分子印迹固相萃取-液液微萃取-气相色谱法测定鱼样品中痕量环境激素  

Determination of trace amounts of environmental hormones in fish samples by molecularly imprinted solid phase extraction,liquid-liquid microextraction and gas chromatography

作　　者：操江飞 朱东湖 韦寿莲 谢春生[1,2] 陈志胜 姬鸿鹤[1,2] CAO Jiangfei;ZHU Donghu;WEI Shoulian;XIE Chunsheng;CHEN Zhisheng;JI Honghe(School of Environmental and Chemical Engineering,Zhaoqing University,Zhaoqing 526061;Guangdong Provincial Key Laboratory of Environmental Health and Resource Utilization,Zhaoqing University,Zhaoqing 526061)

机构地区：[1]肇庆学院环境与化学工程学院,肇庆526061 [2]肇庆学院广东省环境健康与资源利用重点实验室,肇庆526061

出　　处：《中国食品添加剂》2023年第10期279-286,共8页China Food Additives

基　　金：2021年肇庆市省乡村振兴战略专项资金项目(2021N001);肇庆市科技项目(202004030107);肇庆学院校级项目(202005)。

摘　　要：以题示方法测定鱼样品中痕量的双酚A(BPA)、苯胺(AN)、二苯胺(DPA)、4-氯-二甲基苯胺(CMAN)、3-氨基酚(3-AP)、苯酚(PH)等6种环境激素。以双酚A&苯胺双模板磁性分子印迹聚合物(D-MIP)为固相萃取剂,甲醇及乙酸混合溶液为洗脱剂,萃取鱼样品中6种环境激素;乙腈为分散剂,正辛醇为萃取剂,液液微萃取洗脱液,等体积甲醇稀释萃取液后进行气相色谱检测。结果表明,鱼样品经处理后基质干扰已消除,6种环境激素能有效分离。对固相萃取及液液微萃取进行了条件优化,优化结果为:洗脱剂甲醇与乙酸用量为3 mL(V甲醇∶V乙酸=8∶2),洗脱时间2 min,D-MIP用量30 mg,固相萃取时间10 min,鱼样品溶液体积50 mL;液液微萃取剂为正辛醇,正辛醇用量90μL,乙腈为分散剂,乙腈用量0.5m L,5 mL10%NaCl溶液,pH=7。在优化的条件下,6种环境激素的标准曲线的线性范围为0.1~50μg/L,检出限(3S/N)为0.1~0.5 ng/L;对空白鲫鱼肉样品进行2个浓度水平的加标回收试验,6种环境激素的回收率为86.1%~92.5%,测定值的相对标准偏差(n=3)均小于1.8%;方法用于6种鱼样品的分析,只有鲫鱼鳃含有BPA 0.1μg/kg,其他均未检出。此方法将为鱼类中环境激素的含量检测提供方法依据。Six environmental hormones(BPA、AN、DPA、CMAN、3-AP、PH)in fish samples were determined in this work.Six environmental hormones were extracted from fish samples by solid phase extraction method using D-MIP as the solid phase extractant and methanol and acetic acid mixture as the eluents.Extract was extracted from eluate by liquid-liquid micro-extraction method using acetonitrile as the dispersant and n-octanol as the extraction agent.And gas chromatography was performed after dilution of the extract of methanol in equal volumes.The results showed that the matrix interference of the fish samples was eliminated after treatment,and the six environmental hormones could be effectively separated.Conditions were optimized for solid phase extraction and liquid-liquid microextraction.The optimization results showed that the amount of eluent was 3 mL(V methanol∶Vacetic acid=8∶2),the elution time was 2 min,the dosage of D-MIP was 30 mg,the solid phase extraction time was 10 min,and the volume of fish sample solution was 50 mL;the liquid microextraction agent was n-octanol,the amount of n-octanol was 90μL,the amount of acetonitrile was dispersant,the amount of acetonitrile was 0.5 mL,5 mL10%NaCl,pH=7.Under the optimized conditions,the linear range of the six environmental hormones were 0.1〜50μg/L,and the detection limits(3S/N)were 0.1〜0.5 ng/L.The recoveries of the six environmental hormones were 86.1%〜92.5%,and the relative standard deviation(n=3)were all less than 1.8%.The method was used for the analysis of 6 kinds of fish samples,only the crucian carp gills contained BPA 0.1μg/kg,and the others were not detected.This method will provide a method basis for the detection of the content of environmental hormones in fish.

关 键 词：分子印迹聚合物 固相萃取 液液微萃取 气相色谱法 环境激素 鱼 

分 类 号：TS202.1[轻工技术与工程—食品科学] O652.1[轻工技术与工程—食品科学与工程]