苗雪雪, 杨愿愿, 刘登彪, 杨晓云, 徐汉虹. 分散液液微萃取-气质联用法测定牛奶中酰胺类除草剂[J]. 华南农业大学学报, 2015, 36(2): 43-48. DOI: 10.7671/j.issn.1001-411X.2015.02.008
    引用本文: 苗雪雪, 杨愿愿, 刘登彪, 杨晓云, 徐汉虹. 分散液液微萃取-气质联用法测定牛奶中酰胺类除草剂[J]. 华南农业大学学报, 2015, 36(2): 43-48. DOI: 10.7671/j.issn.1001-411X.2015.02.008
    MIAO Xuexue, YANG Yuanyuan, LIU Dengbiao, YANG Xiaoyun, XU Hanhong. Determination of the amide herbicides in milk using dispersive liquid-liquid microextraction prior to GC-MS[J]. Journal of South China Agricultural University, 2015, 36(2): 43-48. DOI: 10.7671/j.issn.1001-411X.2015.02.008
    Citation: MIAO Xuexue, YANG Yuanyuan, LIU Dengbiao, YANG Xiaoyun, XU Hanhong. Determination of the amide herbicides in milk using dispersive liquid-liquid microextraction prior to GC-MS[J]. Journal of South China Agricultural University, 2015, 36(2): 43-48. DOI: 10.7671/j.issn.1001-411X.2015.02.008

    分散液液微萃取-气质联用法测定牛奶中酰胺类除草剂

    Determination of the amide herbicides in milk using dispersive liquid-liquid microextraction prior to GC-MS

    • 摘要:
      目的 实现牛奶中农药残留快速、准确的分析检测,更好地监督牛奶的食品安全问题.
      方法 采用分散液液微萃取技术(DLLME)作为前处理方法,气相色谱-质谱联用(GC-MS)作为色谱分析仪器,建立了牛奶中4种酰胺类除草剂(甲草胺、乙草胺、丙草胺和异丙甲草胺)的残留分析方法.
      结果和结论 对影响萃取效率的因素进行了分析和优化,最终选取40 μL四氯化碳作为萃取剂,1 000 μL甲醇作为分散剂,提取时间设置为1.0 min.在最优的试验条件下,4种酰胺类除草剂质量浓度在0.05~5.00 mg·L-1范围内均具有良好的线性相关,相关系数≥0.997 8.该方法灵敏度高,检出限在0.8~1.4 μg·L-1(S/N=3)范围内.该方法应用于实际牛奶样品的检测,4种目标物的平均添加回收率为67.0%~105.7%,相对标准偏差(RSD)为1.6%~8.3%.

       

      Abstract:
      Objective To supervise the food safety problem in milk and achieve a rapid and accurate determination of pesticide residues in milk.
      Method In this paper, a simple, sensitive and environment friendly dispersive liquid-liquid microextraction (DLLME) technique coupled with gas chromatography-mass spectrometry (GC-MS) was established for the extraction and determination of four amide herbicides (alachlor, acetochlor, pretilachlor, and metolachlor) in milk samples.
      Result and conclusion The factors that affected extraction efficiency were studied and optimized. Eventually, 40 μL carbon tetrachloride was used as the extractant, 1 000 μL methanol was chosen as the dispersant and the extraction time was set to 1.0 min. Under the optimum conditions, the good linearity was exhibited from 0.05 to 5.00 mg·L-1 herbicide, with the correlation coefficient being more than 0.997 8. The method had a high sensitivity, and the limits of detection (S/N=3) of the four amide herbicides ranged from 0.8 to 1.4 μg·L-1. The recoveries of the target analytes from milk samples were found between 67.0% and 105.7%, and the relative standard deviations (RSD) varied from 1.6% to 8.3%. The method can be successfully applied for the analysis of amide herbicides in real milk samples.

       

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