食品研究与开发:2025,46(13):165-176
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QuEChERS-液相色谱串联高分辨质谱法检测果蔬中34 种农药残留
(1.沈阳市食品药品检验所,辽宁沈阳110124;2.辽宁省检验检测认证中心,辽宁沈阳110036)
Determination of 34 Pesticide Residues in Fruits and Vegetables by QuEChERS-Liquid Chromatography-High Resolution Mass Spectrometry
(1.Shenyang Institute of Food and Drug Control,Shenyang 110124,Liaoning,China;2.Liaoning Inspection,Examination and Certification Centre,Shenyang 110036,Liaoning,China)
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投稿时间:2024-04-25    
中文摘要: 采用QuEChERS(quick,easy,cheap,effective,rugged and safe)-液相色谱串联高分辨质谱法建立蔬菜水果样品中34 种农药残留的检测方法,并建立数据库。样品提取条件为4 g 无水硫酸镁、1.5 g 无水乙酸钠、1 g 氯化钠和10 mL 乙腈(1%乙酸),净化剂条件为10 mg 石墨化碳黑、500 mg 乙二胺-N-丙基硅烷化硅胶、600 mg MgSO4 和200 mg C18,在乙腈-水流动相条件下,选择C18 色谱柱进行目标物分离,采用一级全扫描-触发二级全扫描模式进行检测,检测结果通过保留时间、一级精确分子质量和二级碎片进行定性,通过一级精确分子质量对样品进行定量,以韭菜、菠菜、茄子、葡萄、桃和香蕉为代表样品,采用基质匹配标准曲线法进行定量。结果表明,各农药在相应线性范围内呈现良好的线性关系,R2 均大于0.99,检出限为1~5 μg/kg,定量限为2~10 μg/kg,回收率为70.06%~119.79%,精密度为0.23%~13.77%。该方法具有简便快速、准确度高、灵敏度好的特点,适用于蔬菜水果中34 种农药的检测。
Abstract:In this article,QuEChERS(quick,easy,cheap,effective,rugged and safe)-liquid chromatographyhigh resolution mass spectrometry(LC-HRMS)was employed to establish a rapid detection method for 34 pesticides in fruits and vegetables,and to build a database.The sample extraction condition was 4 g of anhydrous magnesium sulfate,1.5 g of anhydrous sodium acetate,1 g of sodium chloride,and 10 mL of acetonitrile(1%acetic acid). The purification agent condition was 10 mg of graphitized carbon black,500 mg of ethylenediamine-N-propyl silanized silica gel,600 mg of MgSO4,and 200 mg of C18.Under the acetonitrile-water mobile phase condition,the C18 chromatography column was selected for target separation.The samples were detected in Full MS/dd-MS2 mode,with results quantified by retention time,first-order exact molecular weight and second-order fragments,and qualified by first-order exact molecular weight. In the quantification,the matrixmatched standard curve was used,with chives,spinach,eggplants,grapes,peaches,and bananas as representative samples. It was shown in the result that each pesticide showed a good linear relationship within the corresponding linear range,with R2 greater than 0.99,a detection limit of 1-5 μg/kg,a quantification limit of 2-10 μg/kg,a recovery rate range of 70.06%-119.79% and a precision of 0.23%-13.77%. This method is simple,fast,super accurate,and highly sensitive,suitable for detecting 34 pesticides in vegetables and fruits.
文章编号:202513021     中图分类号:    文献标志码:
基金项目:辽宁省市场监督管理局科技计划项目(2023JS009)
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