SPE-GC/MS外标法测定水产品中4种丁香酚类麻醉剂  

Determination of 4 Eugenol Derivatives in Aquatic Products by SPE-GC/MS Analysis

作　　者：高平 陈日檬 黄武 黄和[3] 曾丹丹 刘唤明[3] 陈营寿 周凯 颜珲璘 GAO Ping;CHEN Ri-meng;HUANG Wu;HUANG He;ZENG Dan-dan;LIU Huan-ming;CHEN Ying-shou;ZHOU Kai;YAN Hui-lin(Zhanjiang Institute for Food and Drug Control,Zhanjiang 524022,China;Zhangjiang Customs Technology Center,Zhanjiang 524001,China;College of Food Science and Technology,Guangdong Ocean University,Zhanjiang 524088,China)

机构地区：[1]湛江市食品药品检验所,广东湛江524022 [2]湛江海关技术中心,广东湛江524001 [3]广东海洋大学食品科技学院,广东湛江524088

出　　处：《食品工业科技》2019年第18期229-233,共5页Science and Technology of Food Industry

基　　金：广东省食品药品监督管理局食品药品检验检测技术创新专项(2015ZX04);广东省科技计划项目(2014A020208121);湛江市科技计划项目(2017A02001);湛江市海洋经济创新发展示范市建设项目(湛海创2017C8B1)

摘　　要：建立了固相萃取/气相色谱-质谱法(GC-MS)测定水产品中4种丁香酚类(丁香酚、异丁香酚、甲基丁香酚和甲基异丁香酚)麻醉剂的分析方法。样品采用正己烷-丙酮混合液(3∶1,v/v)提取,乙二胺-N-丙基硅烷(PSA)净化,浓缩后再经硅胶固相萃取柱净化,采用GC-MS测定,外标法定量。结果表明:4种丁香酚类麻醉剂在5.0~200 ng/mL范围内均呈现良好线性关系,相关系数均大于0.998,方法检出限(S/N=3)均为3.0μg/kg,方法定量限(S/N=10)均为10.0μg/kg。空白水产品样品在0.01、0.05、0.20 mg/kg等3个加标水平时,4种目标物的平均加标回收率为85.7%~102.5%,相对标准偏差(RSD)为3.3%~9.8%。此方法净化效果较好,灵敏度高,适合水产品中4种丁香酚类麻醉剂的定性和定量分析。A method for determination of four eugenol derivatives(eugenol,iso-eugenol,methyl eugenol and methyl iso-eugenol)in aquatic products by gas chromatography-mass spectrometry with solid-phase extraction(SPE-GC/MS)was established.The samples were extracted with N-hexane-acetone mixture(3∶1,v/v).The extract was cleaned up with silica solid phase extraction column after being purified by PSA and concentrated.The target compounds were detected by GC-MS with SIM mode.The external standard method was applied for quantitative analysis.As a result,The calibration curves of four eugenol derivatives showed good linearity in the range of 5.0~200 ng/mL with correlation coefficients(r)was over 0.998.The limits of detection(LOD)and the limits of qualification(LOQ)were 3.0,10.0μg/kg,respectively.When the spiked concentrations were 0.01,0.05,0.20 mg/kg,the average recoveries of four target compounds were of 85.7%~102.5%with the relative standard deviations(RSD)of 3.3%~9.8%.This method was suitable for determination of four eugenol derivatives in aquatic products qualitatively and quantitatively with satisfactory purification effect and sensitivity.

关 键 词：固相萃取 气相色谱-质谱 丁香酚 甲基丁香酚 异丁香酚 甲基异丁香酚 水产品 

分 类 号：TS254.7[轻工技术与工程—水产品加工及贮藏工程]