超高效液相色谱-串联质谱法测定小麦籽粒中25种磺酰脲类除草剂残留  

Determination of sulfonylurea herbicide residues in wheat kernels by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：刘炜[1] 刘行[2] 杨晓凤[1] 尹全[1] 张义蓉[1] 张富丽[1] 刘茜 LIU Wei;LIU Xing;YANG Xiaofeng;YIN Quan;ZHANG Yirong;ZHANG Fuli;LIU Qian(Analysis and Testing Center of Sichuan Academy of Agricultural Sciences,Chengdu 610066,China;Economic Crops Research Institute Sichuan Academy of Agricultural Sciences,Chengdu 610300,China)

机构地区：[1]四川省农业科学院分析测试中心,四川成都610066 [2]四川省农业科学院经济作物育种栽培研究所,四川成都610300

出　　处：《中国测试》2022年第3期78-83,共6页China Measurement & Test

基　　金：四川省创新能力提升工程公益深化项目资助(2016GYSH-032)。

摘　　要：通过改进QuEChERS前处理方法,建立同时测定小麦籽粒中25种磺酰脲类除草剂残留的超高效液相色谱-串联质谱法(UPLC-MS/MS)。小麦籽粒样品经含1%甲酸的乙腈提取,QuEChERS方法净化,以Waters ACQUITY UPLC CSH C18 Column(100 mm×2.1 mm,1.7μm)进行液相分离,三重四极杆串联质谱以正离子多重反应监测模式(MRM)进行测定,外标法定量。结果表明:在检测浓度范围内,25种除草剂的质量浓度与对应的峰面积间均呈良好的线性关系,相关系数均在0.996 2~0.999 4之间。在1~100μg/kg添加水平下,平均回收率为85.9%~107.2%,相对标准偏差(RSDs)0.9%~6.8%,检出限为0.006~0.21μg/kg,定量限为0.019~0.71μg/kg,基质效应为0.83~1.13。该方法前处理简单,分析时间短,准确度和灵敏度高,适合小麦籽粒样品中25种磺酰脲类除草剂残留实际检测需要。A method for simultaneous determination of 25 sulfonylurea herbicide residues in wheat kernels was developed by improving the pretreatment method of QuEChERS and using Ultra Performance Liquid Chromatography-tandem Mass Spectrometry(UPLC-MS/MS). The samples were extracted with 1% formic acid in acetonitrile, cleaned up by developed QuEChERS method. then separated by waters ACQUITY UPLC CSH C18 Column(100 mm×2.1 mm, 1.7 μm) and detected by by UPLC-MS/MS in multiple reaction monitoring(MRM) mode via positive electrospray ionization(ESI+), and quantified by external standard method. The linear relationships of 25 herbicides were the detection concentration range, the correlation coefficients were 0.996 2 and 0.999 4. The recoveries of the target compounds in two matrices were both 85.9%-107.2%, and the RSDs were both 0.9%-6.8%. The limits of detection(LODs) were 0.006-0.21 μg/kg, the limits of quantitation(LOQs) were 0.019-0.71 μg/kg, the matrix effects were 0.83-1.13. This method is simple, rapid,time-saving, high sensitive and accuracy, and suitable for the actual detection of 25 kinds of sulfonylurea herbicide residues of wheat kernels samples.

关 键 词：超高效液相色谱-串联质谱 小麦籽粒 磺酰脲类除草剂 残留 

分 类 号：O657.63[理学—分析化学] TB9[理学—化学]