NDLI: A Simple and Sensitive LC–MS/MS Method for Simultaneous Determination of Temsirolimus and Its Major Metabolite in Human Whole Blood

Content Provider	Springer Nature Link
Author	Zhang, Xianhua Louie, Alexander Li, Xiaohua Shi, Robert Kelley, Robin K. Huang, Yong
Copyright Year	2012
Abstract	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 μL) 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 × 3.0 mm, 5 μm) at 50 °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.
Starting Page	1405
Ending Page	1413
Page Count	9
File Format	PDF
ISSN	00095893
Journal	Chromatographia
Volume Number	75
Issue Number	23-24
e-ISSN	16121112
Language	English
Publisher	Springer-Verlag
Publisher Date	2012-10-27
Publisher Place	Berlin, Heidelberg
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	LC–MS/MS Temsirolimus Sirolimus Human blood Hepatocellular carcinoma Proteomics Chromatography Pharmacy Laboratory Medicine
Content Type	Text
Resource Type	Article
Subject	Organic Chemistry Analytical Chemistry Biochemistry Clinical Biochemistry

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