高效液相色谱-质谱联用法快速检测中成药和保健食品中非法添加的12种减肥类药物

Rapid determination of 12 kinds of slimming chemical drugs illegally added into traditional Chinese medicine and health food by high performance liquid chromatography-mass spectrometry

目的建立高效液相色谱-离子阱质谱联用法测定保健食品中非法添加的12种化学减肥药物(去甲伪麻黄碱、伪麻黄碱、甲基麻黄碱、咖啡因、安非他明、甲基安非他明、氯卡色林、芬氟拉明、酚酞、比沙可啶、氟西汀、布美他尼)的分析方法。方法采用资生堂CAPCELL-PAK C18色谱柱(4.6 mm×150 mm,5μm),梯度洗脱:流动相A为含0.1%冰乙酸的0.02 mol/L乙酸铵溶液,流动相B为甲醇,流速:0.5 mL/min;扫描方式为正离子扫描;通过与对照品色谱图和质谱图的对比,对样品中非法添加的化学药物进行定性鉴别。结果本法检测上述12种化学物质,各化合物色谱峰之间分离度良好,方法的检出限为0.2~0.5 ng/mL。33批样品中,2批检测出酚酞。结论该方法灵敏、选择性强、快速,可用于中药材和保健食品中非法添加的减肥化学药品的定性检测。

Objective To establish a method for the determination of 12 kinds of slimming chemical drugs(including norpseudoephedrine,pseudoephedrine,methylephedrine,caffeine,amphetamine,methylamphetamine,lorcaserin,fenfluramine,phenolphthalein,bisacodyl,fluoxetine,bumetanide)illegally added into traditional Chinese medicine and health food by high performance liquid chromatography-electrospray ion trap mass-spectrometry.Methods The analysis was performed on a SHISEIDO HPLC PACKED C18 column(4.6 mm×150 mm,5μm)with the mobile phase consisting of methanol-0.02 mol/L ammonium acetate solution containing 0.1%acetic acid in a gradient elution mode at a flow rate of 0.5 mL/min.The scanning mode was positive ion scanning,and the chemical drugs illegally added in the sample were qualitatively identified by comparing with the chromatogram and mass spectrum of the reference substance.Results In this method,the above 12 chemicals were detected,and the resolution between the peaks was good,the detection limit of the method was 0.2-0.5 ng/mL.Phenolphthalein was detected in 2 of 33 samples.Conclusion This method is sensitive,selective and rapid in the qualitative detection of slimming chemical drugs illegally added into traditional Chinese medicines and health food.