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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 k V,漂移管电压7.5 k V,进气温度180℃,漂移管温度180℃,栅电压45 V,栅脉冲宽度120μs,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 establish a rapid detection method of illegitimate addition of phenobarbital, amobarbital and sarcobarbital in sleep-like health care products by ion mobility spectrometry (IMS). Methods: Ion mobility spectrometry was used to set the condition of negative source. The voltage of the ion source was 1.9 kV, the drift tube voltage was 7.5 kV, the inlet temperature was 180 ℃, the drift tube temperature was 180 ℃, the gate voltage was 45 V and the gate pulse width was 120μs , The drift tube flow rate was 1.2 L · min -1, the exhaust pump was 0.8 L · min -1, the running time was 30 s, and the spectral range was 25 ms. The samples were extracted by methanol, injected directly and shifted from the control Time comparison analysis to determine whether there is illegal addition of barbiturates. Results: The detection limit of a barbiturate alone could be achieved and the minimum detectable limit of three barbiturates illegally added was determined according to the signal to noise ratio (S / N) ≥3. A variety of compounds At the same time, the separation and identification of phenobarbital and the other two substances can be effectively achieved, while the isolation and identification of amobarbital and scocoobater can not be achieved. Detection of illicitly added barbiturates in improving sleep-type health supplements is consistent with the identification of mass spectrometry. Conclusion: This method is validated by methodology and can be used to improve the initial screening of illegal addition of barbiturates to sleeping health products.