QuEChERS结合HPLC-MS/MS法同时测定连翘中26种农药残留  

Simultaneous determination of 26 pesticide residues in Forsythia suspensa by QuEChERS combined with HPLC-MS/MS

作　　者：赖华杰 刘瑞[1] 易从圣 吴志鹏 唐毅 LAI Huajie;LIU Rui;YI Congsheng;WU Zhipeng;TANG Yi(CAS Testing Technical Services(Guangzhou)Co.Ltd.,Guangzhou 510650,China;Guangzhou Institute of Chemistry,Chinese Academy of Sciences,Guangzhou 510650,China;New Materials Research Institute of CASCHEM(Chongqing)Co.,Ltd.,Chongqing 400700,China)

机构地区：[1]中科检测技术服务(广州)股份有限公司,广州510650 [2]中国科学院广州化学研究所,广州510650 [3]中科广化(重庆)新材料研究院有限公司,重庆400700

出　　处：《农药》2025年第1期47-52,共6页Agrochemicals

摘　　要：[目的]通过QuEChERS前处理方法与高效液相色谱质谱联用法相结合,建立连翘中26种农药残留的分析测试方法。[方法]样品经1%乙酸水溶液浸泡,加入乙腈振荡提取,提取液经300 mg PSA、100 mg C18和50 mg MWCNTs净化后,使用HPLC-MS/MS检测,基质标曲外标法定量。[结果]26种农药在1~1500μg/L的质量浓度范围内,线性关系良好;在3个添加水平下,26种农药在连翘中的平均添加回收率为75.2%~130%,相对标准偏差<10%;检出限LOD为0.2~27μg/kg,定量限LOQ为0.5~89μg/kg。采用所建方法对市售7批连翘样品进行分析检测,结果显示26种农药残留均未检出(<LOD)。[结论]该方法高效、准确、灵敏,适用于连翘中26种农药残留的同时检测。[Aims]This study aims to establish a method for the simultaneous determination of 26 pesticide residues in Forsythia suspensa,by a combination of QuEChERS pretreatment and high performance liquid chromatographytandem mass spectrometry(HPLC-MS/MS).[Methods]The samples were soaked in acetic acid 1%aqueous solution,extracted with acetonitrile by vortexing.The extracts were purified using 300 mg PSA,100 mg C18 and 50 mg MWCNTs,and tested by HPLC-MS/MS with matrix-matched calibration for quantitative analysis.[Results]The results showed good linearity in the concentration range of 1-1500μg/L for 26 pesticides.The average spiked recoveries of the 26 pesticides in F.suspensa were 75.2%-130%at 3 spiking levels,with RSDs less than 10%.The LODs and the LOQs were 0.2-27 and 0.5-89μg/kg,respectively.The method was applied to the analysis of 7 commercial F.suspensa samples,and the results showed that 26 pesticides were not detected(<LOD).[Conclusions]The developed method is efficient,accurate and sensitive,and can be applied to the simultaneous determination of 26 pesticide residues in F.suspensa.

关 键 词：连翘 农药 QUECHERS HPLC-MS/MS 

分 类 号：TQ450.2[化学工程—农药化工]