Determination of Sirolimus in Rat Whole Blood by HPLC-MS/MS
SUN Ming-hui1,2b, SI Lu-qin2a, ZHAI Xue-zhen2a, LING Jing2a,YANG Xiang-liang2b
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1.Department of Pharmacy, Tongji Hospital Affiliated to the Tongji Medical College, Wuhan 430030, China; 2. Huazhong University of Science and Technology a.School of Pharmacy, Wuhan 430030, China; b.School of Life Science and Technology, Wuhan 430074,China
OBJECTIVE To develop a HPLC-MS/MS method for the determination of sirolimus in rat whole blood. METHODS Sirolimus and internal standard testosterone were extracted from whole blood with liquid-liquid extraction, then separated on a Phenomenex Luna C18 column(2.0 mm×250 mm,5 μm)at the flow-rate of 0.25 mL·min-1. The mobile phase was methanol-water(90∶10) and the column temperature was 55 ℃. Electrospray ionization(ESI) source was applied and operated in the positive ion mode. Multiple reaction monitoring (MRM) mode with the transitions of m/z 936.6→409.2 and m/z 345.4→109.1 were used to quantify sirolimus and the internal standard, respectively. RESULTS The linear calibration curve was obtained in the concentration range of 0.54~108.00 μg·L-1. The low limit of quantification was 0.54 μg·L-1. The inter- and intra-day precisions (RSDs) were less than 12%. CONCLUSION The method has been proved to be specific, sensitive, rapid and suitable for the pharmacokinetic study of sirolimus in rats.
SUN Ming-hui;SI Lu-qin;ZHI Xue-zhen;LING Jing;YNG Xing-ling.
Determination of Sirolimus in Rat Whole Blood by HPLC-MS/MS[J]. Chinese Pharmaceutical Journal, 2010, 45(2): 132-134
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