Essential oil, with more than thirty kinds of compounds separated and identified by gas chromatography-mass spectrometry, was extracted from Shatian shaddock peel and Sweet shaddock peel by squeeze-steam distillation ...Essential oil, with more than thirty kinds of compounds separated and identified by gas chromatography-mass spectrometry, was extracted from Shatian shaddock peel and Sweet shaddock peel by squeeze-steam distillation and direct steam distillation method. Among their composition, the main components are terpene compounds, which account for 93.926% (mass fraction, the same below) and 85.843% of essential oils extracted from Shatian shaddock peel and Sweet shaddock peel, respectively. Although nootkatone is the major contributor of shaddock characteristic scent, and its contents are 1.069% and 1.749% of essential oils from Sweet shaddock peel and Shatian shaddock peel, respectively. The results show that squeeze-steam distillation gives higher yield and good quality of essential oil and the compositions of essential oils from two kinds of shaddock peels are different, but the main contributors of the shaddock scent are the same.展开更多
采用气相色谱-氢火焰离子化检测器法(gas chromatography with hydrogen flame ionization detection,GCFID)、顶空固相微萃取-气相色谱-质谱(headspace solid-phase microextraction coupled with gas chromatography-mass spectrometr...采用气相色谱-氢火焰离子化检测器法(gas chromatography with hydrogen flame ionization detection,GCFID)、顶空固相微萃取-气相色谱-质谱(headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry,HS-SPME-GC-MS)和电子鼻技术分析6种果酒中的挥发性成分,评价果酒风味轮廓特征的差异性。结果表明,GC-FID定量测定樱桃李酒,其中异戊醇、活性戊醇、β-苯乙醇含量最高,乙酸乙酯含量最低;木瓜酒中正丙醇、2,3-丁二醇、癸酸乙酯、乙酸含量最高; 3-羟基-2-丁酮含量在樱桃李酒中最高,山楂酒、甜橙酒中最少。HP-SPME-GC-MS鉴定果酒中挥发性物质94种,其中醇类23种,酯类43种,醛酮类10种,酸类8种,酚类2种,苯环类5种,烷烃类3种。山楂酒、菠萝酒、木瓜酒、甜橙酒、无花果酒和樱桃李酒中香气物质数量分别为34、44、45、45、33、47种。其中山楂酒、木瓜酒和无花果酒中未检出酚类、烷烃类物质。电子鼻对不同果酒香气的区分效果无重叠,W5S传感器区分果酒香气能力最强。比较而言,菠萝酒和樱桃李酒的口感更圆润,香气更愉悦,感官得分最高。展开更多
A method for determination of fatty acids(FA) compositions in human serum by gas chromatography time-of flight mass spectrometry(GC-TOF MS) method was established.The FA in serum were directly transformed into the fat...A method for determination of fatty acids(FA) compositions in human serum by gas chromatography time-of flight mass spectrometry(GC-TOF MS) method was established.The FA in serum were directly transformed into the fatty acid methyl esters by 2.5% H2SO4-methanol.Heptadecanoic acid methyl esters were used as internal standard.The detection and separation of all the FA were performed within 33 min.The established method has the characteristic of simple operation,rapid analysis,high accuracy,large amount of information and safety.So it is suitable for the scientific research to the disease correlating FA.展开更多
Active volatile components in drug pair(DP)Herba Ephedrae-Ramulus Cinnamomi(HE-RC),single drug HE and RC were analyzed by gas chromatography/mass spectrometry(GC/MS),chemometric resolution method(CRM)and overall volum...Active volatile components in drug pair(DP)Herba Ephedrae-Ramulus Cinnamomi(HE-RC),single drug HE and RC were analyzed by gas chromatography/mass spectrometry(GC/MS),chemometric resolution method(CRM)and overall volume integration.By means of CRM,the two-dimensional data obtained from GC-MS instruments were resolved into a pure chromatogram and a mass spectrum of each chemical compound.In total,97,62,and 78 volatile chemical components in volatile oil of HE,RC,and DP HE-RC,were respectively determined qualitatively and quantitatively,accounting for 90.08%,91.62%,and 89.76% total contents of volatile oil of HE,RC,and DP HE-RC respectively.It is further demonstrated that the numbers of volatile components of DP HE-RC are almost the sum of those of two single drugs,but some relative contents of them are changed.Some new components,such as 1,6-dimethylhepta-1,3,5-triene,tetracyclo[4.2.1.1(2,5).0(9,10)]deca-3,7-diene,globulol and(E,E)-6,10,14-trimethyl-5,9,13-pentadecatrien-2-one are found in DP HE-RC because of chemical reactions and physical changes during decoction.展开更多
Poly brominated biphenyl(PBBs) and poly brominated diphenyl ether(PBDEs) in polymers of electrotechnical products have been extracted with toluene and analyzed by gas chromatography-mass spectrometry (GC-MS).The resul...Poly brominated biphenyl(PBBs) and poly brominated diphenyl ether(PBDEs) in polymers of electrotechnical products have been extracted with toluene and analyzed by gas chromatography-mass spectrometry (GC-MS).The result has more credibility when the nature of the sample was determined by retention time and the proportion of characteristic ions.PBBs and PBDEs were quantified by internal standard method and 2′,3,3′,4,4′,5,5′,6,6′-decachlorobiphenyl was used as internal standard.The GC-MS experimental results show,that the average spiked recoveries ranged from 81% to 110%,that the relative standard deviations(RSD) ranged from 1.54% to 8.65%.The research results also showed that the method presented simplicity-operating,excellent linearity and reproducibility.展开更多
采用顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)和液液萃取(liquid-liquid extraction,LLE)结合全二维气相色谱飞行时间质谱(comprehensive two-dimensional gas chromatography time of flight mass spectrometry...采用顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)和液液萃取(liquid-liquid extraction,LLE)结合全二维气相色谱飞行时间质谱(comprehensive two-dimensional gas chromatography time of flight mass spectrometry,GC×GC-TOF-MS)以及香气活度值(odour active value,OAV),对红星二锅头白酒的挥发性成分进行全面解析。研究发现,HS-SPME、LLE分别定性出928、802种挥发性化合物,共计定性出1304种挥发性化合物,共同定性出426种挥发性化合物。基于HS-SPME数据,通过香气数据库筛选出具有香气特征的382种香气化合物,其中酯类相对百分含量占比最高,其次是醇类、酸类和醛类。计算得到了49种香气化合物OAV>1,其中酯类(辛酸乙酯、异戊酸乙酯等)和萜烯类(β-大马酮)对白酒风味的贡献最大,醛类(异戊醛、己醛等)和含硫类(二甲基三硫)其次,醇类(1-辛烯-3-醇)和含氮类(2,3,5-三甲基吡嗪)也有一定风味贡献。该研究丰富了红星二锅头白酒的风味研究,也为下一步生产研究及调控提供了理论和数据支撑。展开更多
建立了一种可用于水产品及食用油中氟乐灵残留量分析的分散型固相萃取-气相色谱-负化学离子源质谱方法。水产品及食用油经乙腈提取，4℃冷藏后，采用分散型固相萃取法净化，由气相色谱-负化学离子源质谱选择离子监测技术进行测定与确证...建立了一种可用于水产品及食用油中氟乐灵残留量分析的分散型固相萃取-气相色谱-负化学离子源质谱方法。水产品及食用油经乙腈提取，4℃冷藏后，采用分散型固相萃取法净化，由气相色谱-负化学离子源质谱选择离子监测技术进行测定与确证，同位素内标法定量。在1～40μg / L 范围内氟乐灵农药的线性关系良好；方法定量限（LOQ）为0.02μg / kg；对鳗鱼、烤鳗、梭子蟹、小龙虾、猪油和橄榄油等6种复杂基质进行1.0、2.0和3.0μg / kg 等3个水平的添加回收试验，平均回收率均处于80％～100％之间，RSD≤10.3％；无干扰现象出现。该方法可作为水产品及食用油中氟乐灵残留检测的确证方法。展开更多
As a major component of lignin and abundantly existing in softwood and hardwood, ferulic acid has been used as a lignin-related compound for lignin biodegradation study. Biodegradation of ferulic acid by Cupriavidus s...As a major component of lignin and abundantly existing in softwood and hardwood, ferulic acid has been used as a lignin-related compound for lignin biodegradation study. Biodegradation of ferulic acid by Cupriavidus sp. B-8, a newly isolated strain, was studied. This strain is able to utilize a wide range of lignin-related aromatic compounds as the sole carbon and energy source, including guaiacol, veratric acid, vanillic acid, cinnamic acid, p-coumaric acid, ferulic acid, and sinapic acid. In addition, the effects of different concentrations of ferulic acid on growth of Cupriavidus sp. B-8 were studied. The growth of Cupriavidus sp. B-8 is better under the condition of lower concentration. High-performance liquid chromatography （HPLC） analysis reveals that above 95% of ferulic acid is degraded within 12 h by Cupriavidus sp. B-8. Based on identification of biodegradation intermediates and further metabolites, the biodegradation pathway of ferulic acid by Cupriavidus sp. B-8 was proposed. Ferulic acid is initially converted to 4-vinylguaiacol, and further oxidized to vanillic acid and protocatechuic acid.展开更多
Labeled polychlorinated dibenzo-p-dioxins and dibenzofurans(PCDD/Fs)were extracted by three different methods,i.e.,soxhlet extraction,hot extraction and accelerated solvent extraction(ASE).The PCDD/Fs were detected by...Labeled polychlorinated dibenzo-p-dioxins and dibenzofurans(PCDD/Fs)were extracted by three different methods,i.e.,soxhlet extraction,hot extraction and accelerated solvent extraction(ASE).The PCDD/Fs were detected by high resolution gas chromatography-high resolution mass spectrometry.Comparisons of the three methods were carried out by recovery of PCDD/Fs,solvent consumption and extraction time.The results showed that all of the method could extract labeled PCDD/Fs efficiently.ASE was a time saving procedure with lowest consumption of solvents compared with the other two methods.展开更多
Ionic liquids ( ILs) based ultrasonic-assisted extract has been applied for the extraction of essential oil from Persicaria minor leaves. The effects of temperature,sonication time,and particle size of the plant mater...Ionic liquids ( ILs) based ultrasonic-assisted extract has been applied for the extraction of essential oil from Persicaria minor leaves. The effects of temperature,sonication time,and particle size of the plant material on the yield of essential oil were investigated. Among the different ILs employed,1-ethyl-3-methyli midazolium acetate was the most effective,providing a 9. 55% yield of the essential oil under optimum conditions( 70 ℃,25 min,IL ∶hexane ratio of 7 ∶10 ( v /v) ,particle size 60-80 mesh) . The performance of 1-ethyl-3-methylimidazolium acetate in the extraction was attributed to its lowviscosity and ability to disintegrate the structural matrix of the plant material. The ability of 1-ethyl-3-methylimidazolium acetate was also confirmed using the conductor like-screening model for realistic solvents. This research proves that ILs can be used to extract essential oils from lignocellulosic biomass.展开更多
文摘Essential oil, with more than thirty kinds of compounds separated and identified by gas chromatography-mass spectrometry, was extracted from Shatian shaddock peel and Sweet shaddock peel by squeeze-steam distillation and direct steam distillation method. Among their composition, the main components are terpene compounds, which account for 93.926% (mass fraction, the same below) and 85.843% of essential oils extracted from Shatian shaddock peel and Sweet shaddock peel, respectively. Although nootkatone is the major contributor of shaddock characteristic scent, and its contents are 1.069% and 1.749% of essential oils from Sweet shaddock peel and Shatian shaddock peel, respectively. The results show that squeeze-steam distillation gives higher yield and good quality of essential oil and the compositions of essential oils from two kinds of shaddock peels are different, but the main contributors of the shaddock scent are the same.
文摘采用气相色谱-氢火焰离子化检测器法(gas chromatography with hydrogen flame ionization detection,GCFID)、顶空固相微萃取-气相色谱-质谱(headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry,HS-SPME-GC-MS)和电子鼻技术分析6种果酒中的挥发性成分,评价果酒风味轮廓特征的差异性。结果表明,GC-FID定量测定樱桃李酒,其中异戊醇、活性戊醇、β-苯乙醇含量最高,乙酸乙酯含量最低;木瓜酒中正丙醇、2,3-丁二醇、癸酸乙酯、乙酸含量最高; 3-羟基-2-丁酮含量在樱桃李酒中最高,山楂酒、甜橙酒中最少。HP-SPME-GC-MS鉴定果酒中挥发性物质94种,其中醇类23种,酯类43种,醛酮类10种,酸类8种,酚类2种,苯环类5种,烷烃类3种。山楂酒、菠萝酒、木瓜酒、甜橙酒、无花果酒和樱桃李酒中香气物质数量分别为34、44、45、45、33、47种。其中山楂酒、木瓜酒和无花果酒中未检出酚类、烷烃类物质。电子鼻对不同果酒香气的区分效果无重叠,W5S传感器区分果酒香气能力最强。比较而言,菠萝酒和樱桃李酒的口感更圆润,香气更愉悦,感官得分最高。
文摘A method for determination of fatty acids(FA) compositions in human serum by gas chromatography time-of flight mass spectrometry(GC-TOF MS) method was established.The FA in serum were directly transformed into the fatty acid methyl esters by 2.5% H2SO4-methanol.Heptadecanoic acid methyl esters were used as internal standard.The detection and separation of all the FA were performed within 33 min.The established method has the characteristic of simple operation,rapid analysis,high accuracy,large amount of information and safety.So it is suitable for the scientific research to the disease correlating FA.
基金Project (01962502) supported by the Natural Science Foundation of Hunan Province, China
文摘Active volatile components in drug pair(DP)Herba Ephedrae-Ramulus Cinnamomi(HE-RC),single drug HE and RC were analyzed by gas chromatography/mass spectrometry(GC/MS),chemometric resolution method(CRM)and overall volume integration.By means of CRM,the two-dimensional data obtained from GC-MS instruments were resolved into a pure chromatogram and a mass spectrum of each chemical compound.In total,97,62,and 78 volatile chemical components in volatile oil of HE,RC,and DP HE-RC,were respectively determined qualitatively and quantitatively,accounting for 90.08%,91.62%,and 89.76% total contents of volatile oil of HE,RC,and DP HE-RC respectively.It is further demonstrated that the numbers of volatile components of DP HE-RC are almost the sum of those of two single drugs,but some relative contents of them are changed.Some new components,such as 1,6-dimethylhepta-1,3,5-triene,tetracyclo[4.2.1.1(2,5).0(9,10)]deca-3,7-diene,globulol and(E,E)-6,10,14-trimethyl-5,9,13-pentadecatrien-2-one are found in DP HE-RC because of chemical reactions and physical changes during decoction.
文摘Poly brominated biphenyl(PBBs) and poly brominated diphenyl ether(PBDEs) in polymers of electrotechnical products have been extracted with toluene and analyzed by gas chromatography-mass spectrometry (GC-MS).The result has more credibility when the nature of the sample was determined by retention time and the proportion of characteristic ions.PBBs and PBDEs were quantified by internal standard method and 2′,3,3′,4,4′,5,5′,6,6′-decachlorobiphenyl was used as internal standard.The GC-MS experimental results show,that the average spiked recoveries ranged from 81% to 110%,that the relative standard deviations(RSD) ranged from 1.54% to 8.65%.The research results also showed that the method presented simplicity-operating,excellent linearity and reproducibility.
文摘采用顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)和液液萃取(liquid-liquid extraction,LLE)结合全二维气相色谱飞行时间质谱(comprehensive two-dimensional gas chromatography time of flight mass spectrometry,GC×GC-TOF-MS)以及香气活度值(odour active value,OAV),对红星二锅头白酒的挥发性成分进行全面解析。研究发现,HS-SPME、LLE分别定性出928、802种挥发性化合物,共计定性出1304种挥发性化合物,共同定性出426种挥发性化合物。基于HS-SPME数据,通过香气数据库筛选出具有香气特征的382种香气化合物,其中酯类相对百分含量占比最高,其次是醇类、酸类和醛类。计算得到了49种香气化合物OAV>1,其中酯类(辛酸乙酯、异戊酸乙酯等)和萜烯类(β-大马酮)对白酒风味的贡献最大,醛类(异戊醛、己醛等)和含硫类(二甲基三硫)其次,醇类(1-辛烯-3-醇)和含氮类(2,3,5-三甲基吡嗪)也有一定风味贡献。该研究丰富了红星二锅头白酒的风味研究,也为下一步生产研究及调控提供了理论和数据支撑。
文摘建立了一种可用于水产品及食用油中氟乐灵残留量分析的分散型固相萃取-气相色谱-负化学离子源质谱方法。水产品及食用油经乙腈提取，4℃冷藏后，采用分散型固相萃取法净化，由气相色谱-负化学离子源质谱选择离子监测技术进行测定与确证，同位素内标法定量。在1～40μg / L 范围内氟乐灵农药的线性关系良好；方法定量限（LOQ）为0.02μg / kg；对鳗鱼、烤鳗、梭子蟹、小龙虾、猪油和橄榄油等6种复杂基质进行1.0、2.0和3.0μg / kg 等3个水平的添加回收试验，平均回收率均处于80％～100％之间，RSD≤10.3％；无干扰现象出现。该方法可作为水产品及食用油中氟乐灵残留检测的确证方法。
基金Foundation item： Project（50925417） supported by the National Science Fund for Distinguished Young Scholars of China Project（50830301） supported by the National Natural Science Foundation of China Project（2011467062） supported by National Research Fund for Public Benefit （Environmental Protection） Industries, China
文摘As a major component of lignin and abundantly existing in softwood and hardwood, ferulic acid has been used as a lignin-related compound for lignin biodegradation study. Biodegradation of ferulic acid by Cupriavidus sp. B-8, a newly isolated strain, was studied. This strain is able to utilize a wide range of lignin-related aromatic compounds as the sole carbon and energy source, including guaiacol, veratric acid, vanillic acid, cinnamic acid, p-coumaric acid, ferulic acid, and sinapic acid. In addition, the effects of different concentrations of ferulic acid on growth of Cupriavidus sp. B-8 were studied. The growth of Cupriavidus sp. B-8 is better under the condition of lower concentration. High-performance liquid chromatography （HPLC） analysis reveals that above 95% of ferulic acid is degraded within 12 h by Cupriavidus sp. B-8. Based on identification of biodegradation intermediates and further metabolites, the biodegradation pathway of ferulic acid by Cupriavidus sp. B-8 was proposed. Ferulic acid is initially converted to 4-vinylguaiacol, and further oxidized to vanillic acid and protocatechuic acid.
文摘Labeled polychlorinated dibenzo-p-dioxins and dibenzofurans(PCDD/Fs)were extracted by three different methods,i.e.,soxhlet extraction,hot extraction and accelerated solvent extraction(ASE).The PCDD/Fs were detected by high resolution gas chromatography-high resolution mass spectrometry.Comparisons of the three methods were carried out by recovery of PCDD/Fs,solvent consumption and extraction time.The results showed that all of the method could extract labeled PCDD/Fs efficiently.ASE was a time saving procedure with lowest consumption of solvents compared with the other two methods.
文摘Ionic liquids ( ILs) based ultrasonic-assisted extract has been applied for the extraction of essential oil from Persicaria minor leaves. The effects of temperature,sonication time,and particle size of the plant material on the yield of essential oil were investigated. Among the different ILs employed,1-ethyl-3-methyli midazolium acetate was the most effective,providing a 9. 55% yield of the essential oil under optimum conditions( 70 ℃,25 min,IL ∶hexane ratio of 7 ∶10 ( v /v) ,particle size 60-80 mesh) . The performance of 1-ethyl-3-methylimidazolium acetate in the extraction was attributed to its lowviscosity and ability to disintegrate the structural matrix of the plant material. The ability of 1-ethyl-3-methylimidazolium acetate was also confirmed using the conductor like-screening model for realistic solvents. This research proves that ILs can be used to extract essential oils from lignocellulosic biomass.
