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目的:建立同时测定改善胃肠功能类保健食品中10种非法添加化学药物含量的超高效液相色谱-串联质谱分析方法。方法:采用Zorbax SB-C18(2.1 mm×100 mm,1.8μm)色谱柱,以0.1%乙酸(含20 mmol·L-1乙酸铵)-甲醇为流动相,梯度洗脱(0~2 min,60%A,40%B;2~7 min,60%A→50%A,40%B→50%B;7~12 min,50%A→30%A,50%B→70%B;12~13 min,30%A→10%A,70%B→90%B;13~13.1 min,10%A→60%A,90%B→40%B;13.1~15 min,60%A,40%B),流速0.2 mL·min-1,柱温35℃;采用电喷雾电离源(ESI+),以多重反应监测(MRM)方式进行检测,喷雾电压4 kV,辅助气温度200℃,辅助气流量14 L·min-1,鞘气温度350℃,鞘气流量11 L·min-1。结果:10种化学药物在定量限到250倍定量限范围内有良好的线性关系,平均回收率(n=15)为86.9%~113%,检测限为0.02~0.4 ng·mL-1,RSD均小于5%(n=6),40批保健食品中检出4批阳性样品。结论:该方法经方法学验证,可用于测定改善胃肠功能类保健食品中芬氟拉明、西咪替丁、西布曲明、雷尼替丁、酚酞、比沙可啶、瑞巴派特、莫沙必利、多潘立酮、西沙必利10种非法添加化学药物。
Objective: To establish a method for the simultaneous determination of 10 kinds of illicitly added chemicals in gastrointestinal health food by ultra performance liquid chromatography-tandem mass spectrometry. METHODS: The mobile phase was eluted with Zorbax SB-C18 (2.1 mm × 100 mm, 1.8 μm) with 0.1% acetic acid (containing 20 mmol·L-1 ammonium acetate) 60% A, 50% A, 40% B → 50% B; 7-12 min, 50% A → 30% A, 50% B → 70% B; 12-13 min 30% A 10% A 70% B 90% B 13-13.1 min 10% A 60% A 90% B 40% B 13.1-15 min 60% A , 40% B) at a flow rate of 0.2 mL · min-1 with a column temperature of 35 ° C. The electrospray ionization source (ESI +) was used for detection by multiple reaction monitoring (MRM) The auxiliary gas flow was 14 L · min-1, the sheath gas temperature was 350 ℃ and the sheath gas flow was 11 L · min-1. Results: The 10 chemicals showed a good linearity within the limit of quantitation of 250-fold. The average recovery (n = 15) was 86.9% -113%. The detection limit was 0.02-0.4 ng · mL-1. Less than 5% (n = 6). Four batches of positive samples were detected in 40 batches of health food. Conclusion: This method is validated by methodology and can be used to determine the effect of fenfluramine, cimetidine, sibutramine, ranitidine, phenolphthalein, bisacodyl, rebamipide , Mosapride, domperidone, cisapride 10 kinds of illegal addition of chemical drugs.