气相色谱-质谱法测定蔬菜中65种除草剂的残留量
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杜晓林 女 研究生 研究方向为食品中农药残留(除草剂残留)检测技术研究 E-mail:xiaolindxl@126.com

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国家科技支撑计划课题(2011BAK10B06)


Determination of 65herbicides in vegetables by gas chromatography-mass spectrometry
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    摘要:

    建立蔬菜中65种不同类别除草剂的气相色谱-质谱(GC-MS)检测方法。方法样品用乙腈超声提取后,经Carb/NH2柱净化,采用GC-MS检测,以基质匹配的标准校正曲线外标法定量。结果除卞草唑的线性范围为20~1000μg/L,其他64种除草剂在10~1000μg/L范围内呈良好线性,相关系数均大于0.998;各农药的方法检出限为0.02~2.2μg/kg,定量限为0.1~7.4μg/kg;以空白蔬菜样品(选取油菜为代表性基质)进行加标水平为5、10和20μg/kg的加标回收试验,除扑草灭和乙氧苯草胺的回收率在41.1%~59.4%之间外,各除草剂的回收率均在60.9%~117.9%之间,相对标准偏差(RSD)低于14.0%。对9份蔬菜样品(包括土豆、油菜、白菜、菠菜)进行检测,1份样品(白菜)检出氟乐灵,其含量为2.0μg/kg。结论该检测方法快速、简便、准确,适用于蔬菜样品中除草剂类农药残留的检测。

    Abstract:

    To develop a new method for quantitative determination of 65herbicides belonging to different chemical families in vegetables by gas chromatography-mass spectrometry(GC-MS).MethodsSamples were ultrasonically extracted with acetonitrile and the extracts were cleanuped with Carb/NH2 cartridge before GC-MS analysis.Matrix-matched calibration was used for quantification.ResultsThe linearity was satisfying within the range of 10~1000μg/L,and the coefficients of determination(r)were above 0.998.The limits of detection(LODs)and the limits of quantification(LOQs)were 0.02~2.2μg/kg and 0.1~7.4μg/kg, respectively. The recoveries for spiked samples at the levels of 5,10and 20μg/kg ranged from 60.9% to 117.9%, except for EPTC and Etobenzanid in the range of 41.1%~59.4%.The relative standard deviations(RSD)were below 14.0%. Trifluralin was detected in 1out of 9vegetable samples collected from local market,with the concentration of 2.0μg/kg.Conclusion The proposed method was rapid,simple and sensitive for the analysis of 65herbicides in vegetables.

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杜晓林,荫硕妍,李荷丽,苗虹,吴永宁.气相色谱-质谱法测定蔬菜中65种除草剂的残留量[J].中国食品卫生杂志,2013,25(3):241-244.

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  • 收稿日期:2013-03-14
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  • 在线发布日期: 2013-06-19
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