[Objectives]To establish a gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)method based on multiple reaction monitoring(MRM)mode for the analysis of the major components in Cang-ai volatile oil(CAVO).[...[Objectives]To establish a gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)method based on multiple reaction monitoring(MRM)mode for the analysis of the major components in Cang-ai volatile oil(CAVO).[Methods]An ultrasensitive gas chromatography-tandem mass spectrometry(GC-MS/MS)method was developed and validated for the determination of three highly abundant components in rat plasma samples.Paeonol was used as an internal standard.A multiple reaction monitoring(MRM)model was employed for the quantification of the three major components of CAVO.[Results]The method demonstrated linearity over the range of 0.25 to 50μg/mL with a correlation coefficient(R 2)greater than 0.9998.The lower limit of quantification was 0.25μg/mL.Intra-day and inter-day accuracy and precision were within 15%.Extraction recovery and matrix effect values ranged from 90.1%to 110.6%and 0.1%to 2.1%,respectively.[Conclusions]This method was successfully applied to the simultaneous determination of the three components in high-level CAVO plasma samples,providing a basis for subsequent studies of CAVO.展开更多
油料作物由于含油量高、基质复杂,导致其弱极性多环芳烃类化合物提取率低,成为准确检测高油样品中多环芳烃的瓶颈。本文对比了16种多环芳烃的GC-MS/MS检测条件SIM(Single Ion Monitoring)模式和SRM(Selective Reaction Monitoring)模式...油料作物由于含油量高、基质复杂,导致其弱极性多环芳烃类化合物提取率低,成为准确检测高油样品中多环芳烃的瓶颈。本文对比了16种多环芳烃的GC-MS/MS检测条件SIM(Single Ion Monitoring)模式和SRM(Selective Reaction Monitoring)模式质谱信号响应,SRM模式干扰峰更少,检出限更低;对比了QuEChERS和超声辅助提取方法对大豆、油菜籽、花生三种油料中16种多环芳烃的提取效果,超声辅助提取的基质效应很高,部分多环芳烃基质减弱80%以上,且油菜籽的提取稳定性差,部分相对标准偏差达到32%~45%。并比较了乙腈和丙酮作为QuCEhERS方法提取溶剂的提取效果。结果表明,QuCEhERS方法中乙腈作为提取溶剂,在极性最弱的多环芳烃回收率低,如苯并[b]荧蒽、苯并[k]荧蒽等,回收率甚至小于10%。而丙酮作为QuCEhERS方法提取溶剂,而在极性弱的多环芳烃中,回收率提高了3~5倍,适合提取高油样品中多环芳烃。三种油料基质匹配标准曲线的相关系数均在0.99以上。16种多环芳烃均能获得较好的回收率(58%~100%),相对标准偏差为0.4%~10.6%,方法稳定性好。展开更多
基金the National Natural Science Foundation of China(NSFC)(82060823)Yunnan Science and Technology Talent and Platform Program(202105AG070012).
文摘[Objectives]To establish a gas chromatography-triple quadrupole mass spectrometry(GC-MS/MS)method based on multiple reaction monitoring(MRM)mode for the analysis of the major components in Cang-ai volatile oil(CAVO).[Methods]An ultrasensitive gas chromatography-tandem mass spectrometry(GC-MS/MS)method was developed and validated for the determination of three highly abundant components in rat plasma samples.Paeonol was used as an internal standard.A multiple reaction monitoring(MRM)model was employed for the quantification of the three major components of CAVO.[Results]The method demonstrated linearity over the range of 0.25 to 50μg/mL with a correlation coefficient(R 2)greater than 0.9998.The lower limit of quantification was 0.25μg/mL.Intra-day and inter-day accuracy and precision were within 15%.Extraction recovery and matrix effect values ranged from 90.1%to 110.6%and 0.1%to 2.1%,respectively.[Conclusions]This method was successfully applied to the simultaneous determination of the three components in high-level CAVO plasma samples,providing a basis for subsequent studies of CAVO.
文摘油料作物由于含油量高、基质复杂,导致其弱极性多环芳烃类化合物提取率低,成为准确检测高油样品中多环芳烃的瓶颈。本文对比了16种多环芳烃的GC-MS/MS检测条件SIM(Single Ion Monitoring)模式和SRM(Selective Reaction Monitoring)模式质谱信号响应,SRM模式干扰峰更少,检出限更低;对比了QuEChERS和超声辅助提取方法对大豆、油菜籽、花生三种油料中16种多环芳烃的提取效果,超声辅助提取的基质效应很高,部分多环芳烃基质减弱80%以上,且油菜籽的提取稳定性差,部分相对标准偏差达到32%~45%。并比较了乙腈和丙酮作为QuCEhERS方法提取溶剂的提取效果。结果表明,QuCEhERS方法中乙腈作为提取溶剂,在极性最弱的多环芳烃回收率低,如苯并[b]荧蒽、苯并[k]荧蒽等,回收率甚至小于10%。而丙酮作为QuCEhERS方法提取溶剂,而在极性弱的多环芳烃中,回收率提高了3~5倍,适合提取高油样品中多环芳烃。三种油料基质匹配标准曲线的相关系数均在0.99以上。16种多环芳烃均能获得较好的回收率(58%~100%),相对标准偏差为0.4%~10.6%,方法稳定性好。
