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Pro ElutTPC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28min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0.9979~0.9999,定量限为0.01~0.03mg/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、Pro ElutTPC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.
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 0.9979~0.9999,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:1.2%~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.
作者
刘超
梅丽宝
尹海飞
李树珍
龙宇宙
LIU Chao;MEI Li-bao;YIN Hai-fei;LI Shu-zhen;LONG Yu-zhou(Baoshan Quality and Technical Supervision Comprehensive Testing Center,Baoshan 678000,China;Flavor Beverage Institute,Chinese Academy of Tropical Agriculture Science,Wanning,Hainan 571533,China)
出处
《食品与机械》
CSCD
北大核心
2023年第1期47-54,共8页
Food and Machinery
基金
国家市场监督管理总局科技计划项目(编号:2019KM068)。
关键词
固相萃取技术
气相色谱-质谱法
咖啡干果皮
农药残留
solid phase extraction technology
gas chromatographymass spectrometry(GC-MS)
coffee peel
pesticide residue
