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 本方法精密、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
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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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参考文献
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脚注
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