SPE/UPLC-MS-MS法测定改善睡眠保健品中5种非法添加药物

Determination of 5 illegally added drugs in sleep-improving healthcare foods by solid phase extracted with ultra performance liquid chromatography-tandem mass spectrometry

建立了HLB固相萃取柱净化、超高效液相色谱-串联质谱同时检测改善睡眠类保健品中佐匹克隆、褪黑素、文拉法辛、氯美扎酮和阿普唑仑5种药物的分析方法。样品经50%甲醇-水溶液提取,HLB固相萃取柱净化,BEH C18色谱柱分离,用0.1%甲酸水溶液和0.1%甲酸乙腈梯度洗脱,采用多反应监测模式检测,基质标准曲线,外标法定量。结果表明,5种药物在9 min内有效分离;线性范围(0.1~50)μg/L内,相关系数(R^2)均大于0.996;在3个添加水平下,片剂样品平均回收率为78.7%~104.0%,RSD在2.0%~9.6%之间;口服液样品平均回收率为80.5%~100.3%,RSD在2.6%~9.4%之间;检出限(0.03~0.15)μg/kg;定量限(0.10~0.50)μg/kg。该方法简便、快速、灵敏度高,可用于改善睡眠类保健品中安眠类药物的检测。

A sensitive method for the simultaneous determination of five illegally added drugs（zopiclone, melatonin, venlafaxine, chlormezanone and alprazolam） was established in sleep-improving healthcare foods using solid phase extracted with ultra performance liquid chromatography-tandem mass spectrometry. The sample was dissolved with 50% methanol aqueous solution, then subjected to be purified by solid phase extraction with Oasis HLB cartridge. The separation was performed on a Waters ACQUITY UPLC BEH C（18） column（100 mm×2.1 mm, 1.7 μm） by using 0.1%（v/v） formic acid acetonitrile and 0.1%（v/v） formic acid solution as the mobile phases with gradient elution at a flow rate of 0.3 m L/min. The electrospray ionization（ESI） source in positive ion mode was used for the analysis of the five drugs in the multiple reaction monitoring（MRM） mode, and quantified with matrix standard curve. The results indicated that the five drugs could be effectively separated in 9 min. The standard curves for the five drugs were obtained with good correlation coefficients（R^20.996） in the concentration range of（0.1~50） μg/L. The average recoveries at three spiked levels of tablet sample were 78.7%~104.0% with the relative standard deviation were 2.0%~9.6%. The average recoveries at three spiked levels of oral liquid sample were 80.5%~100.3% with the relative standard deviation were 2.6%~9.4%. The limits of detection（LOD） for the five drugs were in the range of（0.03~0.15） μg/kg. And the limits of quantitation（LOQ） for the five drugs were in the range of（0.10~0.50） μg/kg. The developed method is simple, rapid, high sensitivity and feasible for the simultaneous determination of the illegally added drugs in sleep-improving health-care foods.