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学科主题: 临床医学
题名:
A Simple and Sensitive LC-MS/MS Method for Simultaneous Determination of Temsirolimus and Its Major Metabolite in Human Whole Blood
作者: 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
发表日期: 2012-12-01
DOI: 10.1007/s10337-012-2341-2
卷: 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
项目资助者: National Comprehensive Cancer Network ; Wyeth-Pfizer ; American Society of Clinical Oncology (ASCO)
WOS记录号: WOS:000311667100006
Citation statistics:
内容类型: 期刊论文
URI标识: http://ir.bjmu.edu.cn/handle/400002259/55035
Appears in Collections:北京大学第三临床医学院_药剂科_期刊论文

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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

Recommended Citation:
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.
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