QuEChERS法前处理结合HPLC法测定苹果和土壤中二氰蒽醌的残留  

Determination and Dissipation Kinetics of Dithianon Residue in Apple and Soil by Modified QuEChERS Coupled with HPLC

作　　者：秦旭[1] 徐应明[1] 赵立杰[1] 黄青青 王林[1] 孙约兵[1] 梁学峰[1] QIN Xu;XU Yingming;ZHAO Lijie;HUANG Qingqing;WANG Lin;SUN Yuebing;LIANG Xuefeng(Agro-Environmental Protection Institute, Ministry of Agriculture, Tianjin 300191, China)

机构地区：[1]农业部环境保护科研监测所,天津300191

出　　处：《食品科学》2017年第20期273-278,共6页Food Science

基　　金：天津市农业科技成果转化与推广项目(201502290)

摘　　要：建立苹果和土壤样品中二氰蒽醌的快速提取及高效液相色谱检测法。样品采用乙腈提取,改进的QuEChERS法净化,安捷伦EclipseXDB-C_(18)色谱柱进行分离,检测波长250nm,基质匹配标准品外标法定量分析。二氰蒽醌在0.02~5.00mg/L质量浓度范围内线性关系良好,在苹果和土壤中的平均回收率为74%~92%,相对标准偏差为1.02%~6.20%,最小检出量(RSN>3)为0.005ng,检出限为0.02mg/kg。田间实验结果表明,二氰蒽醌在苹果和土壤中的消解半衰期分别为3.8~12.6d和1.0~8.3d,在收获期苹果中的残留量均低于我国规定的最大残留限量5mg/kg,推荐采收安全间隔期为14d。A method was developed for the determination of dithianon residues in apple and soil by using high performance liquid chromatography(HPLC).The residues in samples were extracted with acetonitrile,cleaned up by a modified quick,easy,cheap,effective,rugged and safe(QuEChERS)method,separated on an Agilent Eclipse XDB-C18column,and then analyzed by HPLC with variable-wavelength detection(VWD)at a wavelength of250nm.The analyte was quantified by the matrix-matched external standard method.Under the optimal conditions,the calibration curve showed good linearity in the range of0.02-5.00mg/L for dithianon.The average recoveries of dithianon were in the range of74%-92%,with relative standard deviations(RSDs)of1.02%-6.20%.The limit of detection(LOD,RSN>3)of dithianon was0.005ng,and the limit of quantitation(LOQ)was0.02mg/kg.The half-life of dithianon was3.8-12.6and1.0-8.3days in apple and soil,respectively.At harvest,apple samples were found to contain dithianon levels below the maximum residue limit(MRL)in China(5mg/kg).The harvest interval was recommended to be14days after the last application.

关 键 词：二氰蒽醌 QUECHERS 高效液相色谱 苹果 土壤 残留 

分 类 号：S432.4[农业科学—植物病理学] O656.3[农业科学—农业昆虫与害虫防治]