建立了双水相萃取结合气相色谱-三重四极杆串联质谱法(gas chromatography-triple quadrupole tandem mass spectrometry,GC-MS/MS)测定酱香型白酒中挥发性酚类化合物的方法,该方法简单、高效,可快速定量分析酱香型白酒中的7种酚类化合...建立了双水相萃取结合气相色谱-三重四极杆串联质谱法(gas chromatography-triple quadrupole tandem mass spectrometry,GC-MS/MS)测定酱香型白酒中挥发性酚类化合物的方法,该方法简单、高效,可快速定量分析酱香型白酒中的7种酚类化合物。对市售不同品牌系列酱香型白酒及GT提供的一至七轮次酱香型白酒基酒中酚类化合物的含量分布规律进行探索,结果表明,7种酚类化合物的分离效果良好,线性范围为0.0200~10.0000μg/mL,相关系数(R2)均大于0.999,精密度在1.17%~7.64%,回收率为90.74%~120.16%,检出限为0.0011~0.0041μg/mL,定量限为0.0037~0.0137μg/mL。系列酱香型白酒中除JT4、JT5、LT4、LT5未全部检出外,其余样品均检测出7种酚类化合物,酚类化合物的浓度范围是0.0000~0.9268μg/mL。其中4-乙基苯酚(4-Ethylphenol,4-EP)和4-乙基愈创木酚(4-Ethylguaiacol,4-EG)总量的浓度范围是0.0072~0.1275μg/mL,含量最高的是MT3。所选酱香型白酒中4-EP和4-EG总量均小于400μg/L,不会对酒体造成影响。在系列酒中,酚类化合物平均含量GT系列最高(0.6354μg/mL),其次是MT系列(0.5561μg/mL),最低的是LT系列(0.2175μg/mL)。在轮次基酒中,一轮次基酒的酚类化合物总量最高,为0.0373μg/mL,最低的是三轮次,为0.2101μg/mL。同时一轮次中的愈创木酚(Guaiacol,Gua)、4-甲基愈创木酚(4-Methylguaiacol,4-MG)、苯酚(Phenol,Phe)、4-EG、4-乙烯基愈创木酚(4-Vinylguaiacol,4-VG)等物质的含量也显著高于其他轮次基酒,四轮、五轮、六轮次酚类物质的总质量浓度较为接近。展开更多
建立了全自动QuEChERS样品前处理系统结合低压气相色谱-三重四极杆质谱(LPGC-MS/MS)同时检测茶叶中46种农药残留的分析方法。茶叶样品经粉碎均匀后,用全自动QuEChERS样品前处理系统提取、净化,氮吹浓缩后,用TG-5LPGC-MS柱分离,三重四极...建立了全自动QuEChERS样品前处理系统结合低压气相色谱-三重四极杆质谱(LPGC-MS/MS)同时检测茶叶中46种农药残留的分析方法。茶叶样品经粉碎均匀后,用全自动QuEChERS样品前处理系统提取、净化,氮吹浓缩后,用TG-5LPGC-MS柱分离,三重四极杆质谱多反应监测(Multiple Reaction Monitoring,MRM)模式检测目标物,外标法定量。在1倍定量限、2倍定量限和10倍定量限三个添加水平下,选定的空白茶叶样品中的回收率在77.9%~106.3%之间,相对标准偏差(relative standard deviation,RSD)为0.8%~9.4%,方法的检出限(detection of limit,LOD)在0.11~4.3μg·kg^(-1)。该方法自动化程度高,出错率低,耗时短,有效的节省人力资源成本及实验成本,适用于大批量茶叶样品中多种农药残留的快速定性定量。展开更多
基于超高效液相色谱-串联四极杆飞行时间高分辨质谱(ultra-high performance liquid chromatographytriple quadrupole-time of flight tandem mass spectrometry,UPLC-Triple-TOF MS/MS)法对巴氏杀菌乳中的磷脂成分进行分析鉴定。采用...基于超高效液相色谱-串联四极杆飞行时间高分辨质谱(ultra-high performance liquid chromatographytriple quadrupole-time of flight tandem mass spectrometry,UPLC-Triple-TOF MS/MS)法对巴氏杀菌乳中的磷脂成分进行分析鉴定。采用色谱柱ACQUITY UPLC^®BEH C18(2.1 mm×100 mm,1.7μm),以流动相A水-甲醇-乙腈(1∶1∶1,V/V)和流动相B异丙醇-乙腈(1∶1,V/V)进行梯度洗脱,在电喷雾电离正模式下采集数据。依据高分辨质谱提供的保留时间、准分子离子、二级碎片等脂质分析数据,并结合标准品碎裂方式等信息,共鉴定出磷脂分子68种。其中,磷脂酰胆碱22种,占比7.98%;磷脂酰乙醇胺17种,占比56.60%;磷脂酰丝氨酸10种,占比1.70%;磷脂酰肌醇7种,占比1.33%;鞘磷脂12种,占比32.39%。本研究采用灵敏度高、精密度及稳定性良好的UPLC-Triple-TOF MS/MS方法实现了对牛乳中磷脂的全面定性与定量分析。此方法检测出的牛乳磷脂信息完整、磷脂种类多于其他检测技术,可为牛乳的磷脂研究提供数据基础。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
文摘建立了双水相萃取结合气相色谱-三重四极杆串联质谱法(gas chromatography-triple quadrupole tandem mass spectrometry,GC-MS/MS)测定酱香型白酒中挥发性酚类化合物的方法,该方法简单、高效,可快速定量分析酱香型白酒中的7种酚类化合物。对市售不同品牌系列酱香型白酒及GT提供的一至七轮次酱香型白酒基酒中酚类化合物的含量分布规律进行探索,结果表明,7种酚类化合物的分离效果良好,线性范围为0.0200~10.0000μg/mL,相关系数(R2)均大于0.999,精密度在1.17%~7.64%,回收率为90.74%~120.16%,检出限为0.0011~0.0041μg/mL,定量限为0.0037~0.0137μg/mL。系列酱香型白酒中除JT4、JT5、LT4、LT5未全部检出外,其余样品均检测出7种酚类化合物,酚类化合物的浓度范围是0.0000~0.9268μg/mL。其中4-乙基苯酚(4-Ethylphenol,4-EP)和4-乙基愈创木酚(4-Ethylguaiacol,4-EG)总量的浓度范围是0.0072~0.1275μg/mL,含量最高的是MT3。所选酱香型白酒中4-EP和4-EG总量均小于400μg/L,不会对酒体造成影响。在系列酒中,酚类化合物平均含量GT系列最高(0.6354μg/mL),其次是MT系列(0.5561μg/mL),最低的是LT系列(0.2175μg/mL)。在轮次基酒中,一轮次基酒的酚类化合物总量最高,为0.0373μg/mL,最低的是三轮次,为0.2101μg/mL。同时一轮次中的愈创木酚(Guaiacol,Gua)、4-甲基愈创木酚(4-Methylguaiacol,4-MG)、苯酚(Phenol,Phe)、4-EG、4-乙烯基愈创木酚(4-Vinylguaiacol,4-VG)等物质的含量也显著高于其他轮次基酒,四轮、五轮、六轮次酚类物质的总质量浓度较为接近。
文摘建立了全自动QuEChERS样品前处理系统结合低压气相色谱-三重四极杆质谱(LPGC-MS/MS)同时检测茶叶中46种农药残留的分析方法。茶叶样品经粉碎均匀后,用全自动QuEChERS样品前处理系统提取、净化,氮吹浓缩后,用TG-5LPGC-MS柱分离,三重四极杆质谱多反应监测(Multiple Reaction Monitoring,MRM)模式检测目标物,外标法定量。在1倍定量限、2倍定量限和10倍定量限三个添加水平下,选定的空白茶叶样品中的回收率在77.9%~106.3%之间,相对标准偏差(relative standard deviation,RSD)为0.8%~9.4%,方法的检出限(detection of limit,LOD)在0.11~4.3μg·kg^(-1)。该方法自动化程度高,出错率低,耗时短,有效的节省人力资源成本及实验成本,适用于大批量茶叶样品中多种农药残留的快速定性定量。
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.
