【摘要】 目的采用LC-MS/MS法同时测定人血浆中的辛伐他汀和辛伐他汀酸。方法采用BEH C18色谱柱(50 mm×2.1mm,1.7μm),流动相为乙腈-0.01 mol.L-1醋酸铵(72∶28),流速0.15 mL.min-1,柱温40℃,进样量8μL。辛伐他汀、辛伐他汀酸及内标洛伐他汀的检测离子对分别为:m/z 419.43→199.12、437.38→303.26、405.45→199.14。结果辛伐他汀、辛伐他汀酸的线性范围分别为0.241～61.76 ng.mL-1(r=0.999)、0.344～88.16 ng.mL-1(r=0.997)。在人血浆基质中,高、中、低浓度(0.482、3.86、30.88 ng.mL-1)的日内、日间RSD均小于15%,方法回收率分别为95%～104%、97%～108%。样品预处理方法对血浆中的辛伐他汀和辛伐他汀酸测定无干扰。结论所用方法处理简单、灵敏、特异性高,定量准确,可为辛伐他汀制剂的药动学研究提供方法。更多还原

【Abstract】 OBJECTIVE To establish a method for determination of Simvastatin(SV) and Simvastatin hydroxy acid(SVA) in human plasma by LC-MS/MS.METHODS BEH C18(50 mm×2.1 mm,1.7 μm) was used.The mobile phase is consisted of acetonitrile-0.01 mol·L-1 ammonium acetate(72:28)and the flow rate was 0.15 mL·min-1;column temperature was 40 ℃,and injection volume was 8 μL.Positive ion MRM detection of SV and SVA was m/z 419.43→199.12,m/z 437.38→303.26,respectively.Lovastatin(LV)(m/z 405.45→199.14) was used as internal standard.RESULTS A good linearity was shown in the range of 0.241-61.76 ng·mL-1(r=0.999,n=5)for SV,and 0.344-88.16 ng·mL-1(r=0.997,n=5)for SVA.SV and SVA’s intra-day RSD and inter-day RSD were less than 15%.The average recovery was within 95%-104% and 97%-108%.Plasma matrix effect test showed endogenous matrix had no effect on quantification of SV and SVA.CONCLUSION The method is rapid,sensitive and accurate,to be used for determination of SV and SVA in human plasma.更多还原