液质联用法测定蔬菜、水果、土壤中的溴氰虫酰胺残留
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摘要
建立了一种超高效液相色谱-电喷雾电离串联质谱法测定蔬菜、水果和土壤中的溴氰虫酰胺残留的方法。试样经QuEChERS方法前处理,超高效液相色谱-电喷雾电离串联质谱法测定,外标法定量。溴氰虫酰胺在0.5-200μg/L有良好的线性关系,相关系数r>0.999,检出限为0.15μg/kg,定量下限为0.5μg/kg,加标回收率在70%-110%,相对标准偏差小于5.0%,该方法简便、可靠、稳定,灵敏度高,可用于分析蔬菜、水果和土壤中溴氰虫酰胺的残留量。
The extraction and purification improvements of the QuEChERS method combining with LC-MS-MS was devel?oped for the determination of cyantraniliprole in vegetables,fruits and soils.The procedure was validated based on the SAN-CO European Guidelines with satisfactory spiked recovery of 70%-110% and measurement standard deviation less than 5%.The results showed that the calibration curves were linear in the range of 0.5 μg/L-200 μg/L with correlation coefi?cient more than 0.999. The limit of detection was 0.15 μg/kg,and the limit of quantitation was 0.5 μg/kg.The method was simple,rapid and accurate and could meet the requirement of the maximum residue limits for cyantraniliprole in vegeta?bles,fruits and soils.
The extraction and purification improvements of the QuEChERS method combining with LC-MS-MS was devel?oped for the determination of cyantraniliprole in vegetables,fruits and soils.The procedure was validated based on the SAN-CO European Guidelines with satisfactory spiked recovery of 70%-110% and measurement standard deviation less than 5%.The results showed that the calibration curves were linear in the range of 0.5 μg/L-200 μg/L with correlation coefi?cient more than 0.999. The limit of detection was 0.15 μg/kg,and the limit of quantitation was 0.5 μg/kg.The method was simple,rapid and accurate and could meet the requirement of the maximum residue limits for cyantraniliprole in vegeta?bles,fruits and soils.
引文
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[7]王耀,刘少斌,谢翠美,等.加速溶剂萃取凝胶渗透色谱/固相萃取净化气相色谱质谱法测定咸鱼中有机磷农药残留[J].分析化学,2011,39(1):67-71.
[8]许秀丽,李礼,丁罡斗,等.大米中13种有机磷农药的固相萃取结合大体积进样/气相色谱-质谱法快速分析[J].分析测试学报,2008,27(1):23-26.
[9]钱程,吴琼,吕岱竹,等.超高效液相色谱-串联质谱法测定豇豆中溴氰虫酰胺等5种农药残留[J].农药学学报,2014,16(5):594-599.
[2]黄宝勇,潘灿平,张微,等.应用分析保护剂补偿基质效应与气相色谱-质谱快速检测果蔬中农药多残留[J].分析测试学报,2006,25(3):11-13.
[3]Anastassiades M,Lehotay S J,Smjnbaher D,et a1.Fast andeasy multiresidue method employing aeetonitrileextraction/partitioning and dispersive sohd-phaseextraction for the determination of pesticide residues inproduce[J].J AOAC INT,2003(86):412-431.
[4]杨桂秋,黄琦,陈霖,等.新型杀虫剂溴氰虫酰胺研究概述[J].世界农药,2012,34(6):19-21.
[5]王小瑜.蔬菜中有机磷农药残留快速检测方法的研究[D].淄博:山东理工大学,2001(2):1-10.
[6]苏建峰.猪肉中63种有机磷农药的气相色谱筛选与气质联用确证方法[J].分析测试学报,2008,27(12):1298-1302.
[7]王耀,刘少斌,谢翠美,等.加速溶剂萃取凝胶渗透色谱/固相萃取净化气相色谱质谱法测定咸鱼中有机磷农药残留[J].分析化学,2011,39(1):67-71.
[8]许秀丽,李礼,丁罡斗,等.大米中13种有机磷农药的固相萃取结合大体积进样/气相色谱-质谱法快速分析[J].分析测试学报,2008,27(1):23-26.
[9]钱程,吴琼,吕岱竹,等.超高效液相色谱-串联质谱法测定豇豆中溴氰虫酰胺等5种农药残留[J].农药学学报,2014,16(5):594-599.