大气压气相色谱电离源-串联质谱法测定蔬菜中23种农药残留
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(1.中南大学湘雅公共卫生学院,湖南 长沙 410078;2.北京市疾病预防控制中心,北京 100013)

作者简介:

郁欢欢 女 硕士生 研究方向为食品安全检测 E-mail:yuhuan@csu.edu.cn 王建武 男 副教授 研究方向为食品安全检测 E-mail:jianwu_wang@csu.edu.cn

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国家重点研发计划(2017YFC1601600)


Determination of 23 pesticide residues in vegetable by atmospheric pressure gas chromatography-tandem mass spectrometry
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(1.Xiangya Public Health College, Central South University, Hunan Changsha 410078, China;2.Beijing Center for Disease Control and Prevention, Beijing 100013, China)

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    摘要:

    目的 建立蔬菜中23种农药的大气压气相色谱电离源-串联质谱检测方法。方法 采用丙酮提取蔬菜样品中的目标农药,多壁碳纳米管为净化材料,经DB-5MS色谱柱(30 m×0.25 mm,0.25 μm)分离,结合大气压气相色谱电离源技术,正离子多反应监测(MRM)模式进行检测,外标标准曲线法定量。结果 23种农药在0.01~20 μg/L范围内线性良好,相关系数(R2)均大于0.99,在蔬菜基质中23种农药的方法检出限和定量限分别为0.02~0.40和0.05~1.25 μg/kg,回收率为66.7%~110.7%,相对标准偏差(RSD)≤14.8%。结论 本方法具有良好的灵敏度、重现性和特异性,适用于蔬菜中多种农药残留的快速检测。

    Abstract:

    Objective To develop a method for the determination of 23 pesticides in vegetables by atmospheric pressure gas chromatography-tandem mass spectrometry (APGC-MS/MS). Methods Acetone was used to extract target compounds in vegetable samples, while multi-walled carbon nanotubes was used as purifying material. The extracts were separated by DB-5MS column(30 m×0.25 mm, 0.25 μm). APGC-MS/MS was operated in positive ion multiple reaction monitoring mode (MRM) for pesticides detection. External standard calibration method was used for quantification. Results The 23 pesticides showed good linearity in the range of 0.01-20 μg/L, with correlation coefficient (R2) above 0.99. The detection limits and quantification limits of 23 pesticide residues in vegetable substrates were 0.02-0.40 and 0.05-1.25 μg/kg, respectively. The recoveries were between 66.7%-110.7% with relative standard deviation (RSD)≤14.8%. ConclusionThe method had high sensitivity, reproductivity and specificity and was suitable for rapid detection of multiple pesticide residues in vegetables.

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郁欢欢,杨奕,张晶,徐慧兰,王建武.大气压气相色谱电离源-串联质谱法测定蔬菜中23种农药残留[J].中国食品卫生杂志,2020,32(1):31-38.

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  • 收稿日期:2019-12-20
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  • 在线发布日期: 2020-02-25
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