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  

Determination of 10 chemical drugs adulterated in health food for improving gastrointestinal function by UPLC-MS/MS

作　　者：赵超群[1] 李樱红 罗金文[1,2] 

机构地区：[1]浙江工业大学,杭州310014 [2]浙江省食品药品检验研究院,杭州310004

出　　处：《药物分析杂志》2014年第9期1627-1633,共7页Chinese Journal of Pharmaceutical Analysis

基　　金：浙江省分析测试科技计划项目(2012C37016)资助

摘　　要：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 UPLCMS /MS method for simultaneous determination of 10 chemical drugs illegally adulterated in health food for improving gastrointestinal function. Method：The separation and analysis was performed on a Zorbax SB C18column（ 2. 1 mm × 100 mm,1. 8 μm）. The mobile phase consisted of 0. 1%acetic acid containing 20 mmol·L1ammonium acetate and methanol with gradient elution（ 02 min,60% A,40% B; 27 min,60% A→50% A,40% B →50% B; 712 min,50% A→30% A,50% B →70% B; 1213 min,30% A→10% A,70% B→90% B; 1313. 1 min,10% A→60% A,90% B→40% B; 13. 115 min,60%A,40% B）. The column temperature was set at 35 ℃ with flow rate of 0. 2 mL·min1. 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·min1. The sheath gas temperature was 350 ℃ and the sheath gas flow rate was 11 L·min1. Results：The assay linearity of the 10 chemical drugs illegally adulterated was confirmed over 1250 times of the limit of quantification. The average recoveries（ n = 15） were 86. 9%113%,the detection limits were 0. 020. 4 ng·mL1and the relative standard deviation was less than 5%（ n = 6）. Totally 4positive 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.

关 键 词：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 超高效液相色谱串联质谱 多重反应监测 胃肠功能类保健食品 非法添加 含量测定 

分 类 号：R917[医药卫生—药物分析学]