电喷雾离子迁移谱快速检测减肥类保健食品中非法添加的22种化学药物

Rapid Detection of 22 Illegally Added Chemicals Inweight-loss Health Foods by Electrospray Ionization-Ion Mobility Spectrometry

目的:采用电喷雾-离子迁移谱(electrospray ionization-ion mobility spectrometry,ESI-IMS)技术,建立减肥类保健食品中非法添加的22种化学药品的现场快速检测方法。方法:样品经适量80%甲醇溶液超声提取获得供试品储备液,用含0.5%乙酸(V/V)的80%甲醇溶液适量稀释后,采用正离子模式(源电压:2200 V)检测普罗布考、盐酸芬氟拉明、盐酸安非他酮、盐酸吡格列酮、瑞格列奈、吉非罗齐、盐酸西布曲明、盐酸N-单去甲基西布曲明、盐酸N,N-双去甲基西布曲明、盐酸氟西汀、马来酸罗格列酮、盐酸伪麻黄碱、盐酸甲基安非他明、非诺贝特、吲达帕胺、比沙可啶、盐酸二甲双胍、酚酞。供试品储备液用含0.5%氨水(V/V)的80%甲醇溶液适量稀释,在负离子模式(源电压:1800 V)下检测呋塞米、氢氯噻嗪、氯噻嗪、氟伐他汀钠。迁移管电压均为8000 V,进气口温度和迁移管温度为180℃,门电压45 V,栅脉冲宽度120μs。并用所建方法对40批市场抽查减肥类保健食品进行非法添加筛查。结果:该方法专属性良好,22种减肥类标准品迁移时间在8.0~16.3 ms之间,在基质样品中检出限为0.05~8.0 mg·L^-1。样品中1批检出西布曲明,1批检出酚酞,1批检出氟西汀。结论:本方法迅速、灵敏,适用于减肥类保健食品中非法添加化学药品的快速筛查工作。

Objective:To establish a rapid screening method for the 22 illegally added chemical drugs by ion mobility spectrometry(IMS)in weight-loss health foods.Methods:After ultrasonic extraction of the sample with appropriate amount of 80%methanolsolution to obtain the sample reserve solution,the sample reserve solution was diluted with 80%methanolsolution containing 0.5%acetic acid(V/V),and the positive ion mode(source voltage of 2200 V)was employed to detect probucol,fluoxetine hydrochloride,bupropion hydrochloride,pioglitazone hydrochloride,repaglinide,gemfibrozil,sibutramine hydrochloride,N-desmethylsibutramine hydrochloride,N,N-didesmethylsibutramine hydrochloride,fluoxetine hydrochloride,rosiglitazone maleate,pseudoephedrine hydrochloride,methamphetamine hydrochloride,fenofibrate,indapamide,bisacodyl,metformin hydrochloride and phenolphthalein.The sample reserve solution was diluted with 80% methanolsolution containing 0.5%ammonia water(V/V),and the negative ion mode(source voltage of 1800 V)was employed to detect furosemide,hydrochlorothiazide,chlorothiazide and fluvastatin sodium.The drift tube voltage was 8000 V,the gas inlet and drift tube were both controlled at the temperature of 180℃.The gate voltage was 45 V and the gate pulse width was 120μs.40 batches of weight-loss health foods were detected by the established method.Results:This method had good specificity.The drift time of all 22 kinds of weight-loss drugs were between 8.0 and 16.3 ms,and their detection limits were 0.05~8.0 mg·L^-1 in the matrix.Sibutramine was detected in 1 batch,phenolphthalein was detected in 1 batch,and fluoxetine was detected in 1 batch.Conclusion:The established method is rapid and sensitive,which is suitable for the rapid screening of the illegal addition of chemicals in weight-loss health foods.