超高效液相色谱-串联质谱法测定食用菌中9种常见农药残留
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S481+.8

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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)


Determination of 9 Common Pesticide Residues in Edible Fungi by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry
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    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MgSO4盐析后,用N-丙基乙二胺(PSA)、石墨化碳(GCB)、C18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 C18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。

    Abstract:

    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 containing0.1% acetate and water(1∶1). After salting out by NaCl and anhydrous MgSO4, the extract was purified by N-propyl ethylenediamine(PSA), graphenized carbon(GCB), C18and anhydrous magnesium sulfate. The 0.01% formic acid water-acetonitrile system was used as the mobile phase in gradient elution, the BEH C18chromatographic 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 0.05-0.50 μg/kg, the quantitative limits(S/N=10) were 0.1-1.0 μg/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.

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杨明,陈丽娜,时东方,刘春明,李忠和,高星爱,刘宝林.超高效液相色谱-串联质谱法测定食用菌中9种常见农药残留[J].东北农业科学,2023,48(3):138-144.

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  • 收稿日期:2020-03-10
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  • 在线发布日期: 2024-10-24
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