HPLC-IT-TOF-MS快速检测减肥、降脂、降糖类保健食品中非法添加的25种化学药品

Fast Screening of 25 Illegally Added Chemical Drugs in Weight-reducing,Lipid-lowering and Hypoglycemic Health Foods by HPLC-IT-TOF-MS

目的:利用超高效液相色谱-离子阱-飞行时间串联质谱(HPLC-IT-TOF-MS),建立减肥类、降脂类、降糖类保健食品中非法添加的25种化学药品的快速检测方法。方法:样品经甲醇超声提取后,经Waters Acquity UPLC BEH C18(150 mm×2.1 mm,1.7μm)色谱柱分离,流动相A为含0.1%乙酸的20 mmol·L-1乙酸铵溶液,流动相B为甲醇-乙腈(5∶3,v/v)溶液,梯度洗脱,流速为0.2 ml·min-1;采用UPLC-IT-TOF-MS液质联用仪,电喷雾离子源,正、负离子模式同时检测,以保留时间、精确质量数匹配,结合二级特征碎片离子,实现快速定性筛查,一级准分子离子峰定量检测。结果:经方法学验证,25种非法添加化学药物在相应的浓度范围内呈良好的线性关系,相关系数均大于0.995,检出限在2.56~112.10 ng·ml-1之间;3种基质中的回收率均在76.1%~114.3%范围内,RSD均<15%(n=6)。结论:本方法专属、灵敏、快速,适用于减肥、降脂、降糖类保健食品中非法添加化学药品的筛查和确证工作。

Objective： To establish a fast screening method for the simultaneous determination of 25 illegally added chemical drugs in weight-reducing,lipid-lowering and hypoglycemic health foods by high performance liquid chromatography-ion trap-time of flight mass spectrometry（ HPLC-IT-TOF-MS）. Methods： After ultrasonic extracted by methanol,the sample was separated on a Waters Acquity UPLC BEH C18（ 150 mm × 2. 1 mm,1. 7 μm） column with 20 mmol · L-1 ammonium acetate solution（ containing 0. 1% acetic acid） as the mobile phases A and methanol-acetonitrile（ 5 ∶ 3,v/v） as the mobile phases B with gradient elution,and the flow rate was 0. 2 ml · min-1. A UPLC-IT-TOF-MS method was adopted. Electrospray ionization（ ESI） source was applied and operated in a positive and negative mode. The fast screening was performed with the retention time,and precision mass matching and the characteristic fragment ions,and the determination was conducted in an MS1 scan mode. Results： The method was validated. The 25 drugs showed good linear relationships within the ranges of corresponding concentrations with the correlation coefficients above 0. 995. The detection limits were 2. 56-112. 10 ng · ml-1. The recoveries were within the range of 76. 1%-114. 3% with the RSDs less than 15%in the three matrices. Conclusion： The established method is specific,sensitive and rapid in the screening and confirmation of illegally added drugs in weight-reducing,lipid-lowering and hypoglycemic health foods.