叶倩, 朱富伟, 王刚, 廖林瀚, 唐雪妹. 牛奶中14种除草剂残留的气相色谱-串联质谱检测方法开发[J]. 农药学学报, 2022, 24(2): 404-410. DOI: 10.16801/j.issn.1008-7303.2021.0170
    引用本文: 叶倩, 朱富伟, 王刚, 廖林瀚, 唐雪妹. 牛奶中14种除草剂残留的气相色谱-串联质谱检测方法开发[J]. 农药学学报, 2022, 24(2): 404-410. DOI: 10.16801/j.issn.1008-7303.2021.0170
    YE Qian, ZHU Fuwei, WANG Gang, LIAO Linhan, TANG Xuemei. Development of gas chromatography-tandem mass spectrometry detection method for 14 herbicides residues in milk[J]. Chinese Journal of Pesticide Science, 2022, 24(2): 404-410. DOI: 10.16801/j.issn.1008-7303.2021.0170
    Citation: YE Qian, ZHU Fuwei, WANG Gang, LIAO Linhan, TANG Xuemei. Development of gas chromatography-tandem mass spectrometry detection method for 14 herbicides residues in milk[J]. Chinese Journal of Pesticide Science, 2022, 24(2): 404-410. DOI: 10.16801/j.issn.1008-7303.2021.0170

    牛奶中14种除草剂残留的气相色谱-串联质谱检测方法开发

    Development of gas chromatography-tandem mass spectrometry detection method for 14 herbicides residues in milk

    • 摘要: 建立了同时快速检测牛奶中14种除草剂残留的气相色谱-串联质谱(GC-MS/MS)分析方法。样品采用乙腈提取,无水硫酸镁和无水乙酸钠净化,过0.22 μm有机相滤膜后,目标物采用气相色谱-串联质谱(EI离子源)、多反应监测模式(MRM)检测。结果表明:在0.005~1 mg/L范围内,14种目标除草剂的质量浓度与其相应峰面积间呈良好的线性关系,决定系数(R2)均大于0.9902。在0.01、0.05和0.5 mg/kg 3个添加水平下,14种除草剂的平均回收率为76%~113%,相对标准偏差(RSD)为1.2%~8.6% (n=6)。14种除草剂在牛奶中的定量限(LOQ)均为0.01 mg/kg。该方法准确、灵敏、操作步骤简单,适用于同时快速测定牛奶中14种除草剂的残留量。

       

      Abstract: A gas chromatography-tandem mass spectrometry(GC-MS/MS) method for the simultaneous and rapid determination of 14 herbicides in milk was established. The samples were extracted with acetonitrile, cleaned-up with MgSO4 and Na2AC, filtered through 0.22 μm organic filter membrane, and the anlytes were determinated with GC-MS/MS (EI source and MRM mode). The results showed that the calibration curve was linear in the range of 0.005-1 mg/L and determination coefficient (R2) was higher than 0.990 2. The average recoveries of 14 herbicides were 76%-113% and the relative standard deviations (RSD) were 1.2%-8.6% (n=6) when the spiked levels were 0.01, 0.05 and 0.5 mg/kg. The limits of quantitation (LOQ) for 14 herbicides were 0.01 mg/kg. The method is accurate, sensitive, simple, and suitable for the simultaneous and rapid determination of 14 herbicides residues in milk.

       

    /

    返回文章
    返回