气相色谱法测定水产品中五氯苯酚及其钠盐残留量  

Determination of pentachlorophenol and its sodium salt residues in aquatic product by gas chromatography

作　　者：朱晓华[1,2,3] 吴燕如[4] 王凯[1,2,3] 宋红波[1,2,3] 封莉[5] 吴光红[1,2,3] 

机构地区：[1]江苏省水产质量检测中心,江苏南京210017 [2]农业部渔业产品质量监督检验测试中心(南京),江苏南京210017 [3]江苏省淡水水产研究所,江苏南京210017 [4]中国药科大学药学院,江苏南京210009 [5]南京农业大学食品科技学院,江苏南京210095

出　　处：《江苏农业学报》2011年第1期188-194,共7页Jiangsu Journal of Agricultural Sciences

基　　金：江苏省科技公共服务平台(BM2008158)

摘　　要：为准确分析罗非鱼、青虾、中华绒螯蟹、鳕鱼可食部分中五氯苯酚及其钠盐残留量,通过比较前处理方法中提取溶剂正己烷提取次数、加标样品-20℃保存3 d后不同提取方式对回收率的影响及不同衍生操作方式对衍生效果的影响和色谱检测条件的改进,建立了罗非鱼、青虾、中华绒螯蟹、鳕鱼可食部分中五氯苯酚及其钠盐残留量的气相色谱检测方法。结果表明:样品中的五氯苯酚及其钠盐在酸性介质中用匀浆机分散均匀,正己烷提取2次,再用碳酸钾溶液反萃取,萃取物以乙酸酐衍生生成五氯苯乙酸酯,用正己烷提取衍生物后,HP-5(30 m×0.32 mm×0.25μm)色谱柱分离,用配备微池电子捕获检测器的气相色谱测定。该方法在0.2～100.0μg/L范围内线性关系良好,相关系数r=0.999 7。最低检测限为0.6～1.0μg/kg,定量限为3.0～5.0μg/kg。在加标水平为2.0μg/kg、5.0μg/kg、10.0μg/kg时五氯苯酚回收率为76.1%～106.4%,相对标准偏差为4.0%～13.3%。前处理简便,易于操作,适合批量水产品样品中五氯苯酚及其钠盐残留量的测定。The method of gas chromatography for the accurate detection of pentachlorophenol in edible tissues of tilapia,freshwater shrimp,chinese mitten crab and cod were established by comparing the effects of n-hexane extraction times,methods of extraction on recoveries and derivative mode of operation for pentachlorophenol in sample pretreatments and optimizing the chromatographic conditions.The results showed that the target compounds were first extracted two times with n-hexane in an acidic medium,and then back extracted with potassium carbonate solution.The extract was derivatized with acetic anhydride,and the derivative was extracted with n-hexane.Finally,the gas chromatography with HP-5（30 m × 0.32 mm × 0.25 μm） column and the micro-cell electron capture detector was used for the determination.The working curves were linear（r=0.999 7） in the range of 0.2-100.0 μg/L.The detection limit of gas chromatography for pentachlorophenol was 0.6-1.0 μg/kg,the limit of quantitatition was 3.0-5.0 μg/kg.When spiked with 2 μg/kg,5 μg/kg and 10 μg/kg of pentachlorophenol,the average recoveries of pentachlorophenol were 76.1 %-106.4 % and the relative standard deviation（RSD） were 4.0 %-13.3 %.This method for gas chromatography,which was simple in preparation and easy in operation,would be suitable for determination of pentachlorophenol in groups of aquatic product samples.

关 键 词：水产品 五氯苯酚 残留 气相色谱 

分 类 号：TS254[轻工技术与工程—水产品加工及贮藏工程]