螺虫乙酯·伊维菌素在梨和土壤中的残留分析方法  

A method to detect residues of spirotetramat·ivermectin in pear and soil

作　　者：熊永 万亚美 郭聪聪[1] 刘聪娇 庞民好[1] 刘颖超[1] XIONG Yong;WAN Ya-mei;GUO Cong-cong;LIU Cong-jiao;PANG Min-hao;LIU Ying-chao(College of Plant Protection,Heloei Agricultural University,Baoding 071001,China)

机构地区：[1]河北农业大学植物保护学院,河北保定071001

出　　处：《河北农业大学学报》2018年第4期82-86,共5页Journal of Hebei Agricultural University

摘　　要：为了建立梨和土壤中伊维菌素和螺虫乙酯及其代谢物螺虫乙酯烯醇(Spirotetramat-enol)、螺虫乙酯羟基(Spirotetramat-mono-hydroxy)和螺虫乙酯醇酮(Spirotetramat-keto-hydroxy)残留量的超高效液相色谱—质谱联用(UPLC-MS/MS)检测方法,样品经乙腈提取,N-丙基乙二胺(PSA)和硫酸镁为分散净化剂的QuEChERS净化,超高效液相色谱分离,多反应离子监测模式(MRM)检测,外标法定量。结果表明:添加浓度为0.005~1mg/kg范围内,伊维菌素在梨和土壤中平均回收率分别在88%~101%和93%~99%之间,相对标准偏差(RSD)分别在2.5%~3.7%和2.0%~4.4%之间,方法检出限(LOD)为5.6×10-3 ng,定量限(LOQ)为0.005mg/kg。添加浓度为0.007~1.4 mg/kg时,螺虫乙酯及其代谢物在梨和土壤中平均回收率分别为84%~109%和82%~103%,RSD分别在1.3%~5.8%和1.5%~7.5%之间,螺虫乙酯、螺虫乙酯烯醇、螺虫乙酯羟基和螺虫乙酯醇酮的LOD分别为2.2×10^(-4) ng、1.6×10^(-4) ng、8.6×10-3 ng和1.3×10^(-4)ng,LOQ值为0.007mg/kg。该方法适用于24%螺虫乙酯·伊维菌素悬浮剂在梨和土壤中残留检测,操作简便、定量准确。In order to establish a method to detect residues of ivermectin,spirotetramat and its metabolites（BYI 08330-keto-hydroxy,BYI 08330-spirotetramat-Mono-hydroxy and BYI08330-enol）in pear and soil by UPLC-MS/MS,homogenized samples were extracted with acetonitrile,cleaned up by QuEChERS cartridge with N-propyl Ethylenediamine（PSA）and magnesium sulfate as sorbent for cleaning up.Chromatographic separation was achieved by UPLC and the detection was performed by tandem mass spectrometry under the mode of multiple reaction monitoring（MRM）,the quantification analysis of external standard calibration curves was used.At concentration range from 0.005 mg/kg to 1 mg/kg,the average recovery of ivermectin in pear and soil sample was 88%~101%,93%~99%,respectively.The precision of the method in terms of relative standard deviations（RSD）ranged from 2.5%~3.7%and 2.0% ~4.4%respectively.The limit of detection（LOD）was 5.6×10-3 ng and the limit of quantitation（LOQ）was 0.005 mg/kg.At concentration range from 0.007 mg/kg to 1.4 mg/kg,the average recovery of spirotetramat and its metabolites in pear and soil ranged from84% ~109%,82%~103%,respectively.The RSD was 1.3% ~ 5.8% and 1.5%~7.5%.LODof spirotetramat and its metabolites（BYI 08330-keto-hydroxy,BYI 08330-spirotetramatMono-hydroxy and BYI 08330-enol）was 2.2×10^（-4） ng,1.6×10^（-4） ng,8.6×10-3 ng and 1.3×10^（-4） ng,respectively.The limit of quantitation（LOQ）was 0.007 mg/kg.This method is simple,accurate and reliable,and it is suitable for the determination of spirotetramat·ivermectin residues in pear and soil.

关 键 词：伊维菌素 螺虫乙酯 梨 液质联用 残留分析 

分 类 号：O623.624[理学—有机化学]