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目的:建立检测降血糖类保健食品中非法添加8种药物的方法并用于实际检测。方法:采用高效液相色谱-串联质谱法,以ZORBAX Eclipse Plus C18(2.1 mm×50 mm,1.8μm)色谱柱,以0.1%甲酸溶液为流动相A,甲醇为流动相B,梯度洗脱。通过分子离子峰、二级碎片、色谱保留时间等信息,对宣称辅助降血糖类保健食品非法添加8种化学药物进行鉴别和定量测定。结果:8种药物实现了同时分离与专属鉴定,检出限为5.5~76 ng/g,精密度为0.22%~1.19%,回收率为74.0%~111.9%;本法适用于硬胶囊样品;利用本法,从15批样品中检测出9批含非法添加化学药物。结论:本方法专属性强、灵敏度高,结果准确可靠,可作为宣称辅助降血糖类保健食品中检测非法添加化学药物的方法参考。
OBJECTIVE: To establish a method for the illegal addition of 8 drugs in hypoglycemic health food and to test it in practice. Methods: High performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) was performed on a ZORBAX Eclipse Plus C18 (2.1 mm × 50 mm, 1.8 μm) column using 0.1% formic acid as mobile phase A and methanol as mobile phase B, gradient elution. Through the molecular ion peak, secondary debris, chromatographic retention time and other information on the alleged hypoglycemic health food illegally added eight kinds of chemical drugs for identification and quantitative determination. Results: The simultaneous separation and exclusive identification of eight drugs were achieved. The detection limits were 5.5 ~ 76 ng / g, the precision was 0.22% ~ 1.19% and the recoveries were 74.0% ~ 111.9%. The method was applied to hard capsule samples. Using this Act, nine batches containing illicitly added chemicals were detected from 15 batches of samples. Conclusion: This method is highly specific, sensitive and accurate and reliable. It can be used as a reference for the detection of illicit drug adding in hypoglycemic health food.