分子印迹固相萃取-同位素稀释气相色谱质谱法测定肉制品中16种欧盟优控多环芳烃
Determination of 16 European priority polycyclic aromatic hydrocarbons in meat products by the molecularly imprinted solid phase extraction-isotope dilution-gas chromatography mass spectrometry
鞠香 1陈克云 1李海霞 1陈倩倩 1王艳丽 1梁秀清 1刘艳明 1汪勇2
作者信息
- 1. 山东省食品药品检验研究院,国家市场监管重点实验室(肉及肉制品监管技术),产业技术基础公共服务平台,济南,250101
- 2. 岛津企业管理(中国)有限公司,上海,210005
- 折叠
摘要
摘 要 结合分子印迹固相萃取对多环芳烃的特异性净化,建立了同位素稀释气相色谱质谱法测定肉制品中16种欧盟优控多环芳烃的分析方法.样品加入7种氘代同位素内标,经正己烷+二氯甲烷(7∶3,V/V)混合溶液提取,分子印迹固相萃取柱净化,选择离子监测模式(SIM)下采集.在1.0-200 ng·mL-1范围内,16种欧盟优控多环芳烃线性相关系数(r)均大于0.9990,不同加标浓度下,回收率为87.1%-114.8%,相对标准偏差(RSDs)(n=6)在1.0%—5.5%范围内,方法的检出限为0.2-0.3 μg·kg-1,定量限为0.6-0.9 μg·kg-1.方法前处理简单高效,灵敏度高,适用大批量肉制品中多环芳烃的快速测定.
Abstract
Based on the specific purification of the molecularly imprinted solid phase extraction,a method for the determination of 16 EU priority polycyclic aromatic hydrocarbons(PAHs)in meat products by isotope dilution-gas chromatography mass spectrometry was established.Seven deuterium isotope internal standards were added to the samples,which were extracted by a mixture of n-hexane-dichloromethane(7:3,V/V).The samples were purified by the molecular imprinting column,separated by the DB-EUPAH column,collected in select ion monitoring mode(SIM),and quantified by the internal standard method.In the range of 1.0-200 ng·mL-1,the linear correlation coefficients(r2)were all greater than 0.9990,the average recoveries were in the range of 87.1%—114.8%and the relative standard deviations(RSDs)(n=6)were ranged from 1.0%to 5.5%.The detection limits of the method were 0.2-0.3 μg·kg-1 and the limits of quantification were 0.6-0.9 μg·kg-1 respectively.The method is simple,efficient,sensitive and suitable for the rapid determination of the EU PAHs in meat products.
关键词
欧盟优控多环芳烃/气相色谱质谱法/同位素稀释/分子印迹柱/肉制品Key words
European priority polycyclic aromatic hydrocarbons/gas chromatography mass spectrometry/isotope dilution/molecularly imprinted solid phase extraction/meat products引用本文复制引用
基金项目
山东省药品监督管理局科研项目(SDNMPAFZLS202301)
出版年
2024