鱼肉样品以Florisil硅藻土层析柱净化后,经气相色谱-电子轰击离子源-质谱法(GC-EI-MS)分析其中8种邻苯二甲酸酯(PAEs)含量:邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丙酯(DPrP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二...鱼肉样品以Florisil硅藻土层析柱净化后,经气相色谱-电子轰击离子源-质谱法(GC-EI-MS)分析其中8种邻苯二甲酸酯(PAEs)含量:邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丙酯(DPrP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二戊酯(DPeP)、邻苯二甲酸二环己基酯(DCHP)、邻苯二甲酸二己酯(DHP)、邻苯二甲酸二(2-乙基己基)酯(DEHP).比较了外标和内标法定量,并确定苯甲酸苄基酯为内标物;优化了提取剂、吸附剂和洗脱剂的种类,以及洗脱体积等样品前处理方法;尤其对分析空白的控制问题进行了详细讨论;准确分析了5种鱼样品中此类物质含量.该方法的线性范围为50.0～800μg·L-1,相关系数(R)大于0.99986,相对标准偏差(Relative standard deviation,RSD)均小于12.7%,检测限(Limit of detection,LOD)低于3.66μg·L-1,样品的加标回收率为74.0%～113%.其线性范围、相关系数、准确度、精密度和LOD等指标均满足鱼肉中多种PAEs同时分析的要求.展开更多
Gas chromatography mass spectrometry (GC-MS) is a widely used central analytical technology. Commercially available GC-MS systems use different types of mass analyzers such as Quadrupole, Ion Trap and/or Time of Fligh...Gas chromatography mass spectrometry (GC-MS) is a widely used central analytical technology. Commercially available GC-MS systems use different types of mass analyzers such as Quadrupole, Ion Trap and/or Time of Flight, but practically all systems utilize the same Nier type electron ionization (EI) ion source and the same standard GC-MS transferline interface. Consequently, the various GC-MS vendors characterize their systems by a short list of specifications that relate to improvements in the technology of GC or of MS and not of the interfacing technology and ion source. This article presents a list of 62 ways in which the performance of GC-MS as a whole can be improved by an innovative interface and ion source. Such an interface can possibly lead to a GC-MS revolution in a way that is similar to that whichis brought to Liquid Chromatography Mass Spectrometry (LC-MS) by the Electrospray ionization interface and ion source and not by improvements to the technology of LC or MS. These 62 possible GC-MS improvements (grouped into eight main categories) are not merely theoretical as they are provided by the Cold-EI GC-MS interface, which is based on the ionization of vibrationally cold sample molecules in a Supersonic Molecular Beam (SMB) within a fly-through ion source. An explanation and discussion is provided for each of these possible improvements.展开更多
Achillea millefolium and Achillea ptarmica are both plants belonging to the Asteracea family and are traditionally used for their medicinal properties. It has already been shown that some N-alkylamides(NAAs)are respon...Achillea millefolium and Achillea ptarmica are both plants belonging to the Asteracea family and are traditionally used for their medicinal properties. It has already been shown that some N-alkylamides(NAAs)are responsible for these pharmacological actions. Therefore, in the present study, the NAA content of the two plants was analytically characterised. Different extracts were prepared from the roots, the leaves, the stems and the flowers. The structures of NAAs have been assigned in ethanolic extracts of Achillea millefolium and Achillea ptarmica using high performance liquid chromatography – electrospray ionisation – mass spectrometry(HPLC–ESI–MS) and gas chromatography – electron impact – mass spectrometry(GC–EI–MS). Using both analytical techniques, the structures of 14 and 15 NAAs have been assigned in Achillea ptarmica and Achillea millefolium, respectively. Structures of two new NAAs, previously never observed in Achillea ptarmica,were assigned: deca-2E,6Z,8E-trienoic acid 2-methylbutylamide(homospilanthol) or a related isomeric compound and deca-2E,4E-dienoic acid N-methyl isobutylamide. The structure of homospilanthol or a related isomeric compound was also assigned in Achillea millefolium for the first time.展开更多
3-Octyl-thiophene is a reactive monomer important derivatives of polythiophen.3-Octyl-thiophene is prepared by coupling 3-bromothiophene with n-octane bromide.The products of the reaction are analyzed by gas chromatog...3-Octyl-thiophene is a reactive monomer important derivatives of polythiophen.3-Octyl-thiophene is prepared by coupling 3-bromothiophene with n-octane bromide.The products of the reaction are analyzed by gas chromatograph-mass spectrometry.The results show that there are four kinds of compounds in the reactive liquid.The main yield is 3-octyl-thiophene,while main by-product is 3,3’-bithiophene.展开更多
文摘鱼肉样品以Florisil硅藻土层析柱净化后,经气相色谱-电子轰击离子源-质谱法(GC-EI-MS)分析其中8种邻苯二甲酸酯(PAEs)含量:邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丙酯(DPrP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二戊酯(DPeP)、邻苯二甲酸二环己基酯(DCHP)、邻苯二甲酸二己酯(DHP)、邻苯二甲酸二(2-乙基己基)酯(DEHP).比较了外标和内标法定量,并确定苯甲酸苄基酯为内标物;优化了提取剂、吸附剂和洗脱剂的种类,以及洗脱体积等样品前处理方法;尤其对分析空白的控制问题进行了详细讨论;准确分析了5种鱼样品中此类物质含量.该方法的线性范围为50.0～800μg·L-1,相关系数(R)大于0.99986,相对标准偏差(Relative standard deviation,RSD)均小于12.7%,检测限(Limit of detection,LOD)低于3.66μg·L-1,样品的加标回收率为74.0%～113%.其线性范围、相关系数、准确度、精密度和LOD等指标均满足鱼肉中多种PAEs同时分析的要求.
文摘Gas chromatography mass spectrometry (GC-MS) is a widely used central analytical technology. Commercially available GC-MS systems use different types of mass analyzers such as Quadrupole, Ion Trap and/or Time of Flight, but practically all systems utilize the same Nier type electron ionization (EI) ion source and the same standard GC-MS transferline interface. Consequently, the various GC-MS vendors characterize their systems by a short list of specifications that relate to improvements in the technology of GC or of MS and not of the interfacing technology and ion source. This article presents a list of 62 ways in which the performance of GC-MS as a whole can be improved by an innovative interface and ion source. Such an interface can possibly lead to a GC-MS revolution in a way that is similar to that whichis brought to Liquid Chromatography Mass Spectrometry (LC-MS) by the Electrospray ionization interface and ion source and not by improvements to the technology of LC or MS. These 62 possible GC-MS improvements (grouped into eight main categories) are not merely theoretical as they are provided by the Cold-EI GC-MS interface, which is based on the ionization of vibrationally cold sample molecules in a Supersonic Molecular Beam (SMB) within a fly-through ion source. An explanation and discussion is provided for each of these possible improvements.
基金the Special Research Fund of Ghent University (BOF 01D23812 to Lien Taevernier)
文摘Achillea millefolium and Achillea ptarmica are both plants belonging to the Asteracea family and are traditionally used for their medicinal properties. It has already been shown that some N-alkylamides(NAAs)are responsible for these pharmacological actions. Therefore, in the present study, the NAA content of the two plants was analytically characterised. Different extracts were prepared from the roots, the leaves, the stems and the flowers. The structures of NAAs have been assigned in ethanolic extracts of Achillea millefolium and Achillea ptarmica using high performance liquid chromatography – electrospray ionisation – mass spectrometry(HPLC–ESI–MS) and gas chromatography – electron impact – mass spectrometry(GC–EI–MS). Using both analytical techniques, the structures of 14 and 15 NAAs have been assigned in Achillea ptarmica and Achillea millefolium, respectively. Structures of two new NAAs, previously never observed in Achillea ptarmica,were assigned: deca-2E,6Z,8E-trienoic acid 2-methylbutylamide(homospilanthol) or a related isomeric compound and deca-2E,4E-dienoic acid N-methyl isobutylamide. The structure of homospilanthol or a related isomeric compound was also assigned in Achillea millefolium for the first time.
文摘3-Octyl-thiophene is a reactive monomer important derivatives of polythiophen.3-Octyl-thiophene is prepared by coupling 3-bromothiophene with n-octane bromide.The products of the reaction are analyzed by gas chromatograph-mass spectrometry.The results show that there are four kinds of compounds in the reactive liquid.The main yield is 3-octyl-thiophene,while main by-product is 3,3’-bithiophene.
