离子迁移谱快速检测改善睡眠类保健品中非法添加的巴比妥类药物

目的:采用离子迁移谱(ion mobility spectrometry,IMS)技术,建立改善睡眠类保健品中苯巴比妥、异戊巴比妥、司可巴比妥的非法添加快速检测方法。方法:采用离子迁移谱技术,设定条件为负源,离子源电压1.9 kV,漂移管电压7.5 kV,进气温度180℃,漂移管温度180℃,栅电压45 V,栅脉冲宽度120 μs,漂移管流速1.2 L·min^-1,排气泵0.8 L·min^-1,运行时间30 s,光谱范围25 ms;样品经甲醇提取,直接进样,与对照品的迁移时间进行比对分析,判断是否有巴比妥类药物的非法添加。结果:可以实现单独存在一种巴比妥类化合物时的检测鉴定,并根据信噪比(S/N)≥3确定出3种非法添加巴比妥类化合物的最低检出限;多种化合物同时存在时,可以有效地实现苯巴比妥与另2种物质的分离鉴别,而对异戊巴比妥与司可巴比妥无法实现分离鉴定。在改善睡眠类保健食品中检出了非法添加的巴比妥类药物,与质谱的鉴定结果完全一致。结论:本方法经方法学验证,可用于改善睡眠类保健品中非法添加巴比妥类药物的初步筛选。

Objective: To develop a fast detecting method for the illegally added barbiturates(phenobarbital, amobarbital and secobarbital)by ion mobility spectrometry(IMS)in sleep-improving healthy foods.Methods: The analysis was performed on negative source of ion mobility spectrometry under following conditions:source voltage 1.9 kV,drift tube voltage 7.5 kV,gas inlet temp 180℃,drift tube temp 180℃,gate voltage 45 V,gate pulse width 120 μs,drift gas flow 1.2 L·min^-1,exhaust pump 0.8 L·min^-1,run time 30 s and spectrum length 25 ms.The samples were extracted by methanol,and then injected into IMS.The analysis of whether sleep-improving drugs was detected or not was performed using the migration time by comparing with the standards.Results: When only one kind of barbiturates compound exists,it could be easily detected.The limit of detection(LOD)was determined according to noise ratio(S/N)≥3.When more than one kind of barbiturates compound exist in the samples,Phenobarbital could be separated from the other two and detected easily,while the established method failed to separate Amobarbital or Secobarbital from each other.In addition,the barbiturates drugs adulterated in sleep-improving healthy food were rapidly identified and the results were conformed by HPLC-MS.Conclusion: The established IMS method for detecting adulterated barbiturates sleep-improving is simple and rapid,which can be used as an initial screening method in drug rapid detecting system.