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A Simple and Sensitive LC-MS/MS Method for Simultaneous Determination of Temsirolimus and Its Major Metabolite in Human Whole Blood
Zhang, Xianhua1,2; Louie, Alexander1; Li, Xiaohua1; Shi, Robert1; Kelley, Robin K.3; Huang, Yong1
关键词Lc-ms/ms Temsirolimus Sirolimus Human Blood Hepatocellular Carcinoma
刊名CHROMATOGRAPHIA
2012-12-01
DOI10.1007/s10337-012-2341-2
75期:23-24页:1405-1413
收录类别SCI
文章类型Article
WOS标题词Science & Technology
类目[WOS]Biochemical Research Methods ; Chemistry, Analytical
研究领域[WOS]Biochemistry & Molecular Biology ; Chemistry
关键词[WOS]TANDEM MASS-SPECTROMETRY ; RENAL-CELL CARCINOMA ; PHASE-II TRIAL ; LIQUID-CHROMATOGRAPHY ; MTOR INHIBITOR ; SIROLIMUS RAPAMYCIN ; ADVANCED CANCER ; CCI-779 ; RECURRENT ; PHARMACOKINETICS
英文摘要

A simple, fast and sensitive LC-MS/MS method was developed and validated for the simultaneous determination of the concentrations of temsirolimus and its major metabolite, sirolimus, in human whole blood. The blood sample (100 mu L) after adding temsirolimus-d7 and sirolimus-d3 internal standards was precipitated with 0.200 mL of methanol/0.300 M zinc sulfate (70/30, v/v), then analyzed by a Shimatzu LC system coupled to a Sciex API-5000 mass spectrometer. The chromatographic separation was carried out on a BDS Hypersil C8 column (50 x 3.0 mm, 5 mu m) at 50 A degrees C with a mobile phase composed of methanol/water/formic acid (72/28/0.1) (v/v/v) containing 2.50 mM ammonium acetate. Mass spectrometric detection was performed using electrospray positive ionization with multiple reaction monitoring mode. This method was validated from 0.250 to 100 ng mL(-1) for temsirolimus and 0.100 to 40.0 ng mL(-1) for sirolimus. The lower limits of quantitation were 0.25 ng mL(-1) for temsirolimus and 0.1 ng mL(-1) for sirolimus. The intra-day and inter-day precisions (CV %) of spiked quality control (QC) samples were less than 10.4 and 9.6 %, respectively. The accuracies as determined by the relative error for QC samples were less than 12.1 % for intra-day and 7.3 % for inter-day. No significant matrix effect was observed. This method has been successfully applied to analyze clinical pharmacokinetic study samples. The assay reproducibility was also demonstrated by using incurred samples.

语种英语
WOS记录号WOS:000311667100006
资助机构National Comprehensive Cancer Network ; Wyeth-Pfizer ; American Society of Clinical Oncology (ASCO)
引用统计
被引频次:2[WOS]   [WOS记录]     [WOS相关记录]
文献类型期刊论文
条目标识符http://ir.bjmu.edu.cn/handle/400002259/55035
专题北京大学第三临床医学院_药剂科
北京大学第一临床医学院_医学影像科
作者单位1.Peking Univ, Dept Pharm, Hosp 3, Beijing 100191, Peoples R China
2.Univ Calif San Francisco, Drug Studies Unit, Dept Bioengn & Therapeut Sci, San Francisco, CA 94143 USA
3.Univ Calif San Francisco, Helen Diller Family Comprehens Canc Ctr, San Francisco, CA 94143 USA
推荐引用方式
GB/T 7714
Zhang, Xianhua,Louie, Alexander,Li, Xiaohua,et al. A Simple and Sensitive LC-MS/MS Method for Simultaneous Determination of Temsirolimus and Its Major Metabolite in Human Whole Blood[J]. CHROMATOGRAPHIA,2012,75(23-24):1405-1413.
APA Zhang, Xianhua,Louie, Alexander,Li, Xiaohua,Shi, Robert,Kelley, Robin K.,&Huang, Yong.(2012).A Simple and Sensitive LC-MS/MS Method for Simultaneous Determination of Temsirolimus and Its Major Metabolite in Human Whole Blood.CHROMATOGRAPHIA,75(23-24),1405-1413.
MLA Zhang, Xianhua,et al."A Simple and Sensitive LC-MS/MS Method for Simultaneous Determination of Temsirolimus and Its Major Metabolite in Human Whole Blood".CHROMATOGRAPHIA 75.23-24(2012):1405-1413.
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