[Objectives] To establish Qu ECh ERS based extraction method for determining multiple pesticide residues in okra combined with programmed temperature vaporizer-gas chromatography-triple quadrupole mass spectrometry( P...[Objectives] To establish Qu ECh ERS based extraction method for determining multiple pesticide residues in okra combined with programmed temperature vaporizer-gas chromatography-triple quadrupole mass spectrometry( PTV-GC-MS/MS) and ultra high performance liquid chromatography-mass spectrometry( UPLC-MS/MS). [Methods] In this experiment,124 pesticide residues in okra were determined by an optimized Qu ECh ERS method combined with PTV-GC-MS/MS and UPLC-MS/MS. The pesticides in okra were extracted and purified by the optimized Qu ECh ERS pretreatment method and determined by PTV-GC-MS/MS and UPLC-MS/MS. [Results] In this experiment,124 kinds of pesticides had a good linearity with a limit of detection( LOD) of 0. 000 5-0. 008 0 mg/kg; the average recovery rate at three levels was 65. 5%-128. 1% with relative standard deviation of 2. 2%-9. 7%. [Conclusions] This method is simple,rapid,accurate and sensitive,and can provide reliable and valid data support for the determination of multiple pesticide residues in okra by GC-MS/MS and UPLC-MS/MS.展开更多
建立了程序升温进样-气相色谱-三重四级杆串联质谱仪(PTV-GC-MS/MS)检测水产品中42种农药残留和超高效液相色谱-串联质谱(UPLC-MS/MS)测定水产品中28种兽药残留的分析方法。样品经2%甲酸乙腈提取,Oasis PRi ME HLB固相萃取柱净化后,通...建立了程序升温进样-气相色谱-三重四级杆串联质谱仪(PTV-GC-MS/MS)检测水产品中42种农药残留和超高效液相色谱-串联质谱(UPLC-MS/MS)测定水产品中28种兽药残留的分析方法。样品经2%甲酸乙腈提取,Oasis PRi ME HLB固相萃取柱净化后,通过优化色谱参数和质谱参数,提高灵敏度、降低基质及农药重叠峰干扰,采用多反应监测(MRM)模式,以保留时间和离子对进行定性,峰面积定量。42种农药和28种兽药线性关系良好,相关系数大于0.99,在3个添加水平下的平均回收率为62.4%~111.3%,相对标准偏差为1.1%~11.1%,检出限(LOD)为0.0002~0.0079mg·kg-1,定量限(LOQ)为0.0007~0.0261 mg·kg-1。该法具有操作简单、快速、节省溶剂、准确灵敏等特点,适用于水产品中农兽药多残留的快速筛查。展开更多
基金Supported by Science and Technology Planning Project of Guangdong Province(2014A040401008)
文摘[Objectives] To establish Qu ECh ERS based extraction method for determining multiple pesticide residues in okra combined with programmed temperature vaporizer-gas chromatography-triple quadrupole mass spectrometry( PTV-GC-MS/MS) and ultra high performance liquid chromatography-mass spectrometry( UPLC-MS/MS). [Methods] In this experiment,124 pesticide residues in okra were determined by an optimized Qu ECh ERS method combined with PTV-GC-MS/MS and UPLC-MS/MS. The pesticides in okra were extracted and purified by the optimized Qu ECh ERS pretreatment method and determined by PTV-GC-MS/MS and UPLC-MS/MS. [Results] In this experiment,124 kinds of pesticides had a good linearity with a limit of detection( LOD) of 0. 000 5-0. 008 0 mg/kg; the average recovery rate at three levels was 65. 5%-128. 1% with relative standard deviation of 2. 2%-9. 7%. [Conclusions] This method is simple,rapid,accurate and sensitive,and can provide reliable and valid data support for the determination of multiple pesticide residues in okra by GC-MS/MS and UPLC-MS/MS.
文摘建立了程序升温进样-气相色谱-三重四级杆串联质谱仪(PTV-GC-MS/MS)检测水产品中42种农药残留和超高效液相色谱-串联质谱(UPLC-MS/MS)测定水产品中28种兽药残留的分析方法。样品经2%甲酸乙腈提取,Oasis PRi ME HLB固相萃取柱净化后,通过优化色谱参数和质谱参数,提高灵敏度、降低基质及农药重叠峰干扰,采用多反应监测(MRM)模式,以保留时间和离子对进行定性,峰面积定量。42种农药和28种兽药线性关系良好,相关系数大于0.99,在3个添加水平下的平均回收率为62.4%~111.3%,相对标准偏差为1.1%~11.1%,检出限(LOD)为0.0002~0.0079mg·kg-1,定量限(LOQ)为0.0007~0.0261 mg·kg-1。该法具有操作简单、快速、节省溶剂、准确灵敏等特点,适用于水产品中农兽药多残留的快速筛查。
