| 苏建峰,陈劲星,连文浩,马莹,徐佳,沈松,刘建军.橄榄油中农药多残留前处理方法研究及其应用于气相色谱、气质联用测定效果评估[J].中国粮油学报,2019,34(6):120-128 |
| 橄榄油中农药多残留前处理方法研究及其应用于气相色谱、气质联用测定效果评估 |
| Evaluation of Multi-residue determination method for the analysis of pesticide residues in olive oil by gas chromatography and gas chromatography-mass spectrometry |
| 投稿时间：2018-08-27 修订日期：2018-11-07 |
| DOI： |
| 中文关键词: 农药多残留 橄榄油 气相色谱法 气相色谱-质谱法 固相萃取 |
| 英文关键词:multiresidual analysis method olive oil gas chromatography(GC) gas chromatography-mass spectrometry(GC-MS) solid phase extraction(SPE) |
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| 摘要点击次数: 518 |
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| 中文摘要: |
| 建立了串联双柱净化前处理方法用于橄榄油中313种农药多残留的测定。橄榄油样品采用正己烷溶解,正己烷-乙腈-盐水三相分配除去部分杂质,农药组分转移至乙腈中,经串联双柱净化后供气相色谱仪(GC)和气相色谱-质谱仪(GC-MS)分析。气相色谱法采用火焰光度检测器(FPD)和电子捕获检测器(ECD)测试,外标法定量,适用于有机磷、有机氯和拟除虫菊酯等部分农药的测定。气相色谱-质谱法采用选择离子监测方式(SIM),外标法定量,适用于本法中所有313项农药的测定。在优化后的条件下进行分析,气相色谱-质谱法的检出限(S/N≥3)为0.01～0.03 mg/kg,在加标水平为0.01、0.05、0.20 mg/kg时,平均回收率为57.5%～148.4%(百菌清为44.3%),其中回收率在70%～120%之间的占93.9%,相对标准偏差为2.1%～17.8%。方法准确、灵敏、快速,可满足橄榄油中多种农药残留的风险监控需求并可扩展到其他植物油检测。 |
| 英文摘要: |
| A method was developed and applied to determine the residual amounts of 313 pesticides in olive oil by gas chromatography(GC)and gas chromatography-mass spectrometry(GC-MS)．For the method,the residues were extracted from oil with acetonitrile,separated with liquid-liquid partition．The clear supernatant liquid purified by solid phase extraction(Envi-18 and PSA columns)was ready for GC and GC-MS analysis．Determinations were performed by using selected ion monitoring (SIM) mode in GC-MS method for all pesticides,and flame photometric detector (FPD) or electron capture detector (ECD) in GC method for organophosphorous,organochlorine and pyrethroid pesticides．Then external standard method was used in the quantification．The methods were convenient and rapid after investigating the conditions of pretreatment and determination．Under the optimal conditions,the detection limits for the GC-MS method(S/N≥3)of pesticides were 0.01～0.03 mg/kg,Tests for recovery were carried by addition of standards at concentration of 0.01～0.20 mg/kg,the recoveries were 57.5%～148.4%(Chlorothalonil 44.3%),among which the recoveries for 93.9% pesticides were between 70% and 120%,the relative standard deviations were 2.1%～17.8%．The methods are easy,fast,more sensitive and can meet the requirement of the multiresidual analysis in olive oil． |
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