超高效液相色谱-高分辨质谱法快速筛查确证调味品中的19种非食用物质  

Screening of 19 kinds of illegal chemical dyes in condiments by ultra performance liquid chromatography-linear ion trap-orbitrap high resolution mass spectrometry

作　　者：徐琴[1] 吕宁[1] 郝鹏飞[1] 孟慧琴[1] 徐丽[1] 修晓丽[1] 罗忻[1] 

机构地区：[1]山东出入境检验检疫局检验检疫技术中心,青岛266002

出　　处：《食品安全质量检测学报》2017年第11期4174-4183,共10页Journal of Food Safety and Quality

摘　　要：目的建立超高效液相色谱-高分辨质谱法检测调味品中19种非食用物质的分析方法。方法样品经乙酸乙酯-环己烷提取,采用凝胶渗透色谱(gel permeation chromatography,GPC)净化与在线定量浓缩,然后经C_(18)色谱柱分离,乙腈和5 mmol/L乙酸铵(含0.1%甲酸)溶液梯度洗脱后经超高效液相色谱-线性离子阱/静电场轨道阱高分辨质谱(ultra performance liquid chromatography-linear ion trap-orbitrap high resolution mass spectrometry,UPLC-LTQ-orbitrap MS)测定。结果 19种目标物在15 min内实现良好分离,线性相关系数均≥0.996,定量限(limit of quantitation,LOQ)为5~15μg/kg,加标回收率在61.9%~105.8%之间,相对标准偏差(relative standard deviation,RSD)为2.3%~12.9%。结论本研究建立的方法准确、简单,可适用于调味品中19种非食用物质的定性定量及确证分析。Objective To establish a method for the determination of 19 kinds of illegal chemical dyes in condiments by the ultra performance liquid chromatography-linear ion trap-orbitrap high resolution mass spectrometry（UPLC-LTQ-Orbitrap MS）. Methods The samples were extracted with ethyl acetate-cyclohexane and purified by gel permeation chromatography（GPC） and online quantitative enrichment, and then were separated by the C_（18） column, and detected by UPLC-LTQ/Orbitrap MS after gradient elution of 5 mmol/L ammonium acetate aqueous solution containing 0.1% formic acid finally. Results Nineteen targets were well separated in 15 min with the correlation coefficients above 0.996, and the limits of quantification（LOD） were 5-15 μg/kg. The recoveries were 61.9%-105.8%, with the relative standard deviations of 2.3%-12.9%. Conclusion The established method is accurate and simple, which can be used in the qualitative and quantitative analysis of 19 kinds of non-edible substances in the condiment.

关 键 词：线性离子阱静电场轨道阱 高分辨质谱 凝胶渗透色谱 调味品 非食用物质 

分 类 号：O657.63[理学—分析化学] TS264[理学—化学]