高效液相色谱法同时测定水产品中4种酰胺类农药残留  

Analyses of Four Amide Residues in Aquatic Products by High Performance Liquid Chromatography

作　　者：刘伶俐[1,2] 徐飞良 黄向荣 索纹纹 万译文[1] LIU Ling-li;XU Fei-liang;HUANG Xiang-rong;SUO Wen-wen;WAN Yi-wen(Hunan Fisheries Science Research Institute, Changsha 410153, China;Ministry of Agriculture and Rural’s Test Center for Fishery Products Quality Supervision and Inspection in Changsha, Changsha 410153, China;Hunan Provincial Feed Industry Office, Changsha 410011, China;Collaborative Innovation Center for Efficient and Health Production of Fisheries in Hunan, Changde 415000, China)

机构地区：[1]湖南省水产科学研究所,中国长沙410153 [2]农业农村部渔业产品质量监督检验测试中心(长沙),中国长沙410153 [3]湖南省饲料工业办公室,中国长沙410011 [4]水产高效健康生产湖南省协同创新中心,中国常德415000

出　　处：《湖南师范大学自然科学学报》2021年第3期68-73,共6页Journal of Natural Science of Hunan Normal University

基　　金：湖南省科技重大专项资金资助项目(2017NK1030)。

摘　　要：为建立水产品中氯虫苯甲酰胺、氟虫双酰胺、唑虫酰胺和氟啶虫酰胺残留量的检测方法,样品经乙腈提取、碱性氧化铝柱净化、收集流出液、平行蒸发仪旋蒸浓缩,用乙腈-乙酸铵水溶液(体积比60∶40)溶解残留物,过0.22μm滤膜后待测。采用Waters T3色谱柱,以乙腈-0.1 mol·L^(-1)乙酸铵缓冲液等度洗脱、UV检测器测定、外标法定量。在优化条件下,4种酰胺类的线性范围均为0.05~5.0 mg·L^(-1),线性相关系数均不低于0.9999。氯虫苯甲酰胺、氟啶虫酰胺及氟虫双酰胺的检出限均为0.1μg·g^(-1),唑虫酰胺的检出限为0.2μg·g^(-1)。水产品中氟啶虫酰胺、氯虫苯甲酰胺和氟虫双酰胺在0.1,0.5,1.0μg·g^(-1)时回收率为99.5%~110.5%,RSD值为1.53%~3.93%;唑虫酰胺在0.2,1.0,2.0μg·g^(-1)时回收率为93.7%~109.4%,RSD值为0.83%~3.14%。该方法简便、高效、精密度高,适用于水产品中氯虫苯甲酰胺、氟虫双酰胺、唑虫酰胺和氟啶虫酰胺残留量的测定。To establish a method for the determination of chlorantraniliprole,flubendiamide,tolfenpyrad and flonicami eresidues in aquatic products,in this study,samples were extracted by acetonitrile and purified by the alkaline alumina column with the effluent separately collected.The solution was then evaporated to dryness by parallel evaporation and the power was redissolved with acetonitrile-ammonium acetate aqueous solution(60∶40,by volume).Then the solution was filtered by 0.22 microns filter membrane,followed by using the waters T3 column and acetonitrile-0.1 mol·L^(-1)ammonium acetate buffer solution system by isoelution.The purity of the product was determined by a UV detector and quantified by the external standard method.Strong linearities were obtained for the concentration range of 0.05~5.0 mg·L^(-1)for chlorantraniliprole,flubendiamide,tolfenpyrad and flonicamie,with the correlation coefficients no less than 0.9999.The detection limit of chlorantraniliprole,flonicamie and flubendiamide was 0.1μg·g^(-1),whereas of tolfenpyrad was 0.2μg·g^(-1).The recovery for flonicamie,chlorantraniliprole and flubendiamide at the fortified level of 0.1,0.5,1.0μg·g^(-1)was between 99.5%~110.5%,with their relative standard deviation(RSD)in the range of 1.53%~3.93%.The recoveries for tolfenpyrad at fortified levels of 0.2,1.0,2.0μg·g^(-1)were in the range of 93.7%~109.4%,with RSDs between 0.83%~3.14%.Based on these results,we conclude that our present method is simple,efficient,accurate,and suitable for the determination of chlorantraniliprole,flubendiamide,tolfenpyrad and flonicamie in aquatic products.

关 键 词：水产品 氯虫苯甲酰胺 氟虫双酰胺 唑虫酰胺 氟啶虫酰胺 残留 高效液相色谱法 

分 类 号：O657.63[理学—分析化学]