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目的建立超高效液相飞行串联质谱(ultra performance liquid chromatography/time-of-flight mass spectrometry,UPLC-Q-TOF-MS-MS)快速检测改善睡眠类保健食品中22种违法添加化学物质的方法。方法样品经甲醇提取后,采用超高效液相色谱/质谱测定法,以ACQUITYTM UPLC HSS T3(50 mm×1.8 mm×1.7μm)为分析柱,0.1%甲酸溶液-乙腈为流动相进行梯度洗脱,电喷雾电离(ESI),正、负离子模式进行质谱数据采集,对改善睡眠类保健食品中22种违法添加化学物质进行筛选分析。结果建立了快速分离检测保健食品中22种非法添加物质的测定方法,22种违法添加化学物质的色谱图分离度良好,检测限均低于1 ng,质谱分辨率符合鉴别要求。结论该方法专属性强、灵敏度高,快捷,可作为改善睡眠类违法添加药物的有效检测方法。
OBJECTIVE To establish a rapid method for the determination of 22 illegal substances in sleep-type health food by ultra performance liquid chromatography / time-of-flight mass spectrometry (UPLC-Q-TOF-MS-MS) Methods The samples were extracted with methanol and analyzed by ultra performance liquid chromatography / mass spectrometry with ACQUITY UPLC HSS T3 (50 mm × 1.8 mm × 1.7 μm) column and gradient elution with 0.1% formic acid-acetonitrile as mobile phase , Electrospray ionization (ESI), positive and negative ion mass spectrometry data acquisition, to improve the sleep health food 22 kinds of illegal addition of chemicals for screening analysis. Results The method for determination of 22 illegal additives in fast food was established. The chromatograms of 22 illegal chemicals were well separated, the detection limits were less than 1 ng, and the MS resolution was consistent with the identification requirements. Conclusion The method is highly specific, sensitive and fast, and can be used as an effective method to improve illegal drug addition in sleep disorders.