Reque法结合高效液相色谱-高分辨质谱法测定粮谷中克瘟散残留量  

Determination of edifenphos residue in grain by Reque method combined with high performance liquid chromatography-high resolution mass spectrometery

作　　者：刘洋 胡婷婷 赵巍巍 高越 李爱军 姜佳颖 LIU Yang;HU Ting-Ting;ZHAO Wei-Wei;GAO Yue;LI Ai-Jun;JIANG Jia-Ying(Technology Center of Changchun Customs,Changchun 130062,China)

机构地区：[1]长春海关技术中心,长春130062

出　　处：《食品安全质量检测学报》2024年第23期167-173,共7页Journal of Food Safety and Quality

基　　金：长春海关科研项目(2017JK013)。

摘　　要：目的建立Reque法结合高效液相色谱-高分辨质谱法测定粮谷中克瘟散残留量。方法本研究优化了粮谷中克瘟散残留量测定前处理方法,分析液相色谱-高分辨质谱仪的仪器条件、检出限、线性范围、回收率等关键参数。样品通过90%乙腈溶液提取,由Reque净化柱净化,经配备Phenomenex Kinetex F5色谱柱的液相色谱分离,通过高分辨质谱扫描进行定性、定量分析。结果粮谷中克瘟散在1~100 ng/mL范围内具有良好的线性关系(r>0.999)。5种粮谷的检出限均为10 ng/g,方法准确度和精密度通过加标回收实验进行验证,在10、20、100 ng/mL的加标水平下,回收率范围为90.6%~109.8%,相对标准偏差为2.10%~5.20%。结论本方法能够快速、灵敏、准确地测定粮谷中克瘟散的残留量,适用于多种粮谷中克瘟散残留量的检测。Objective To establish a method for the determination of residue of edifenphos in grain by Reque method combined with high performance liquid chromatography-high resolution mass spectrometry.Methods In this study,the pre-treatment method for the determination of residue of edifenphos in grain was optimized,and the key parameters such as instrument condition,limit of detection,linear range and recovery rate of liquid chromatography-high resolution mass spectrometer were analyzed.Samples were extracted with 90%acetonitrile solution,purified by Reque purification column,separated by liquid chromatography with Phenomenex Kinetex F5 column,and analyzed qualitatively and quantitatively by high resolution mass spectrometry.Results The edifenphos in grain had a good linear relationship(r>0.999)in the range of 1–100 ng/mL.The limits of detection of 5 kinds of grains were all 10 ng/g.The accuracies and precisions of the method were verified by standard recovery experiments.Under the standard addition levels of 10,20 and 100 ng/mL,the recovery ranged from 90.6%to 109.8%,and the relative standard deviation ranged from 2.10%to 5.20%.Conclusion The method can quickly,sensitively and accurately determine the residue of edifenphos in grain,and is suitable for the detection of edifenphos residue in many kinds of grain.

关 键 词：克瘟散 Reque 高效液相色谱-高分辨质谱法 粮谷 

分 类 号：O657.63[理学—分析化学] TS210.7[理学—化学]