Journal of Chromatography B: Biomedical Sciences and Applications最新文献_第9页

High-performance liquid chromatographic determination of diclofenac in human plasma after solid-phase extraction 固相萃取后高效液相色谱法测定人血浆中双氯芬酸含量

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00383-8

Cinzia Arcelloni , Roberto Lanzi , Silvia Pedercini , Giulia Molteni , Isabella Fermo , Antonio Pontiroli , Rita Paroni

引用次数: 88

Determination of efavirenz in human plasma by high-performance liquid chromatography with ultraviolet detection 紫外检测高效液相色谱法测定人血浆中依非韦伦的含量

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00357-7

Marı́a Sarasa-Nacenta , Yolanda López-Púa , Luis F López-Cortés , Josep Mallolas , José Mª Gatell , Xavier Carné

{"title":"Determination of efavirenz in human plasma by high-performance liquid chromatography with ultraviolet detection","authors":"Marı́a Sarasa-Nacenta , Yolanda López-Púa , Luis F López-Cortés , Josep Mallolas , José Mª Gatell , Xavier Carné","doi":"10.1016/S0378-4347(01)00357-7","DOIUrl":"10.1016/S0378-4347(01)00357-7","url":null,"abstract":"<div>Efavirenz is a non-nucleoside reverse transcriptase inhibitor for the treatment of the HIV infection. A simple, high-performance liquid chromatographic method has been developed and validated for the quantitative determination of efavirenz in human plasma. The method involved solid-phase extraction of the drug and the internal standard (L-737,354) from 300 μl of human plasma. The analysis was via UV detection at 250 nm using a reversed-phase C8 analytical column and a isocratic mobile phase consisting of phosphate buffer (pH 5.75)–acetonitrile that resolved the drug and internal standard from endogenous matrix components and potential coadministered drugs. Within- and between-day precisions were less than 8.6% for all quality control samples. The lower limit of quantification was 0.1 μg/ml. Recovery of efavirenz from human plasma was greater than 83%. This validated assay is being used in pharmacokinetic studies with efavirenz.</div>","PeriodicalId":15463,"journal":{"name":"Journal of Chromatography B: Biomedical Sciences and Applications","volume":"763 1","pages":"Pages 53-59"},"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)00357-7","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80530232","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: 51

Chromatographic performance of a thin microporous bed of nitrocellulose 硝酸纤维素微孔薄层的色谱性能

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00376-0

Maria Lönnberg , Jan Carlsson

引用次数: 18

Improved selectivity in detection of polar basic drugs by liquid chromatography–electrospray ionization mass spectrometry 提高液相色谱-电喷雾质谱法检测极性碱性药物的选择性

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00355-3

M.A. Campanero , I. Bueno , M.A. Arangoa , M. Escolar , E.G. Quetglás , A. López-Ocáriz , J.R. Azanza

{"title":"Improved selectivity in detection of polar basic drugs by liquid chromatography–electrospray ionization mass spectrometry","authors":"M.A. Campanero , I. Bueno , M.A. Arangoa , M. Escolar , E.G. Quetglás , A. López-Ocáriz , J.R. Azanza","doi":"10.1016/S0378-4347(01)00355-3","DOIUrl":"10.1016/S0378-4347(01)00355-3","url":null,"abstract":"<div>It is well to assume that bioanalytical chromatographic methods for the determination of polar basic drugs are developed and optimised according to a standardised procedure which involves two alternatives: (a) modifications in the sample preparation procedures, and (b) changes in the stationary phase of the chromatographic system. In this paper, a simple and rapid chromatographic procedure using a specific analytical detection method (ESI tandem mass spectrophotometric detection) in combination with a fast and efficient sample work-up procedure, protein precipitation, is presented. A demonstration of the entire chromatographic procedure is given for an HPLC method for the determination of famotidine in human plasma, a basic polar drug with poor solubility in organic solvents. In order to optimize the mass detection of famotidine, several parameters such as ionization mode, fragmentor voltage, m/z ratios of ions monitored, type of organic modifier and eluent additive, were investigated. Each analysis required 5 min. The calibration curve of famotidine in the range 1–200 ng/ml was linear with a correlation coefficient of 0.9992 (n=6), and a detection limit a signal-to-noise ratio of 3 was ∼0.2 ng/ml. The within- and between-day variations in the famotidine analysis were 5.2 (n=6) and 6.7% (n=18), respectively. The applicability of this method was also demonstrated for the analysis of plasma samples in a Phase-I human pharmacokinetic study.</div>","PeriodicalId":15463,"journal":{"name":"Journal of Chromatography B: Biomedical Sciences and Applications","volume":"763 1","pages":"Pages 21-33"},"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)00355-3","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73937112","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: 27

Author Index Vol. 763 作者索引卷763

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00413-3

引用次数: 0

Quantitation of promethazine and metabolites in urine samples using on-line solid-phase extraction and column-switching 在线固相萃取和柱切换法测定尿样中的异丙嗪及其代谢物

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00351-6

Q Song , L Putcha

{"title":"Quantitation of promethazine and metabolites in urine samples using on-line solid-phase extraction and column-switching","authors":"Q Song , L Putcha","doi":"10.1016/S0378-4347(01)00351-6","DOIUrl":"10.1016/S0378-4347(01)00351-6","url":null,"abstract":"<div>A chromatographic method for the quantitation of promethazine (PMZ) and its three metabolites in urine employing on-line solid-phase extraction and column-switching has been developed. The column-switching system described here uses an extraction column for the purification of PMZ and its metabolites from a urine matrix. The extraneous matrix interference was removed by flushing the extraction column with a gradient elution. The analytes of interest were then eluted onto an analytical column for further chromatographic separation using a mobile phase of greater solvent strength. This method is specific and sensitive with a range of 3.75–1400 ng/ml for PMZ and 2.5–1400 ng/ml for the metabolites promethazine sulfoxide, monodesmethyl promethazine sulfoxide and monodesmethyl promethazine. The lower limits of quantitation (LLOQ) were 3.75 ng/ml with less than 6.2% C.V. for PMZ and 2.50 ng/ml with less than 11.5% C.V. for metabolites based on a signal-to-noise ratio of 10:1 or greater. The accuracy and precision were within ±11.8% in bias and not greater than 5.5% C.V. in intra- and inter-assay precision for PMZ and metabolites. Method robustness was investigated using a Plackett–Burman experimental design. The applicability of the analytical method for pharmacokinetic studies in humans is illustrated.</div>","PeriodicalId":15463,"journal":{"name":"Journal of Chromatography B: Biomedical Sciences and Applications","volume":"763 1","pages":"Pages 9-20"},"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)00351-6","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78654842","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: 16

Quantification of busulfan in plasma by liquid chromatography–ion spray mass spectrometry 液相色谱-离子喷雾质谱法定量测定血浆中的丁硫丹

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-11-05 DOI: 10.1016/S0378-4347(01)00356-5

Marie-Hélène Quernin , Michel Duval , Catherine Litalien , Etienne Vilmer , Evelyne Jacqz Aigrain

{"title":"Quantification of busulfan in plasma by liquid chromatography–ion spray mass spectrometry","authors":"Marie-Hélène Quernin , Michel Duval , Catherine Litalien , Etienne Vilmer , Evelyne Jacqz Aigrain","doi":"10.1016/S0378-4347(01)00356-5","DOIUrl":"10.1016/S0378-4347(01)00356-5","url":null,"abstract":"<div>Optimisation of busulfan dosage in patients undergoing bone marrow transplantation is recommended in order to reduce toxic effects associated with high drug exposure. A new method was developed coupling liquid chromatography with mass spectrometry (LC–MS) and was validated for the determination of busulfan concentrations in plasma. Recovery was 86.7%, the limit of detection was 2.5 ng/ml and linearity ranged from 5 to 2500 ng/ml. The correlation between the busulfan concentrations measured by our previously published HPLC–UV method and the new HPLC–MS method was highly significant (P<0.0001). Sample volume was reduced and the method was rapid, sensitive and less expensive than the methods previously used in our laboratory. This method was used to determine the pharmacokinetic parameters of busulfan after the first administration of 1 mg/kg orally, in 13 children receiving the drug as part of the preparative regimen for bone marrow transplantation. Our results were similar to previously reported data. They showed that the apparent oral clearance of busulfan was 0.299±0.08 l/h/kg, and that it was significantly higher (P=0.02) in patients below the age of 5 years than in older children.</div>","PeriodicalId":15463,"journal":{"name":"Journal of Chromatography B: Biomedical Sciences and Applications","volume":"763 1","pages":"Pages 61-69"},"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)00356-5","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"91428110","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: 29

High-performance liquid chromatographic–fluorimetric assay of chymotrypsin-like esterase activity 高效液相色谱-荧光法测定凝乳胰蛋白酶样酯酶活性

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-10-25 DOI: 10.1016/S0378-4347(01)00353-X

Kazuki Kushida , Takeshi Kato , Toshiyuki Chikuma , Hiroshi Hojo

{"title":"High-performance liquid chromatographic–fluorimetric assay of chymotrypsin-like esterase activity","authors":"Kazuki Kushida , Takeshi Kato , Toshiyuki Chikuma , Hiroshi Hojo","doi":"10.1016/S0378-4347(01)00353-X","DOIUrl":"10.1016/S0378-4347(01)00353-X","url":null,"abstract":"<div>A sensitive and reproducible assay for the determination of chymotrypsin-like esterase activity is reported. This method is based on fluorimetric detection of a dansylated amino acid, 5-dimethylaminonaphthalene-1-sulfonyl-l-phenylalanine, enzymatically formed from the substrate 5-dimethylaminonaphthalene-1-sulfonyl-l-phenylalanine ethyl ester, after separation by high-performance liquid chromatography using a C18 reversed-phase column and isocratic elution. This method is sensitive enough to measure 5-dimethylaminonaphthalene-1-sulfonyl-l-phenylalanine at concentrations as low as 40 pmol/ml, yields highly reproducible results and requires less than 9.5 min per sample for quantitation. The optimum pH for chymotrypsin-like esterase activity was 7.7–8.3. The Km and Vmax values were, respectively 25 μM and 0.241 pmol/μg protein/h with the use of enzyme extract obtained from mouse kidney. The approximate molecular mass of this enzyme was estimated to be 67 000 by gel filtration. Chymotrypsin-like esterase activity was strongly inhibited by N-tosyl-l-phenylalaline chloromethyl ketone. Among the mouse organs examined, the highest specific activity of the enzyme was found in lung. This new method would be useful for clarification of the physiological role of this enzyme.</div>","PeriodicalId":15463,"journal":{"name":"Journal of Chromatography B: Biomedical Sciences and Applications","volume":"762 2","pages":"Pages 137-145"},"PeriodicalIF":0.0,"publicationDate":"2001-10-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0378-4347(01)00353-X","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74210983","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: 3

Simultaneous determination of enantiomers of structurally related anticholinergic analogs in human serum by liquid chromatography–electrospray ionization mass spectrometry with on-line sample cleanup 液相色谱-电喷雾质谱同时测定人血清中结构相关的抗胆碱能类似物对映体

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-10-25 DOI: 10.1016/S0378-4347(01)00364-4

Vladimı́r Čápka , Yan Xu

引用次数: 26

Improved high-performance liquid chromatographic method for the combined analysis of phospholipase, lipoxygenase and cyclooxygenase activities 改进的高效液相色谱法联合分析磷脂酶、脂加氧酶和环加氧酶的活性

Journal of Chromatography B: Biomedical Sciences and Applications Pub Date : 2001-10-25 DOI: 10.1016/S0378-4347(01)00363-2

Denis Reynaud , Andrea Sun , Peter Demin , Cecil R Pace-Asciak

{"title":"Improved high-performance liquid chromatographic method for the combined analysis of phospholipase, lipoxygenase and cyclooxygenase activities","authors":"Denis Reynaud , Andrea Sun , Peter Demin , Cecil R Pace-Asciak","doi":"10.1016/S0378-4347(01)00363-2","DOIUrl":"10.1016/S0378-4347(01)00363-2","url":null,"abstract":"<div>We report herein an improved method for the high-performance liquid chromatographic separation and analysis of eicosanoids formed during the stimulation of human platelets in vitro with collagen. Since the products of interest, excepting arachidonic acid, contain hydroxyl groups (one to several), our method involves the conversion of the hydroxyl groups into acetates (pyridine/acetic anhydride) after derivatization with anthryl diazomethane (ADAM) rendering the compounds with much decreased polarity for separation on a reversed-phase column. This procedure is superior to that involving ADAM esters only, i.e. with free hydroxyl groups, as it leads to the excellent separation of the desired compounds from each other and from extraneous peaks observed due to the ADAM reagent and sharpens the peak of thromboxane. We have successfully applied the method to investigate the formation of thromboxane B2 and 12-hydroxyheptadecatrienoic acid (HHT) (products of cyclooxygenase and thromboxane A2 synthase), 12-hydroxyeicosatetraenoic acid (12-HETE, a 12-lipoxygenase product) and arachidonic acid (AA, product of phospholipase A2) formed during the in vitro aggregation of human platelets induced by collagen. A correlation between the inhibition of aggregation by aspirin and thromboxane/HHT formation was observed. All four compounds can be chromatographed in a single run. We employed prostaglandin B1 (PGB1) as internal reference standard to quantify the products. The method is useful to investigate selectivity of drugs which may affect either or all of these enzyme pathways at the same time.</div>","PeriodicalId":15463,"journal":{"name":"Journal of Chromatography B: Biomedical Sciences and Applications","volume":"762 2","pages":"Pages 175-180"},"PeriodicalIF":0.0,"publicationDate":"2001-10-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.1016/S0378-4347(01)00363-2","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87453383","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: 2