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建立了降血糖功能食品中二甲双胍和苯乙双胍的液相色谱-串联质谱测定方法。采用体积比1:1的甲醇-乙醇溶液超声提取降血糖功能食品降糖粉、奶粉、口服液、胶囊、清渴茶中的二甲双胍和苯乙双胍,提取液经WCX固相萃取柱净化后,以乙腈和2 mmol/L NH4Ac溶液(含0.1%甲酸)为流动相进行梯度洗脱,经Agilent ZORBAX Eclipse XDB-C18色谱柱分离,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,基质回收标准曲线定量。二甲双胍和苯乙双胍的定量限(LOQ)均为10.0μg/kg,在不同基质中添加水平为10.0,20.0,50.0μg/kg时,二甲双胍和苯乙双胍的平均回收率分别为92.7%～99.6%和91.3%～100.3%,RSD分别为2.1%～8.4%和1.1%～11%。本方法可用于降血糖功能食品中双胍类药物的测定和确证。
A method for the determination of metformin and phenformin in hypoglycemic food was established by liquid chromatography-tandem mass spectrometry. The volume of 1: 1 by volume of methanol - ethanol ultrasonic extraction hypoglycemic food hypoglycemic powder, milk powder, oral solution, capsules, thirst tea in the metformin and phenformin, the extract was purified by WCX solid phase extraction column, The mobile phase was eluted with acetonitrile and 2 mmol / L NH4Ac solution (containing 0.1% formic acid). The mobile phase was separated on an Agilent ZORBAX Eclipse XDB-C18 column. Electrospray positive ionization (ESI + Pattern detection, matrix recovery standard curve quantitative. The limits of quantitation (LOQ) of metformin and phenformin were both 10.0μg / kg. The mean recoveries of metformin and phenformin were 10.0%, 10.0% and 50.0μg / kg respectively in different matrices, and the average recoveries of metformin and phenformin were 92.7% ~ 99.6 % And 91.3% ~ 100.3%, RSD 2.1% ~ 8.4% and 1.1% ~ 11% respectively. The method can be used for measuring and confirming biguanide in hypoglycemic food.