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
Long-term indoor-air limit for formaldehyde stipulated by the European Commission is 1 μg/m3,while the World Health Organization has set a threshold of 100 μg/m3 that should not be exceeded for more than 30 min. To ...Long-term indoor-air limit for formaldehyde stipulated by the European Commission is 1 μg/m3,while the World Health Organization has set a threshold of 100 μg/m3 that should not be exceeded for more than 30 min. To date,however,only a few analytical techniques have been developed that can be used to detect formaldehyde at these very restrictive limits. Thus,there is a need to develop for comprehensive methods for analyzing airborne formaldehyde and other carbonyl pollutants in the ambient environment. The aim of this study is to develop a highly sensitive online automated preconcentration gas chromatographic method using large-volume injection with a programmed temperature vaporization injector for the analysis of airborne formaldehyde and ten other carbonyl compounds. The influence of several parameters,such as the maximum volume injected,programmed temperature vaporization transfer time and temperature,carrier gas flow rate,and type of packing material was investigated. After optimization,highly satisfactory results in terms of the absolute and methodological detection limits were achieved,i. e. as low as the μg/m3 level for all the carbonyl pollutants studied. A commercially available sampler,originally designed for active sampling,was evaluated as a passive sampling device;this optimized technique was applied to monitor the concentrations of carbonyl pollutants in the indoor air of ten public buildings in Florence. The strength of this methodology lies both in the low detection limits reached in the simultaneous analysis of a wide group of 2,4-dinitrophenylhydrazine derivatives,and the potential adaptability of this method to other gas chromatographic applications to achieve lower sensitivity.展开更多
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。
文摘Long-term indoor-air limit for formaldehyde stipulated by the European Commission is 1 μg/m3,while the World Health Organization has set a threshold of 100 μg/m3 that should not be exceeded for more than 30 min. To date,however,only a few analytical techniques have been developed that can be used to detect formaldehyde at these very restrictive limits. Thus,there is a need to develop for comprehensive methods for analyzing airborne formaldehyde and other carbonyl pollutants in the ambient environment. The aim of this study is to develop a highly sensitive online automated preconcentration gas chromatographic method using large-volume injection with a programmed temperature vaporization injector for the analysis of airborne formaldehyde and ten other carbonyl compounds. The influence of several parameters,such as the maximum volume injected,programmed temperature vaporization transfer time and temperature,carrier gas flow rate,and type of packing material was investigated. After optimization,highly satisfactory results in terms of the absolute and methodological detection limits were achieved,i. e. as low as the μg/m3 level for all the carbonyl pollutants studied. A commercially available sampler,originally designed for active sampling,was evaluated as a passive sampling device;this optimized technique was applied to monitor the concentrations of carbonyl pollutants in the indoor air of ten public buildings in Florence. The strength of this methodology lies both in the low detection limits reached in the simultaneous analysis of a wide group of 2,4-dinitrophenylhydrazine derivatives,and the potential adaptability of this method to other gas chromatographic applications to achieve lower sensitivity.
