高效液相色谱-质谱联用测定大鼠体内西罗莫司血药浓度

孙明辉 斯陆勤 翟雪珍 凌婧 杨祥良

中国药学杂志 ›› 2010, Vol. 45 ›› Issue (2) : 132-134.

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中国药学杂志 ›› 2010, Vol. 45 ›› Issue (2) : 132-134.
论著

高效液相色谱-质谱联用测定大鼠体内西罗莫司血药浓度

  • 孙明辉1,2b,斯陆勤2a,翟雪珍2a,凌婧2a,杨祥良2b
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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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摘要

目的 建立测定SD大鼠体内雷帕霉素(RAPA)血药浓度的HPLC-MS/MS联用方法方法 色谱柱为Phenomenex Luna C18(2.0 mm×250 mm,5 μm);以甲醇-水(90∶10)为流动相;流速0.25 mL·min-1;柱温55 ℃。选用ESI源,以多反应采集模式(MRM)进行正离子检测,RAPA m/z 936.6→409.2和丙酸睾酮(内标)m/z 345.4→109.1。取全血样品经液-液萃取后,HPLC进样10 μL。结果 RAPA的线性范围为0.54~108.00 μg·L-1,定量下限为0.54 μg·L-1,日内、日间精密度(RSD)均小于12%。结论方法精密、准确,适用于RAPA在大鼠体内的药动学研究。

Abstract

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.

关键词

西罗莫司 / 高效液相色谱-质谱联用

Key words

sirolimus / HPLC-MS

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孙明辉 斯陆勤 翟雪珍 凌婧 杨祥良. 高效液相色谱-质谱联用测定大鼠体内西罗莫司血药浓度[J]. 中国药学杂志, 2010, 45(2): 132-134
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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