辅助降血糖类保健食品非法添加化学物质检测方法研究

目的：利用超高效液相-串联四级杆-飞行时间液质联用系统（UPLC-DAD-Q-TOF-MS/MS）,建立快速可靠灵敏的测定辅助降血糖类保健食品中非法添加二甲双胍、丁二胍、苯乙双胍、甲苯磺丁脲、格列齐特、吡格列酮、罗格列酮、格列波脲、格列吡嗪、瑞格列奈、格列美脲、格列本脲和格列喹酮13种化学药品的液质联用检测方法。方法：采用UPLC-DAD-Q-TOF-MS/MS检测,以Agilent ZORBAX Eclipse Plus C18为填充柱;0.1%甲酸-0.01 mol/L乙酸铵水溶液和甲醇梯度洗脱,流速0.3 mL/min;ESI正离子模式,一级、二级质谱全扫描,进行UPLC-DAD-Q-TOF-MS/MS的定性及定量分析。结果：此方法经过验证,线性良好（r〉0.99）、精密度RSD〈3%、样品回收率在74.1%-90.0%之间,检出限在9.29-60.0 ng/mL之间,均能满足辅助降血糖类保健食品非法添加化学成分筛查的要求。结论：此方法快速、准确、灵敏度高、分离度高,可为辅助降血糖类保健食品非法添加筛查检测提供有力工具。

Study on the Detection Method for Illegally Added Chemicals in Auxiliary Hypoglycemic Health Food

Objective：To establish a fast , accurate and sensitive method for the detection of illegally added chemicals in auxiliary hypoglycemic health food by UPLC-DAD-Q-TOF-MS/MS . The chemicals include metformin , buformin , phenformin , tolbutamide , gliclazide , pioglitazone , rosiglitazone , glibornuride , glipizide , repaglinide , glimepiride, glyburide and gliquidone. Methods：Agilent ZORBAX Eclipse Plus C18 analysis column was adopted with a mobile phase of 0 . 01 mol/L ammonium acetate （ containing 0 . 1% acetic acid ）-methanol using gradient elution , and the flow rate was 0 . 3 mL/min . ESI＋ scan and MS/MS mode were taken . Qualitative and quantitative analysis were carried out by UPLC-DAD-Q-TOF-MS/MS . Results：The method was validated , a linear range was good （r 〉 0 . 99） with a precision of RSD 〈 3%, the recovery was between 74 . 1% - 90 . 0% and the limit of detection was between 9 . 29 - 60 . 0 ng/mL , which can fully meet the screening requirements . Conclusion：This method is fast and accurate with a high sensitivity and a high degree of separation . It can be used for the screening and detection of illegally added chemicals in auxiliary hypoglycemic health food .