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QuEChERS结合HPLC-MC法同时测定黄秋葵中72种农药残留 被引量:4

Determinatian of 72 pesticide residues in Okra by high performance liquid chromatography-tandem mass spectrometry with QuEChERS
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摘要 建立了黄秋葵中72种农药的多残留的液相色谱-串联质谱分析方法。前处理采用改良QuEChERS方法,经乙腈提取,引入缓冲盐体系,使用喷射流离子聚焦-电子喷雾离子源(AJS ESI)和动态多重反应监测(DMRM)模式测定,基质匹配标准曲线定量。结果表明:72种农药在10~200μg·L^(-1)(50~400μg·L^(-1))范围内具有较好的线性关系,相关系数均大于0.997。3个添加水平(10(50)、100、200μg·L^(-1))下,72种农药的加标回收率为78.2%~118.5%。检出限为0.0026~4.9238μg·kg-1,定量限为0.0256~49.2384μg·kg-1,相对标准偏差范围为1.2%~9.8%。该方法样品前处理简单、分析时间短、灵敏、可靠、适用于黄秋葵中多种农药残留的检测。 A simple and rapid method was developed for the determinatian of 72 pesticide residues in Okra by high performance liq-uid chromatography-tandem mass spectrometry. The sample was prepared by the modified QuEChERS (Quick、Easy、Cheap、Effective、 Rugged、 Safe) method,extracted with acetonitrile. Electrosprary ion source ( AJS ESI),dynamic multiple reaction monitoring mode (Dynamic MRM)and matrix-matched external standard method were applied to sample analysis. The calibration curves of 72 pesticide residues were linear in the range of 10-2 0 0μg·L-1 ( 50-4 0 0μg·L-1) w ith correlation coefficients more than 0. 997. The recoveries for all compounds in Okra at the fortified levels of 10(50 )μg·L-1, 100μg ·L-1 and 200μg·L-1 were 78. 2% -118. 5%.The limits of detection ( LOD) were in the range of 0. 0026 -4. 9 238μg ·kg-1,with limits of quantitation (LOQ) of 0.0256-49.2384pg· kg-1,and the RSDs were from 1.2% -9. 8%. The method was simple, rapid and reliable,and could meet the requirement for simultaneous determinatian of 72 pesticide residues in Okra.
出处 《化学研究与应用》 CSCD 北大核心 2017年第7期1094-1104,共11页 Chemical Research and Application
基金 广东省省级科技计划项目(2014A040401008)资助
关键词 QUECHERS 高效液相色谱-串联质谱 DMRM 农药残留 黄秋葵 QuEChERS high performance l iquid chromatography-tandem mass spectrometry dynamic MRM pesticide residues Okra
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