摘要
建立一种同时测定猴头菇、榛蘑、香菇、榆黄蘑和珊瑚菌5种食用菌中9种常用农药残留的QuEChERS-超高效液相色谱-串联质谱方法。样品经0.1%乙酸乙腈-水(1∶1)振荡提取,NaCl和无水MgSO_(4)盐析后,用N-丙基乙二胺(PSA)、石墨化碳(GCB)、C_(18)和无水硫酸镁净化。以0.01%甲酸水-乙腈系统为流动相,梯度洗脱,BEH C_(18)色谱柱分离,利用UPLCMS/MS进行确证和测定。在各自的线性范围内,9种农药的质量浓度与峰面积呈良好的线性关系,相关系数r>0.99,检出限(S/N=3)为0.05~0.50μg/kg,定量限(S/N=10)为0.1~1.0μg/kg,加标回收率在74.58%~115.95%,相对标准偏差为1.28%~16.42%。该方法操作简单、快速且灵敏度高,适用于检测食用菌中9种常用农药残留。
QuEChERS combined with ultra-high performance liquid chromatography-tandem mass spectrometry was established for the determination of 9 pesticide residues in edible fungi,including hericium,hazel mushroom,shiitake,pleurotus ostreatus and coral fungus.The samples were extracted with a solution of acetonitrile containing 0.1%acetate and water(1∶1).After salting out by NaCl and anhydrous MgSO_(4),the extract was purified by N-propyl ethylenediamine(PSA),graphenized carbon(GCB),C_(18)and anhydrous magnesium sulfate.The 0.01%formic acid water-acetonitrile system was used as the mobile phase in gradient elution,the BEH C_(18)chromatographic column was used as stationary phase for separation,and UPLC-MS/MS was used for confirmation and determination.Good linear relationships of the 9 pesticides between the mass concentrations and peak area have been obtained with r>0.99 in their respective linear ranges.The detection limits(S/N=3)were 0.05-0.50μg/kg,the quantitative limits(S/N=10)were 0.1-1.0μg/kg,the spiked recoveries were 74.58%-115.95%,and the relative standard deviations were 1.28%-16.42%.This method is simple,rapid,highly sensitive,and is suitable for the determination of 9 pesticide residues in edible fungi.
作者
杨明
陈丽娜
时东方
刘春明
李忠和
高星爱
刘宝林
YANG Ming;CHEN Lina;SHI Dongfang;LIU Chunming;LI Zhonghe;GAO Xing′ai;LIU Baolin(Central laboratory of Changchun normal university,Changchun 130032;Jilin Academy of Agricultural Sci⁃ences,Changchun 130033,China)
出处
《东北农业科学》
2023年第3期138-144,共7页
Journal of Northeast Agricultural Sciences
基金
吉林省应用生态工程实验室自主创新能力建设项目(2018C0022)
吉林省教育厅“十三五”科学技术项目(JJKH20170658KJ)
长春师范大学自然科学基金项目(长师大自科合字【2016】第002号)
