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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。
The HLB solid phase extraction column was used to purify and the combination of ultra performance liquid chromatography-tandem mass spectrometry (LS-HQ-MS / MS) was applied to detect five drugs, Zopiclocin, Melatonin, Chlormethazolone and Alprazolam, Analytical method. The samples were extracted with 50% methanol-water solution, purified by HLB SPE cartridge, separated on a BEH C18 column, eluted with a 0.1% formic acid aqueous solution and a 0.1% formic acid acetonitrile gradient, detected by multiple reaction monitoring mode, Quantitative. The results showed that the five drugs were effectively separated within 9 min. The correlation coefficients (R ~ 2) were all greater than 0.996 in the linear range of 0.1 ~ 50 μg / L. The average recoveries of the three samples were The average recovery of oral samples was 80.5% -100.3%, RSD was between 2.6% and 9.4%, and the detection limit (0.03-0.15) μg / kg was between 78.7% and 104.0% with RSD between 2.0% and 9.6% ; Limit of quantification (0.10 ~ 0.50) μg / kg. The method is simple, rapid and sensitive, and can be used to improve the detection of sleeping drugs in sleeping health products.