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目的:建立LC-MS/MS法测定人血浆中二甲双胍的浓度。方法:人血浆样本以乙腈沉淀蛋白后,选用Zorbax SB-C18Narrow-Bore色谱柱(150 mm×2.1 mm,5μm),以甲醇-10 mmol.L-1乙酸铵(含1%甲酸)(5:95)为流动相,流速为0.3 mL.min-1;选用API3200型三重四极杆串联质谱仪的多重反应监测(MRM)扫描方式进行监测,电喷雾离子化源,正离子方式,选择监测离子反应分别为m/z130.1→m/z71.0(二甲双胍)和m/z147.1→m/z58.2(内标米曲肼)。结果:二甲双胍和米曲肼的保留时间分别为1.27 min和1.26 min;血浆中二甲双胍的线性范围为0.010～3.000 mg.L-1(r>0.99),定量下限为0.010mg.L-1;日内、日间RSD均小于6%;相对偏差(RE)均在±6%的范围以内;平均提取回收率为(86.6±5.4)%;稳定性试验中,在各种贮存条件下血浆中二甲双胍均较稳定。结论:该方法快速、灵敏,专属性强,重现性好,适用于人血浆中二甲双胍浓度的测定,可应用于盐酸二甲双胍肠溶片的人体生物等效性研究。
Objective: To establish a method for the determination of metformin in human plasma by LC-MS / MS. METHODS: Human plasma samples were precipitated with acetonitrile, and were separated on a Zorbax SB-C18 Narrow-Bore column (150 mm × 2.1 mm, 5 μm) using methanol 10 mmol·L -1 ammonium acetate (containing 1% formic acid) 95) as the mobile phase at a flow rate of 0.3 mL.min-1. Multiplex reaction monitoring (MRM) was performed with an API3200 triple quadrupole mass spectrometer. Electrospray ionization (ESI) source and positive ion mode The responses were m / z130.1 → m / z 71.0 (metformin) and m / z 147.1 → m / z 58.2 (internal standard Meldonium). Results: The retention times of metformin and melitraz were 1.27 and 1.26 min, respectively. The linear range of metformin in plasma was 0.010-3.000 mg.L-1 (r> 0.99) and the lower limit of quantitation was 0.010 mg.L-1. , RSD of day were less than 6%, relative deviation (RE) were within ± 6%, average recovery was (86.6 ± 5.4)%. In the stability test, metformin More stable. Conclusion: The method is rapid, sensitive, specific and reproducible. It is suitable for the determination of metformin in human plasma and can be applied to the bioequivalence study of metformin hydrochloride enteric-coated tablets.