减肥保健食品中违禁添加双胍类西药的分析方法研究

Study on determination of illegal drugs metformin and phenformin added in the weight-loss functional foods

目的:建立测定减肥保健食品中违禁添加二甲双胍和苯乙双胍的超高效液相色谱-串联质谱分析方法,并通过研究其质谱特征,推测质谱裂解途径。方法:不同基质类型的减肥保健食品超声提取15min,经弱阳离子交换固相萃取小柱WCX净化后,以ACQUITY UPLC BEH HILIC(1.7μm,100mm×2.1mm)分离,进行UPLC-MS/MS多反应监测模式下的定性及定量分析。结果:苯乙双胍在0.1～50μg/L的范围内呈良好的线性关系,相关系数为0.9996;二甲双胍在0.05～50μg/L的范围内呈良好的线性关系,相关系数为0.9995。在3个添加水平范围内的平均回收率为80.7%～96.3%;日内精密度均小于8%,日间精密度均小于10%。结论:本方法分析速度快,灵敏度高,回收率好,可用于不同减肥保健食品中违禁添加二甲双胍和苯乙双胍的同时检测。

Objective：To develop a simple and rapid analytical method for the simultaneous determination of metformin and phenformin in the weight-loss functional foods by ultra performance liquid chromatography tandem mass spectrometry and study mass spectra characterization in order to speculate on fragmentation pathways. Methods.Various weight-loss functional foods were extracted under ultrasonication in 15min and purified by WCX column. Qualitative and quantitative analysis was carried out for the samples under the MRM mode after the chromatographic separation on ACQUITY UPLC BEH HILIC column （1.7um,100mm×2.1mm）. Results ： phenformin was linear in the range 0.1 -50ug/L and the linear correlation coefficient reached 0.9996; metformin was linear in the range 0.05-50ug/L and the linear correlation coefficient reached 0.9995. The method recoveries at the three spiked levels （low,middle,high） were 80.7%-96.3%,with the intra-day precision less than 8% and the Inter-day precision less than 10%. Conclusion：The method was reliable,sensitive,high recovery and adapts to the determination of metformin and phenformin in the weight-loss functional foods.