固相萃取—气相色谱/质谱法同时测定咖啡干果皮中24种农药残留
CSTR:
作者:
作者单位:

(1. 保山市质量技术监督综合检测中心,云南 保山 678000;2. 中国热带农业科学院香料饮料研究所,海南 万宁 571533)

作者简介:

刘超,男,保山市质量技术监督综合检测中心工程师,硕士。

通讯作者:

梅丽宝(1970—),女,保山市质量技术监督综合检测中心高级工程师,硕士。E-mail: 1259066294@qq.com

中图分类号:

基金项目:

国家市场监督管理总局科技计划项目(编号:2019KM068)


Simultaneous determination of 24 kinds of pesticide residues in coffee peel by solid phase extraction-gas chromatography-mass spectrometry
Author:
Affiliation:

(1. Baoshan Quality and Technical Supervision Comprehensive Testing Center, Baoshan 678000, China; 2. Flavor Beverage Institute, Chinese Academy of Tropical Agriculture Science, Wanning, Hainan 571533, China)

Fund Project:

  • 摘要
  • |
  • 图/表
  • |
  • 访问统计
  • |
  • 参考文献
  • |
  • 相似文献
  • |
  • 引证文献
  • |
  • 资源附件
  • |
  • 文章评论
    摘要:

    目的:建立一种同时分析咖啡干果皮中24种农药残留的固相萃取—气相色谱/质谱方法。方法:样品用水润湿,加入乙腈提取,过ProElut TPC固相萃取柱净化,乙腈—甲苯(V乙腈∶V甲苯=3∶1)洗脱,氮吹浓缩,并采用峰面积内标法定量。结果:在28 min内24种农药得到很好的分离,农药残留量为0.016~0.400 mg/kg,方法的线性良好,相关系数为0.997 9~0.999 9,定量限为0.01~0.03 mg/kg。当农药加标水平为0.03,0.30 mg/kg时,加标回收率分别为65.2%~108.5%和81.4%~105.7%,日内精密度相对标准偏差分别为3.7%~6.8%和2.5%~5.9%,日间精密度相对标准偏差为4.2%~7.2%和2.8%~6.4%。当采用乙腈—甲苯(V乙腈∶V甲苯=3∶1)作洗脱溶剂、ProElut TPC固相萃取小柱作净化柱时,洗脱和净化效率最高,效率值为95%。结论:该方法各性能参数均满足国家标准要求,测定结果准确、可靠,能运用于咖啡干果皮中多组分农药残留的定性和定量分析。

    Abstract:

    Objective: A solid phase extraction-gas chromatography/mass spectrometry (GC-MS) method was developed for the simultaneous determination of 24 pesticide residues in coffee peel. Methods: The sample was wetted with water, extracted with acetonitrile, the extract solution is concentrated and then purified with ProElut TPC solid phase extraction column, eluted with acetonitrile and toluene=3∶1, after concentration, the sample was determinated by GC-MS and the peak area was measured by internal standard method. Results: The 24 pesticides were separated well within 28 minutes. The residue of pesticide was in the range of 0.016~0.400 mg/kg, the linearity of the method was good, the correlation coefficient r was between 0.997 9~0.999 9, the quantitative limit was between 0.01~0.03 mg/kg, when the concentration of pesticide is 0.03 mg/kg and 0.30 mg/kg, the recovery rate is between 65.2%~108.5% and 81.4%~105.7%, The relative standard deviation of intra day precision is between 3.7%~6.8% and 2.5%~5.9%, and the relative standard deviation of daytime precision is between 4.2%~7.2% and 2.8%~6.4%, compared with acetonitrile∶toluene=3∶1, as eluting solvent and ProElut TPC as purification column, the elution and purification efficiency were the highest, and the recovery was 95%. Conclusion: The performance parameters of the method meet the requirements of national standards, and the determination results are accurate and reliable. It can be applied to the qualitative and quantitative analysis of multi-component pesticide residues in dried coffee peel.

    参考文献
    相似文献
    引证文献
引用本文

刘 超,梅丽宝,尹海飞,等.固相萃取—气相色谱/质谱法同时测定咖啡干果皮中24种农药残留[J].食品与机械,2023,39(1):47-54.
LIU Chao, MEI Li-bao, YIN Hai-fei, et al. Simultaneous determination of 24 kinds of pesticide residues in coffee peel by solid phase extraction-gas chromatography-mass spectrometry[J]. Food & Machinery,2023,39(1):47-54.

复制
相关视频

分享
文章指标
  • 点击次数:
  • 下载次数:
  • HTML阅读次数:
  • 引用次数:
历史
  • 收稿日期:2022-05-07
  • 最后修改日期:
  • 录用日期:
  • 在线发布日期: 2023-04-25
  • 出版日期:
文章二维码