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建立了固相萃取-高效液相色谱测定降糖汤药中化学添加成分盐酸二甲双胍的方法。降糖汤药样品经乙醇涡旋超声提取后,使用弱阳离子固相萃取小柱净化后进样,使用Lnertsil ODS-3 C18(4.6 mm×250 mm,5μm)色谱柱,流动相为乙腈:甲醇:0.02 mol/L乙酸铵=20:20:60(V/V/V),流速0.4 m L/min,柱温30℃,紫外检测波长237 nm,外标法定量。标准曲线的线性范围在2.5~200 mg/L之间,相关系数r~2=0.9998,方法检出限为0.04 mg/L,加标回收率为89.5%~93.9%,RSD为5.3%。方法适用于降糖汤药中盐酸二甲双胍非法添加量的测定。
A method was established for the determination of metformin hydrochloride, a chemical additive in Jiangtang decoction, by solid-phase extraction and high performance liquid chromatography. Jiangtang Decoction sample was extracted by ethanol vortex and then purified by weak cation SPE column. The sample was separated on a Lnertsil ODS-3 C18 (4.6 mm × 250 mm, 5 μm) column with a mobile phase of acetonitrile: methanol: 0.02 mol / L ammonium acetate = 20:20:60 (V / V / V), the flow rate was 0.4 m L / min, the column temperature was 30 ℃, UV detection wavelength was 237 nm. The linear range of the standard curve was between 2.5 and 200 mg / L with a correlation coefficient of r = 2 = 0.9998. The detection limit of this method was 0.04 mg / L. The spiked recoveries ranged from 89.5% to 93.9% with a RSD of 5.3%. The method is suitable for measuring the amount of illegal addition of metformin hydrochloride in Jiangtang decoction.