气相色谱法测定水产品有机氯农药和多氯联苯  

Determination of Organochlorine Pesticides and Polychlorinated Biphenyls in Aquatic Products by Gas Chromatography

作　　者：许仁杰[1,2] 蔡春平[2] 丁立平 陈丽叶[1] 方婷[1] 陈锦权[1] 

机构地区：[1]福建农林大学食品科学学院,福州350001 [2]福建出入境检验检疫局技术中心,福州350001 [3]福清出入境检验检疫局技术中心,福清350300

出　　处：《食品工业》2017年第3期287-292,共6页The Food Industry

基　　金：国家质检总局科技项目(2015IK033);国家自然科学基金(31401597);福建出入境检验检疫局科技项目(FK2013-19);福建省科技计划项目(2016Y0085);福建省高水平大学建设项目"海洋生物资源综合加工及安全风险评估工程研究中心"(612014043);2015年中青年教师教育科研项目杰出人才计划

摘　　要：建立了同时测定水产品中有机氯农药和多氯联苯残留量的双重净化-气相色谱法。样品以二氯甲烷-正己烷(1∶1)混合溶剂提取,再经浓硫酸和焙烧型水滑石双重净化后采用气相色谱分析和外标法定量。结果表明,在10~200μg·kg^(-1)浓度范围内,7种多氯联苯、4种六六六和2种滴滴涕线性关系好,相关系数r>0.999。方法的检测限(LOD)和定量限(LOQ)范围分别为0.14~0.68μg·kg^(-1)和0.47~2.27μg·kg^(-1)。在海捕虾、鲳鱼及花蛤空白样品中添加10,20和100μg·kg^(-1)3个水平的7种多氯联苯、4种六六六和2种滴滴涕,加标回收率范围为81.04%~106.10%,相对标准偏差(RSD)范围为1.23%~5.97%。该方法操作简便快速、准确度和灵敏度高,可满足水产品中有机氯农药和多氯联苯残留量的同时测定。A double depuration-gas chromatography（GC） method was developed to simultaneously determine the residues of organochlorine pesticides（hexachlorocyclohexanes and dichlorodiphenyltrichloroethanes） and polychlorinated biphenyls（PCBs） in aquatic products. The samples were extracted by the mixture of methylene chloride-n-hexane（1∶1）, double purified by concentrated sulfuric acid and calcined hydrotalcite, and then analyzed by GC and quantified with external standard method. Results indicated that good linearities were obtained for seven PCBs, four hexachlorocyclohexanes（BHCs） and two dichlorodiphenyltrichloroethanes（DDTs） with correlation coefficients greater than 0. 999 in the range of 10-200 μg·kg^（-1）. The limits of detection（LOD） and limits of quantitation（LOQ） for GC method were 0.14-0.68 μg·kg^（-1） and 0.47-2.27 μg·kg^（-1）, respectively. At three spiked levels of 10, 20 and 100 μg·kg^（-1）, the spiked recoveries of seven PCBs, four BHCs and two DDTs from shrimp, butterfish and clam ranged from 81.04% to 106.10%, and the relative standard deviation（RSD） ranged from 1.23% to 5.97%. The method was simple, with high accuracy and sensitivity, it was suitable for simultaneously determining the residues of organochlorine pesticides（BHCs and DDTs） and PCBs in aquatic products.

关 键 词：水产品 六六六 滴滴涕 多氯联苯 气相色谱法 

分 类 号：O657.71[理学—分析化学]