UHPLC-QQQ-MS法测定食品中30种非法添加调节消化功能类化合物  

Determination of 30 illegally added drugs of disgestive regulation in foods by UHPLC-QQQ-MS

作　　者：冯睿[1] 胡青[1] 孙健[1] 于泓[1] 张甦[1] 张静娴[1] 沈盈盈[1] 诸艳蓉[1] 王柯[1] 季申[1] FENG Rui;HU Qing;SUN Jian;YU Hong;ZHANG Su;ZHANG Jing-xian;SHEN Ying-ying;ZHU Yan-rong;WANG Ke;JI Shen(Shanghai Institute for Food and Drug Control,Shanghai 201203,China)

机构地区：[1]上海市食品药品检验所

出　　处：《上海预防医学》2019年第6期432-438,共7页Shanghai Journal of Preventive Medicine

基　　金：上海市科委技术服务平台(18DZ2292200);上海市科委仪器专项课题(18142202300)

摘　　要：【目的】建立了超高效液相色谱-三重四极杆质谱(UHPLC-QQQ-MS)测定食品(含保健食品)中30种调节消化功能类非法添加化合物的方法。【方法】采用WatersCORTECST3色谱柱(100mm×2.1mm,2.7μm),以乙腈-0.1%甲酸水溶液为流动相梯度洗脱分离该30种化合物,在电喷雾离子化正离子模式下,以多反应监测方式(MRM)检测。【结果】30种化合物在1~10μg/L范围内,相关系数(r^2)均大于0.99;除美沙拉嗪等5种基质效应较明显的化合物,其余在定量限1倍、2倍、10倍添加水平下的平均加标回收率为80.1%~116.6%,相对标准偏差(RSD)为0.7%~8.8%(n=6);检出限为25μg/kg。【结论】本方法专属、灵敏、高效,可用于调节消化功能类非法添加化合物的检测,填补了调节消化功能类非法添加化合物方法上的空白,可有效打击类该药物的非法添加行为。[Objective]An analytical method was developed for the determination of 30 digestive system drugs in foods and dietary supplements by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry(UHPLC-QQQ-MS).[Methods]A Waters CORTECS T3 column(100 mm×2.1 mm,2.7μm)was used with acetonitrile and 0.1%formic acid aqueous solution as mobile phases by gradient elution for separation of 30 compounds.All the compounds were detected by electrospray ion souce in positive mode with multiple reactions monitoring(MRM)mode.[Results]The calibration curves showed good linearities for the 30 compounds during the range of 1-10μg/L.The correlation coefficients of the standard calibration curves for the 30 compounds were all above 0.99.The recoveries of the drugs at spiked levels of limits of quantitation(LOQs),double LOQs,ten times of LOQs were at the range of 80.1%~116.6%with the RSDs between 0.7%and 8.8%(n=6),except for the 5 compounds such as mesalazine with strong matrix effects.The LODs were 25μg/kg for the 30 compounds.[Conclusion]The method proves to be sensitive and accurate for the determination of the digestive system drugs.This method fills the gap of the determination of the digestive system drugs,which strikes illegal adulteration behavior effectively.

关 键 词：超高效液相色谱-三重四极杆质谱 非法添加 调节消化功能类 食品 

分 类 号：R155.5[医药卫生—营养与食品卫生学]