气相色谱-质谱法测定水产品中19种氯代酚及其钠盐  

Determination of 19 Chlorophenols and Their Sodium Salts by Gas Chromatography-Mass Spectrometry in Aquatic Products

作　　者：钟惠英 柳海 柴丽月 郑丹 杨家锋 邱纪时 邱洁琼 

机构地区：[1]宁波市海洋与渔业研究院,浙江宁波315012

出　　处：《分析科学学报》2016年第3期371-376,共6页Journal of Analytical Science

基　　金：2012年宁波市海洋与渔业局专项资金资助(海洋环保3-2);"水产"浙江省重中之重学科开放基金(No.xkzsc1427);宁波市科技局农业重大项目(No.2013C11027)

摘　　要：建立了用气相色谱-质谱（GC-MS）联用法测定水产品中19种氯代酚及其钠盐的分析方法。试样用H2SO4消解后,用环己烷-乙酸乙酯提取酸解液中的氯代酚,利用酚类易溶于稀碱溶液的性质,将氯代酚提取到稀碱液中,调稀碱液pH至微酸性,用二氯甲烷-正己烷溶液萃取,无水Na2SO4脱水,浓缩定容并硅烷化衍生后,用GC-MS仪EI源选择离子模式检测,氘代4-氯-3-甲基酚（PCMC-d2）和氘代2,4,6-三溴苯酚（2,4,6-TBP-d2）为内标,内标法定量。氯代酚在2.070.0μg/L范围内,其浓度和峰面积呈良好的线性相关（r≥0.999）;水产品中添加量为1.00μg/kg、2.00μg/kg、3.00μg/kg和7.00μg/kg时,回收率一氯酚（MCP）为55.2%88.8%,二氯酚（DCP）为63.0%114%,三氯酚（TCP）为76.0%116%、四氯酚（TeCP）为78%125%,五氯酚（PCP）为83.2%104%;方法检出限在0.20.4μg/kg之间。A method is described for the determination of 19 chlorophenols and their sodium salts by GCMS in aquatic products.Chlorophenols and their sodium salts were extracted with cyclohexane-ethyl acetate solution after digestion with sulfuric acid.Chlorophenols were extracted from organic phase to dilute alkali solution,then extracted with dichloromenthane-n-hexane.The extractive liquid was dehydrated,concentrated and silylation-derivatized.Then the chlorophenols were determined by gas chromatography-mass spectrometry（GC/MS）with EI-source and selected ion monitoring（SIM）mode.The PCMC-d2 and 2,4,6-TBP-d2 were used as internal standards.The peak area and concentration of chlorophenols had a good linear correlation over the range from 2.00μg/L to 70.0μg/L.The recovery ranges of MCP,DCP,TCP,TeCP and PCP were 55.2%-88.8%,63.0%-114%,76%-116%,78%-125% and 83.2%-104%,respectively when the addition was 1.00μg/kg,2.00μg/kg,3.00μg/kg and 7.00μg/kg.The detection limits were 0.2-0.4μg/kg.

关 键 词：氯代酚 水产品 气相色谱-质谱 

分 类 号：O657.63[理学—分析化学]