超高效液相色谱-串联质谱测定保健食品中添加的10种化学药物

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，1.8 μm)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 UPLC-MS/MS method for simultaneous determination of 10 chemical drugs illegally adulterated in health food for improving gastrointestinal function. Methods: The separation and analysis was performed on a Zorbax SB C₁₈ column(2.1 mm×100 mm,1.8 μm).The mobile phase consisted of 0.1% acetic acid containing 20 mmol·L^-1ammonium acetate and methanol with gradient elution(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).The column temperature was set at 35 ℃ with flow rate of 0.2 mL·min^-1.Electrospray ionization(ESI)source was applied and operated in the positive mode.Multiple reaction monitoring(MRM)mode was used to quantify the 10 chemical drugs.The spray voltage was set at 4 kV.The auxiliary gas temperature was 200 ℃ and the auxiliary gas flow rate was 14 L·min^-1.The sheath gas temperature was 350 ℃ and the sheath gas flow rate was 11 L·min^-1. Results: The assay linearity of the 10 chemical drugs illegally adulterated was confirmed over 1-250 times of the limit of quantification.The average recoveries(n=15)were 86.9%-113%,the detection limits were 0.02-0.4 ng·mL^-1and the relative standard deviation was less than 5%(n=6).Totally 4 positive samples in the 40 batches of health food were detected. Conclusion :The established method can be used to determine 10 chemical drugs illegally adulterated in health food for improving gastrointestinal function;the chemical drugs included fenfluramine,cimetidine,sibutramine,ranitidine,phenolphthalein,bisacodyl,rebamipide,mosapride,domperidone and cisapride.