豆粉中31种杀菌剂残留的UPLC-MS/MS测定法  

Determination of 31 fungicides residues in soybean powder by UPLC-MS/MS

作　　者：张波 郭二菱 黄笑晨 郭爱静[2] 王可[2] ZHANG Bo;GUO Erling;HUANG Xiaochen;GUO Ajing;WANG Ke(Food Inspection Laboratory,Chengde Food and Drug Inspection and Testing Center,Chengde Hebei,067000,China;Shijiazhuang Center for Disease Control and Prevention,Shijiazhuang Technology Innovation Center for Chemical Poison Detection and Risk Early Warning,Shijiazhuang Hebei,050011,China)

机构地区：[1]承德市食品药品检验检测中心食品检验室 [2]石家庄市疾病预防控制中心,石家庄市化学毒物检测及风险预警技术创新中心

出　　处：《职业与健康》2024年第12期1590-1595,共6页Occupation and Health

基　　金：河北省医学适用技术跟踪项目(GZ2022081)。

摘　　要：目的建立QuEChERS(quick、easy、cheap、effective、rugged、safe)结合超高效液相色谱-串联质谱(ultra performance liquid chromatography tandem mass spectrometry,UPLC-MS/MS)测定豆粉中31种苯并咪唑类和三唑类杀菌剂残留的方法。方法乙腈提取豆粉样品,用十八烷基键合硅胶(C_(18))填料和无水硫酸镁净化上清液后氮吹干。待测样品经Kinetex^(@)F5100A(3.0×100 mm,2.6μm)柱子进行分离,以0.1%甲酸水溶液(A相)和甲醇(B相)作为流动相,电喷雾正离子源(electrospray ionization,ESI+)模式电离,多反应监测(multiple reaction monitoring,MRM)模式进行检测,基质匹配法定量分析。结果31种杀菌剂浓度为0.1~100μg/L,呈良好的线性关系(r>0.999),各杀菌剂检出限为0.01~1.03μg/kg,定量限为0.01~3.44μg/kg,在3个不同浓度下的加标平均回收率为71.3%~118.7%,相对标准偏差为0.4%~9.9%。结论该方法操作简便,适用于大豆样品中31种苯并咪唑类和三唑类杀菌剂的高通量快速检测。Objective To establish a QuEChERS(quick,easy,cheap,effective,rugged,safe)method combined with ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)for detecting residues of 31 benzimidazole and triazole fungicides in soybean powder.Methods The soybean powder samples were extracted using acetonitrile,the supernatant was purified using octadecyl bonded silica gel(C_(18))and anhydrous magnesium sulfate,and then blow dry with nitrogen.The samples were separated using Kinetex@F5100A(3.0×100 mm,2.6μm)with mobile phases consisting of 0.1%formic acid aqueous solution(phase A)and methanol(phase B).The electrospray ionization(ESI+)mode was used for ionization,while detection was conducted using multiple reaction monitoring(MRM).The quantitative detection was performed utilizing the matrix matching method.Results Totally 31 fungicides exhibit a good linear relationship(r>0.999)within the mass concentration range of 0.1-100μg/L.The limits of detection of the fungicides were 0.01-1.03μg/kg,the limits of quantitation were 0.01-3.44μg/kg.The average recovery rate of spiked samples at three different concentrations was 71.3%-118.7%,and the relative standard deviations were 0.4%-9.9%.Conclusion The method is uncomplicated and suitable for rapidly detecting 31 triazole and benzimidazole fungicides in soybean powder samples.

关 键 词：超高效液相色谱-串联质谱 苯并咪唑类杀菌剂 三唑类杀菌剂 豆粉 QuEChERS 

分 类 号：R155.5[医药卫生—营养与食品卫生学]