新型亲水性SPE-HPLC联用检测猪肉中四类农兽药残留

Detection of Four Kinds of Pesticide Residues in Pork by New Hydrophilic SPE-HPLC

采用本体聚合的方法制备了针对磺胺类、磺酰脲类、雌激素及氨基甲酸酯类农兽药残留具有选择性的亲水性固相萃取材料,建立固相萃取-高效液相色谱联用技术检测猪肉中四类农兽药残留的方法。该方法对磺胺类、磺酰脲类、雌激素和氨基甲酸酯类的最低检出限范围分别为0.39~2.77,5.82~39.00,4.28~6.66和2.11μg/kg。优化了影响富集效果的因素,包括样品pH、洗脱剂种类及体积。结果表明,最佳固相萃取条件:上样pH 3.45,洗脱剂为1 mL的二氯甲烷-甲醇(1︰1,V/V),1 mL丙酮-甲醇(1︰1,V/V)和1 mL氨水-甲醇(1︰1,V/V),洗脱液体积3 mL。对样品进行10,15和20μg/kg的加标回收,回收率在64.99%~117.69%,RSD在1.12%~9.84%(n=3)。该方法对磺胺类、磺酰脲类、雌激素及氨基甲酸酯类农兽药具有良好的富集和检测作用。

A selective hydrophilic solid phase extraction material was prepared by bulk polymerization for the detecting of sulfonamides, sulfonylureas, estrogens and carbamates pesticide residues. The solid phase extraction-high performance liquid chromatography technique was established for the detection of four kinds of veterinary drugs in pork. The detection limits of the sulfonarnides, sulfonylureas, estrogens and carbamates were 0.39-2.77, 5.82-39.00, 4.28-6.66 and 2.11 μg/kg, respectively. Optimize the factors affecting the enrichment effect, including the pH of the sample, the type and volume of the eluent. The results showed that the best solid phase extraction condition were pH 3.45, 1 mL of dichloromethane- methanol （1 ： 1, V/V）, 1 mL of acetone-methanol （1 ： 1, V/V） and 1 mL of aqueous ammonia-methanol （1 ： 1, V/V）, eluent volume of 3 mL. The samples were collected at 10, 15 and 20 μg/kg, the recovery rate between 64.99%-117.69%, and RSD between 1.12%-9.84% （n=3）. The method was good for enrichment and detection of sulfonamides, sulfonylureas, estrogens and carbamate veterinary drugs.