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当前位置: 首页 > 文章 > 气相色谱-串联质谱法检测水产品运输水和暂养水中丁香酚残留 中国渔业质量与标准 2019 (1) 56-63
Position: Home > Articles > Determination of eugenol residues in transport water and temporary water for aquatic products by gas chromatography-tandem mass spectrometry Chinese Fishery Quality and Standards 2019 (1) 56-63

气相色谱-串联质谱法检测水产品运输水和暂养水中丁香酚残留

作  者：
王正全;倪玲;谢庆超;齐自元;刘源;汪立平;赵勇;王锡昌;谢晶
单  位：
农业部冷库及制冷设备质量监督检验测试中心(上海);上海海洋大学食品学院;农业部水产品贮藏保鲜质量安全风险评估实验室(上海)
关键词：
丁香酚;气相色谱-串联质谱;水体;前处理;残留;检测;基质分散固相萃取;内标法
摘  要：
建立了流通环节中水产品运输和暂养水样中丁香酚残留的气相色谱-串联质谱检测方法。运输和暂养水样经固相分散基质萃取,再逐步经聚合氧化铝(PAC)、N-丙基乙二胺(PSA)和氯化钠(Na Cl)净化后,用二氯甲烷和正己烷萃取,然后浓缩至干并定容检测,采用电喷雾(ESI)正离子模式同时扫描,选择反应监控模式(SRM)配合基质匹配溶液内标法定量检测。结果显示:本方法的丁香酚检出限(LOD)为0. 5μg/L,其定量限(LOQ)为1. 5μg/L;在LOQ添加水平时,信噪比S/N为10. 95,并在1. 5～50. 0μg/L线性范围内,回收率为82. 3%～109. 9%,RSD <6. 9%;线性回归方程为Y=-0. 006 424+0. 000 391 7X,相关系数r为0. 993 6。本方法简单、稳定、灵敏、省时,能够满足实际检测需要,适用于环境水样等复杂基质检验检测。为验证本方法的检测可行性,已将本方法应用于2014年排查的沪浙闽地区18个运输水样和26个暂养水样的检测,阳性检出率大于20%,为水产品质量监控提供了技术支持。
译  名：
Determination of eugenol residues in transport water and temporary water for aquatic products by gas chromatography-tandem mass spectrometry
作  者：
WANG Zhengquan;NI Ling;XIE Qingchao;QI Zi Yuan;LIU Yuan;WANG Liping;ZHAO Yong;WANG Xichang;XIE Jing;College of Food Science and Technology,Shanghai Ocean University;Laboratory of Quality and Safety Risk Assessment for Aquatic Product on Storage and Preservation ( Shanghai) ,Ministry of Agriculture;Quality Supervision,Inspection and Testing Center for Cold Storage and Refrigeration Equipment( Shanghai) ,Ministry of Agriculture;
单  位：
Shanghai
关键词：
eugenol;;gas chromatography-tandem mass spectrometry(GC-MS/MS);;transport and temporary water;;pretreatment;;residue;;inspection;;matrix solid phase dispersion;;internal standard method
摘  要：
A method of gas chromatography-tandem mass spectrometry( GC-MS/MS) was established for the determination of eugenol residues in transport water and temporary water during the transportation circulation of aquatic products. The samples were prepared by a simple solid phase dispersion matrix method with successively purifying using sorbents including polyaluminum chloride( PAC),primary secondary amine( PSA) and sodium chloride( NaCl),followed with organic solvent extraction with dichloromethane and n-hexane,and then the organic solvent layer was directly concentrated to dryness for detection. The eugenol residues were determined using the positive electrospray ionization( ESI) mode with select reaction monitor( SRM) mode and calculated by internal standard method with matrix matching. The results showed that the limit of detection( LOD) for eugenol was 0. 5 μg/L,and the limit of quantitation( LOQ) was 1. 5 μg/L,at the signal-to-noise ratio( S/N) of 10. 95. The recoveries were maintained at 82. 3%-109. 9% with a linear range of 1. 5-50. 0 μg/L,the relative standard deviation( RSD) was less than 6. 9%,and the linear regression equation is Y =-0. 006 424 + 0. 000 391 7X with the correlation coefficient r of 0. 993 6. This method was simple,stable,sensitive,time-saving and was considered to be capable of meeting the actual needs for residue analysis in complex matrix such as environmental water samples. In order to demonstrate the availability of this method,it was applied to the investigation of 18 transport water samples and 26 temporary water samples from Shanghai,Zhejiang and Fujian in 2014. The positive rate was more than 20%,which was worth paying attention to the eugenol residual problem.

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