QuEChERS-超高效液相色谱-四级杆飞行时间质谱法检测青菜中214种农药残留
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(1.江苏省疾病预防控制中心,江苏 南京 210009;2.SCIEX中国,上海 200335)

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朱峰 男 副主任技师 研究方向为食品和水质理化检验 E-mail:zf850824@163.com 吉文亮 男 主任技师 研究方向为食品和水质理化检验 E-mail:641827872@qq.com

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江苏省预防医学科研课题(Y2018081);江苏省医学重点学科(实验室)(ZDXKA2016008)


Determination of 214 pesticide residues in green vegetables using QuEChERS-ultra high performance liquid chromatography coupled with quadrupole time of flight mass spectrometry
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(1.Jiangsu Provincial Center for Disease Control and Prevention, Jiangsu Nanjing 210009, China;2.SCIEX China, Shanghai 200335, China)

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    摘要:

    目的 基于QuEChERS方法,建立了利用超高效液相色谱-四级杆飞行时间质谱检测青菜中214种农药残留的方法。方法 青菜样品经乙腈提取后,用N-丙基乙二胺(PSA)、C18、硫酸钠和石墨化碳黑(GCB)混合净化剂净化,以5 mmol/L甲酸铵溶液(0.1%甲酸)和乙腈作为流动相梯度洗脱,目标物质经Waters ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.7 μm)分离,采用高分辨质谱信息依赖扫描模式(information dependent acquisition, IDA)在正离子模式下进行测定。结果 214种农药在4~1 000 ng/L范围内线性关系良好,相关系数(r2)均大于0.99,各目标物质在空白青菜样品中3个浓度添加水平下的回收率为41.9%~128.5%,相对标准偏差(RSD)为0.4%~14.3%(n=6),方法检出限和定量限分别为0.004~5.443和0.206~18.125 μg/kg。实际样品中共检测出8种农药残留。结论 该方法具有准确、快速、简单、高灵敏度、高通量等优点,适用于日常青菜样品中农药残留的快速筛查与检测。

    Abstract:

    Objective A method for the determination of 214 pesticide residues in green vegetables by QuEChERS using ultra high performance liquid chromatography coupled with quadrupole time of flight mass spectrometry was established. Methods After extracted by acetonitrile, the green vegetables were cleaned-up by a mixed sorbent with primary secondary amine (PSA), C18, Na2SO4 and graphitized carbon black (GCB). The target compounds were separated by Waters ACQUITY UPLC BEH C18 column (2.1 mm×100 mm, 1.7 μm) using 5 mmol/L ammonium formate solution (0.1% formic acid) and acetonitrile as mobile phase by gradient elution, and analyzed in positive electrospray ionization mode by time of flight mass spectrometry (TOF-MS) scan-information dependent acquisition (IDA)-product ion scan. Results All the 214 pesticides showed good linear relationships in the range of 4-1 000 ng/L, and the correlation coefficients(r2)were higher than 0.99. The recoveries at three different spiked levels for all target compounds in blank matrices were 41.9%-128.5%, and the relative standard deviations (RSD) were 0.4%-14.3%(n=6). The limits of detection and quantitation of the method were 0.004-5.443 and 0.206-18.125 μg/kg, respectively. Eight pesticide residues were detected in the real samples. Conclusion The method was suitable for rapid screening and analysis of pesticide residues in green vegetables with the advantages of accuracy, rapidity, simplicity, high sensitivity and high throughput.

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朱峰,于洁,霍宗利,刘华良,张昊,刘德晔,吉文亮. QuEChERS-超高效液相色谱-四级杆飞行时间质谱法检测青菜中214种农药残留[J].中国食品卫生杂志,2020,32(1):25-31.

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  • 收稿日期:2019-12-02
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  • 在线发布日期: 2020-02-25
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