液相色谱法同时测定脂肪组织中视黄醇、β-胡萝卜素和α-生育酚

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00349-8

S Casal, B Macedo, M.B.P.P Oliveira

引用次数: 37

Determination of cyclosporin A in human and mouse plasma by reversed-phase high-performance liquid chromatography 反相高效液相色谱法测定人和小鼠血浆中环孢素A的含量

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00389-9

Heleen A. Bardelmeijer , Mariët Ouwehand , Jos H. Beijnen , Jan H.M. Schellens , Olaf van Tellingen

{"title":"Determination of cyclosporin A in human and mouse plasma by reversed-phase high-performance liquid chromatography","authors":"Heleen A. Bardelmeijer , Mariët Ouwehand , Jos H. Beijnen , Jan H.M. Schellens , Olaf van Tellingen","doi":"10.1016/S0378-4347(01)00389-9","DOIUrl":"10.1016/S0378-4347(01)00389-9","url":null,"abstract":"<div><p>An isocratic reversed-phase high-performance liquid chromatographic method with ultraviolet detection at 227 nm has been validated for the determination of cyclosporin A in human and mouse plasma. The cyclosporin D analog PSC 833 was used as internal standard. Plasma samples were pretreated by liquid–liquid extraction with diethyl ether. A good chromatographic separation between cyclosporin A, the internal standard and two potentially interfering endogenous peaks was achieved using a stainless steel column packed with 5 μm Nova-Pak phenyl material operated at 72°C, and a mobile phase consisting of acetonitrile–methanol–water (20:52:28, v/v/v). The calibration curve for cyclosporin A in human plasma was linear over the tested concentration range of 0.11 to 5.34 μ<em>M</em>. Murine plasma samples (200 μl) were diluted up to a total volume of 500 μl with blank human plasma and the concentrations were read from the calibration curve prepared in human plasma. The lower limit of quantitation was 0.11 μ<em>M</em> using 500 μl of human plasma and 0.28 μ<em>M</em> using 200 μl of mouse plasma. The validation data showed that the assay is sensitive, selective and reproducible for determination of cyclosporin A. The applicability was demonstrated in a pharmacokinetic experiment where mice received oral cyclosporin A.</p></div>","PeriodicalId":15463,"journal":{"name":"Journal of Chromatography B: Biomedical Sciences and Applications","volume":"763 1","pages":"Pages 201-206"},"PeriodicalIF":0.0,"publicationDate":"2001-11-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0378-4347(01)00389-9","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81508464","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}

引用次数: 6

Development of a high-performance liquid chromatographic method for bioanalytical applications with sulpiride 高效液相色谱法在舒必利生物分析中的应用

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00387-5

Ming-Chuan Huang , Hsiu-O Ho , Geng-Cheng Yeh , Wen-Ting Ke , Li-Chin Lin , T.-M Bruce Hsu , Ching-Cheng Kao , Ming-Thau Sheu

{"title":"Development of a high-performance liquid chromatographic method for bioanalytical applications with sulpiride","authors":"Ming-Chuan Huang , Hsiu-O Ho , Geng-Cheng Yeh , Wen-Ting Ke , Li-Chin Lin , T.-M Bruce Hsu , Ching-Cheng Kao , Ming-Thau Sheu","doi":"10.1016/S0378-4347(01)00387-5","DOIUrl":"10.1016/S0378-4347(01)00387-5","url":null,"abstract":"<div><p>An improved HPLC method using a silica gel column with fluorescence detection (excitation at 300 nm and emission at 365 nm) was developed for the determination of sulpiride concentrations in plasma. Analysis of sulpiride in plasma samples was simplified by a one-step liquid–liquid extraction after alkaline treatment of only 1 ml of plasma. The low limit of quantitation was 20 ng/ml with a coefficient of variation of less than 20%. A linear range was found from 20 to 1500 ng/ml. This HPLC method was validated with the precision for inter-day and intra-day runs being 0.36–8.01% and 0.29–5.25%, respectively, and the accuracy (standard deviation of mean, SD) for inter-day and intra-day runs being −1.58 to 5.02% and −2.14 to 5.21%, respectively. Bioequivalence of the two products was evaluated in 12 normal healthy male volunteers in a single-dose, two-period, two-sequence, two-treatment cross-over study. Sulpiride plasma concentrations were analyzed with this validated HPLC method. Results demonstrated that the two tablet formulations of sulpiride appear to be bioequivalent.</p></div>","PeriodicalId":15463,"journal":{"name":"Journal of Chromatography B: Biomedical Sciences and Applications","volume":"763 1","pages":"Pages 157-163"},"PeriodicalIF":0.0,"publicationDate":"2001-11-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0378-4347(01)00387-5","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81797279","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}

引用次数: 34

Sensitive liquid chromatographic assay for the basic DNA intercalator (N,N-dimethylaminoethyl)-9-amino-5-methylacridine-4-carboxamide and its nitroarylmethyl quaternary prodrugs in biological samples 生物样品中碱性DNA插入剂(N,N-二甲氨基乙基)-9-氨基-5-甲基吖啶-4-羧酰胺及其硝基甲基季前药的灵敏液相色谱分析

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00381-4

Dianne M Ferry, Pierre L van Zijl, William R Wilson

引用次数: 2

Identification of phase I and phase II metabolites of ketobemidone in patient urine using liquid chromatography–electrospray tandem mass spectrometry 用液相色谱-电喷雾串联质谱法鉴定患者尿液中酮贝酮的I期和II期代谢物

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00375-9

Ingela Sundström , Ulf Bondesson , Mikael Hedeland

引用次数: 16