本文建立了一种自动顶空-固相微萃取结合气相色谱-串联质谱法(Automatic Headspace-Solid Phase Microextraction Combined with Gas Chromatography-Tandem Mass Spectrometry,Auto-SPME-GC-MS/MS)测定武都花椒中6种有机氯和5种拟除虫...本文建立了一种自动顶空-固相微萃取结合气相色谱-串联质谱法(Automatic Headspace-Solid Phase Microextraction Combined with Gas Chromatography-Tandem Mass Spectrometry,Auto-SPME-GC-MS/MS)测定武都花椒中6种有机氯和5种拟除虫菊酯类农药的方法。采用自动顶空固相微萃取装置,自动在线完成样品加热、吸附、解吸、进样。通过改变不同萃取因素来探究萃取效率,确定最佳萃取纤维头、萃取试剂和萃取溶剂、盐用量、样品加热及振荡时间、样品吸附和解吸时间。结果显示,该方法的线性范围为0.01~1.00 ng·L^(-1),相关系数在0.998 7~0.999 9,呈现出良好的线性关系;方法检出限为0.005 ng·L^(-1);11种目标物的加标回收率在85.7%~104.4%,相对标准偏差在3.2%~9.6%。该方法准确度和精密度良好,可有效用于武都花椒中拟除虫菊酯类和有机氯农药的痕量分析。展开更多
采用顶空固相微萃取结合气质联用(headspace-solid phase microextraction coupled with gas chromatography-mass spectrometry,SPME-GC/MS)技术,对常温贮存下羊奶粉中挥发性成分进行提取与分析。在常温贮存1年的羊奶粉中,共检出41种...采用顶空固相微萃取结合气质联用(headspace-solid phase microextraction coupled with gas chromatography-mass spectrometry,SPME-GC/MS)技术,对常温贮存下羊奶粉中挥发性成分进行提取与分析。在常温贮存1年的羊奶粉中,共检出41种挥发性成分。其中酸类成分最多,共13种,其次是酯类、烃类、醇类和醛酮类,分别为6、4、4和3种。羊奶粉的主体挥发性成分组成是丁酸、己酸、庚酸、辛酸、4-甲基辛酸、癸酸、月桂酸、邻苯二甲酸二甲酯、辛酸乙酯、十五烷、苯甲醛、甘菊环、己内酰胺,己酸、辛酸、4-甲基辛酸和癸酸在贮存6个月之后含量有明显增加趋势。在整个贮存期间,对羊奶粉膻味有较大影响的酸类物质有己酸、辛酸、4-甲基辛酸和癸酸,尤其是4-甲基辛酸,由于其较低阈值,成为最主要的羊膳物质,并且随着贮存时间的增加,酸类、酯类含量逐渐增加。展开更多
Aroma is an important component for characteristic of wine. β-glucosidase is an enzyme for enhancing wine aroma during fermentation and aging. The aim of this study was to evaluate β-glucosidase activities from 17 y...Aroma is an important component for characteristic of wine. β-glucosidase is an enzyme for enhancing wine aroma during fermentation and aging. The aim of this study was to evaluate β-glucosidase activities from 17 yeast strains. It was found that strain 71 B-1122 exhibited highest activity of β-glucosidase. The purified enzyme of this strain was characterized. The purified enzyme was added in Muscat must before wine making process. The must and wine were determined for volatile compounds by headspace-SPME/GC-MS and found that the hexyl acetate, linalool, phenethyl, nerol and geraniol compounds were significantly increased after treated with the enzyme. Sensory evaluation of the combined alcoholic fermentation and flavour enrichment of Muscat juice by adding of purified β-glucosidase enzyme showed well oenological properties especially aroma. Therefore, in producing wine, yeast strain selection and addition of β-glucosidase enzyme should be considered because they were important factors affecting wine aroma.展开更多
目的:鉴定不同产地鱼露的挥发性物质。方法:采用顶空固相微萃取与气相色谱-质谱联用结合,对不同产地鱼露中的挥发性物质进行分析检测,结合相对保留指数、质谱自动解卷积系统对挥发性物质进行定性。结果:5种鱼露样品共有93种挥发性物质,...目的:鉴定不同产地鱼露的挥发性物质。方法:采用顶空固相微萃取与气相色谱-质谱联用结合,对不同产地鱼露中的挥发性物质进行分析检测,结合相对保留指数、质谱自动解卷积系统对挥发性物质进行定性。结果:5种鱼露样品共有93种挥发性物质,其中广东鱼露样品中酯类和芳香类挥发性物质的相对含量高,泰国鱼露样品中酮类挥发性物质的相对含量高,越南鱼露样品中酸类和杂环类挥发性物质的相对含量高,实验室自制鱼露样品中烃类、醛类和醇类挥发性物质相对含量高。五种鱼露不同个批号的样品经验证积分器(Assignment Validator and Integrator,GAVIN)自动峰对齐后,检出各自的独有组分35种,共有组分11种。共有组分被用于主成成分分析,不同产地的鱼露在主成分分析图上得到较好的分离。结论:提供了不同产地鱼露气味物质的特征,提供了一种利用气质联用的挥发物分析进行产品产地溯源的方法和工作流程。展开更多
为了有效地检测和监测葡萄酒中的木塞污染物,更好把控葡萄酒的品质,建立了自动顶空-固相微萃取-气相色谱三重四级杆质谱(Automatic headspace-solid phase microextraction combined with gas chromatography-triple quadrupole mass sp...为了有效地检测和监测葡萄酒中的木塞污染物,更好把控葡萄酒的品质,建立了自动顶空-固相微萃取-气相色谱三重四级杆质谱(Automatic headspace-solid phase microextraction combined with gas chromatography-triple quadrupole mass spectrometry,Auto-HS-SPME-GC-MS/MS)检测葡萄酒中9种卤代苯甲醚和卤代苯酚类木塞污染物的方法。实验中,卤代苯酚类化合物与乙酸酐发生在线衍生化反应得到乙酰化产物,卤代苯甲醚和卤代苯酚乙酰化产物再通过HS-SPME浓缩富集后经GC-MS/MS检测,同位素内标法定量。通过优化自动固相微萃取的实验条件,对葡萄酒和起泡酒的样品进行了测定。结果表明,方法线性范围为3~300 ng/L,相关系数R^(2)为0.9988~0.9999,线性关系良好。方法检出限为1 ng/L,9种目标物加标回收率在63.7%~118.4%之间,具有较好的准确度;相对标准偏差为2.0%~16.4%,说明实验方法及仪器具有良好的精密度。该方法自动化程度高且可靠稳定,适用于葡萄酒中卤代苯甲醚、卤代苯酚类化合物的痕量检测。展开更多
文摘本文建立了一种自动顶空-固相微萃取结合气相色谱-串联质谱法(Automatic Headspace-Solid Phase Microextraction Combined with Gas Chromatography-Tandem Mass Spectrometry,Auto-SPME-GC-MS/MS)测定武都花椒中6种有机氯和5种拟除虫菊酯类农药的方法。采用自动顶空固相微萃取装置,自动在线完成样品加热、吸附、解吸、进样。通过改变不同萃取因素来探究萃取效率,确定最佳萃取纤维头、萃取试剂和萃取溶剂、盐用量、样品加热及振荡时间、样品吸附和解吸时间。结果显示,该方法的线性范围为0.01~1.00 ng·L^(-1),相关系数在0.998 7~0.999 9,呈现出良好的线性关系;方法检出限为0.005 ng·L^(-1);11种目标物的加标回收率在85.7%~104.4%,相对标准偏差在3.2%~9.6%。该方法准确度和精密度良好,可有效用于武都花椒中拟除虫菊酯类和有机氯农药的痕量分析。
文摘采用顶空固相微萃取结合气质联用(headspace-solid phase microextraction coupled with gas chromatography-mass spectrometry,SPME-GC/MS)技术,对常温贮存下羊奶粉中挥发性成分进行提取与分析。在常温贮存1年的羊奶粉中,共检出41种挥发性成分。其中酸类成分最多,共13种,其次是酯类、烃类、醇类和醛酮类,分别为6、4、4和3种。羊奶粉的主体挥发性成分组成是丁酸、己酸、庚酸、辛酸、4-甲基辛酸、癸酸、月桂酸、邻苯二甲酸二甲酯、辛酸乙酯、十五烷、苯甲醛、甘菊环、己内酰胺,己酸、辛酸、4-甲基辛酸和癸酸在贮存6个月之后含量有明显增加趋势。在整个贮存期间,对羊奶粉膻味有较大影响的酸类物质有己酸、辛酸、4-甲基辛酸和癸酸,尤其是4-甲基辛酸,由于其较低阈值,成为最主要的羊膳物质,并且随着贮存时间的增加,酸类、酯类含量逐渐增加。
文摘Aroma is an important component for characteristic of wine. β-glucosidase is an enzyme for enhancing wine aroma during fermentation and aging. The aim of this study was to evaluate β-glucosidase activities from 17 yeast strains. It was found that strain 71 B-1122 exhibited highest activity of β-glucosidase. The purified enzyme of this strain was characterized. The purified enzyme was added in Muscat must before wine making process. The must and wine were determined for volatile compounds by headspace-SPME/GC-MS and found that the hexyl acetate, linalool, phenethyl, nerol and geraniol compounds were significantly increased after treated with the enzyme. Sensory evaluation of the combined alcoholic fermentation and flavour enrichment of Muscat juice by adding of purified β-glucosidase enzyme showed well oenological properties especially aroma. Therefore, in producing wine, yeast strain selection and addition of β-glucosidase enzyme should be considered because they were important factors affecting wine aroma.
文摘目的:鉴定不同产地鱼露的挥发性物质。方法:采用顶空固相微萃取与气相色谱-质谱联用结合,对不同产地鱼露中的挥发性物质进行分析检测,结合相对保留指数、质谱自动解卷积系统对挥发性物质进行定性。结果:5种鱼露样品共有93种挥发性物质,其中广东鱼露样品中酯类和芳香类挥发性物质的相对含量高,泰国鱼露样品中酮类挥发性物质的相对含量高,越南鱼露样品中酸类和杂环类挥发性物质的相对含量高,实验室自制鱼露样品中烃类、醛类和醇类挥发性物质相对含量高。五种鱼露不同个批号的样品经验证积分器(Assignment Validator and Integrator,GAVIN)自动峰对齐后,检出各自的独有组分35种,共有组分11种。共有组分被用于主成成分分析,不同产地的鱼露在主成分分析图上得到较好的分离。结论:提供了不同产地鱼露气味物质的特征,提供了一种利用气质联用的挥发物分析进行产品产地溯源的方法和工作流程。
文摘为了有效地检测和监测葡萄酒中的木塞污染物,更好把控葡萄酒的品质,建立了自动顶空-固相微萃取-气相色谱三重四级杆质谱(Automatic headspace-solid phase microextraction combined with gas chromatography-triple quadrupole mass spectrometry,Auto-HS-SPME-GC-MS/MS)检测葡萄酒中9种卤代苯甲醚和卤代苯酚类木塞污染物的方法。实验中,卤代苯酚类化合物与乙酸酐发生在线衍生化反应得到乙酰化产物,卤代苯甲醚和卤代苯酚乙酰化产物再通过HS-SPME浓缩富集后经GC-MS/MS检测,同位素内标法定量。通过优化自动固相微萃取的实验条件,对葡萄酒和起泡酒的样品进行了测定。结果表明,方法线性范围为3~300 ng/L,相关系数R^(2)为0.9988~0.9999,线性关系良好。方法检出限为1 ng/L,9种目标物加标回收率在63.7%~118.4%之间,具有较好的准确度;相对标准偏差为2.0%~16.4%,说明实验方法及仪器具有良好的精密度。该方法自动化程度高且可靠稳定,适用于葡萄酒中卤代苯甲醚、卤代苯酚类化合物的痕量检测。
