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目的建立液相色谱-串联质谱法(liquid chromatography-mass spectrometry/mass spectrometry,LC-MS/MS)测定人血浆中青霉素V的浓度,并用于人体药代动力学研究。方法以甲醇和乙腈沉淀蛋白处理样品,采用C18色谱柱,流动相为5 mmol/L醋酸胺+0.5%甲酸水溶液-乙腈(55∶45,v/v),以氯硝西泮为内标,电喷雾离子源,选择正离子多离子反应监测模式,检测离子分别为m/z351.10→m/z160.10(青霉素V)和m/z316.00→m/z270.00(内标),并测定了19名健康志愿者口服单剂量青霉素V钾片0.472 g后血药浓度。结果青霉素V在0.05~20.00 mg/L浓度范围内线性关系良好,相对回收率大于96.7%,提取回收率大于94.9%,日内相对标准差(relative standard deviation,RSD)小于2.3%,日间RSD小于10.4%。结论本法准确可靠专属性强,可作为人血浆中青霉素V的测定方法。
Objective To establish a liquid chromatography-mass spectrometry / mass spectrometry (LC-MS / MS) method for the determination of penicillin V in human plasma and to study its pharmacokinetics. Methods The protein samples were precipitated with methanol and acetonitrile. The mobile phase consisted of 5 mmol / L ammonium acetate and 0.5% formic acid in acetonitrile (55:45, v / v) on a C18 column. Clonazepam was used as internal standard, Electrospray ionization source was used to select the positive ion multi-ion reaction monitoring mode. The detected ions were m / z351.10 → m / z160.10 (penicillin V) and m / z316.00 → m / z270.00 The plasma concentration of 0.472 g of single dose penicillin V potassium tablet was measured in 19 healthy volunteers. Results The linear range of penicillin V was 0.05-20.00 mg / L. The relative recovery was more than 96.7%. The recovery of penicillin V was more than 94.9%. The relative standard deviation (RSD) was less than 2.3%. The daytime RSD was less than 10.4%. Conclusion This method is accurate and reliable and can be used as a method for determination of penicillin V in human plasma.