摘要
目的建立超高效液相色谱-串联质谱同时测定减肥类食品中55种非法添加物的分析方法。方法样品经甲醇超声提取后,采用Agilent Eclipse Plus C18 RRHD色谱柱(2.1 mm×100 mm,1.8μm)分离,以乙腈-0.1%甲酸为流动相进行梯度洗脱。在正负离子扫描条件下,采用动态多反应监测模式监测。结果55种非法添加药物在相应的线性范围内均呈现良好线性关系,相关系数大于0.995,平均回收率75.2%~121.6%,相对标准偏差<12%,各化学药物的检测限在0.02~1.25μg/g。应用该方法对50批样品进行了检测,其中有38批次样品检出托拉塞米、大黄素、西布曲明、N-单去甲基西布曲明、N,N-双去甲基西布曲明、比沙可啶、麻黄碱、甲基麻黄碱、氢氯噻嗪、氟西汀等非法添加物。结论该方法简单、快速、灵敏、准确、高效,兼具定性定量检测的优点,可用于食品中减肥类化学药物的高通量检测。
Objective To establish an analytical method for simultaneous determination of 55 illegal addition of compounds in doet foods by ultra-performance liquid chromatography tandem mass spectrometry.Methods After ultrasonic extraction with methanol,the samples were separated on Agilent Eclipse Plus C18 RRHD column(2.1 mm×100 mm,1.8μm)with gradient elution using a mobile phase of 0.1%formic acid aqueous solution and acetonitrile.Under positive and negative ion scanning conditions,dynamic multiple-reaction monitoring mode was used for monitoring.Results The 55 illegal addition of compounds showed good linear relationship in the corresponding linear range with all the correlation coefficient greater than 0.995.The average recoveries were 75%-125%,and the relative standard deviations were less than 12%,the LODs were all in the range of 0.02-1.25μg/g.Fifty batches of samples were tested by this method.Fluoxetine,sibutramine,N-monodesmethyl sibutramine,N-didesmethyl sibutramine,bisacodyl,torasemide were detected in 38 samples.Conclusion This method is simple,rapid,sensitive,efficient and accurate,which can be widely applied in the high-throughput detection of illegally added chemicals in different kinds of diet foods matrices.
作者
胡紫艳
金鑫
张玲
HU Ziyan;JIN Xin;ZHANG Ling(Nanjing Institute for Food and Drug Control,Jiangsu Nanjing 210000,China)
出处
《中国食品卫生杂志》
CSCD
北大核心
2023年第1期38-48,共11页
Chinese Journal of Food Hygiene
