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
Metabolism of free fatty acids（FFAs） is related to several important physiological events and therefore their quantitaion in biological samples arouses extensive interest and efforts.Existing gas chromatography with...Metabolism of free fatty acids（FFAs） is related to several important physiological events and therefore their quantitaion in biological samples arouses extensive interest and efforts.Existing gas chromatography with flame ionization detector（GC-FID） methods for the analysis of FFAs normally require derivatization of them in order to lower boiling points.But this extra procedure tends to induce additional error and it is laborious and time-consuming.A derivatization-free method was therefore established in the present investigation to determine FFAs in human plasma by capillary（GC-FID）.After extraction of FFAs from plasma,a highly polar FFAP（free fatty acid in plasma） column was employed to directly quantitate FFAs concentration,free from derivatization reaction.All sample pretreatments were carried out at room temperature,improving recovery of short-chain FFAs.Heptadecanoic acid（C17：0） was employed as internal standard,and the proposed method was validated for recovery,precision,sensitivity,stabi-lity,and linearity.Validation data show that it is suitable for clinical study that has been applied to the evaluation of FFAs levels in plasma of diabetic nephropathy（DN） patients during the course of treatment.Forty-seven patients diagnosed with DN were admitted to the double-blind experiment.Control group（n=17） underwent solely basic treatment and the patients did not show significant change in FFAs concentration during six months of treatment.Experiment group（n=30） was supplied with traditional Chinese medicine besides basic treatment.After six months of medication,their plasma concentration of palmitic acid（C16：0）,stearic acid（C18：0） and oleic acid（C18：1n-9） decreased while linolenic acid（C18：3n-3） increased significantly（P〈0.05）.These four compounds could be served as biomar-kers in the evaluation of drug efficacy,and their quantitation in plasma may provide additional information for disease progression in DN patients.展开更多
该研究采用人工感官评价、顶空气相色谱火焰离子化检测器法(headspace gas chromatography with flame ionization detection,HS-GC-FID)、顶空固相微萃取气相色谱-质谱联用技术(headspace solid phase microextraction gas chromatogra...该研究采用人工感官评价、顶空气相色谱火焰离子化检测器法(headspace gas chromatography with flame ionization detection,HS-GC-FID)、顶空固相微萃取气相色谱-质谱联用技术(headspace solid phase microextraction gas chromatography-mass spectrometry,HS-SPME-GC-MS)及顶空固相微萃取-全二维气相色谱-飞行时间质谱(headspace solid phase microextraction-comprehensive two-dimensional gas chromatograph-time of flight mass spectrometer,HS-SPME-GC×GC-TOFMS)技术对国内6种品牌的Lager啤酒的特征香气成分进行了分析。通过HS-SPME-GC×GC-TOFMS技术对6种啤酒中的香气化合物进行了全面检测及半定量分析,分别测出520、520、519、522、518、513种物质,并首次在Lager啤酒中测出罗勒烯、白铃兰醇、桃醛等化合物。通过HS-GC-FID及HS-SPME-GC-MS技术共定量了61种香气成分,其中酯类24种、醇类14种、醛类10种、酸类6种、酮类3种、酚类2种、含S及含O杂环化合物各1种。结合多元变量统计分析方法,通过一维色谱发现主要差异物质为异戊醇、苯乙醇、乙酸乙酯等,通过HS-SPME-GC×GC-TOFMS的相对定量结果进一步表明,差异物质还体现在2,3-丁二醇硝酸酯等含N化合物及(E)-β-金合欢烯、罗勒烯等其他共计100种化合物上。此外,通过多元统计学、气味活性值结合皮尔森相关性分析发现,啤酒麦芽香高低与菠萝酮的含量高低相关,酒花香与芳樟醇、乙酸芳樟酯的含量相关,花香、酯香与乙酸乙酯、辛酸乙酯、乙酸苯乙酯等的含量相关,醇香与异丁醇的含量相关,异香与柠檬醛、壬醛的含量相关。通过二维结合正交偏最小二乘-判别分析还发现,麦芽香还与2,3-丁二醇硝酸酯,1,2-丙二醇硝酸酯等含N化合物相关。展开更多
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。
基金Supported by the National Basic Research Program of China(Nos.2007CB511903,2005CB523503)the International Cooperation Project of Ministry of Science and Technology of China(No.S2010GR0583)the National Natural Science Founda- tion of China(Nos.90709045,20805026)
文摘Metabolism of free fatty acids（FFAs） is related to several important physiological events and therefore their quantitaion in biological samples arouses extensive interest and efforts.Existing gas chromatography with flame ionization detector（GC-FID） methods for the analysis of FFAs normally require derivatization of them in order to lower boiling points.But this extra procedure tends to induce additional error and it is laborious and time-consuming.A derivatization-free method was therefore established in the present investigation to determine FFAs in human plasma by capillary（GC-FID）.After extraction of FFAs from plasma,a highly polar FFAP（free fatty acid in plasma） column was employed to directly quantitate FFAs concentration,free from derivatization reaction.All sample pretreatments were carried out at room temperature,improving recovery of short-chain FFAs.Heptadecanoic acid（C17：0） was employed as internal standard,and the proposed method was validated for recovery,precision,sensitivity,stabi-lity,and linearity.Validation data show that it is suitable for clinical study that has been applied to the evaluation of FFAs levels in plasma of diabetic nephropathy（DN） patients during the course of treatment.Forty-seven patients diagnosed with DN were admitted to the double-blind experiment.Control group（n=17） underwent solely basic treatment and the patients did not show significant change in FFAs concentration during six months of treatment.Experiment group（n=30） was supplied with traditional Chinese medicine besides basic treatment.After six months of medication,their plasma concentration of palmitic acid（C16：0）,stearic acid（C18：0） and oleic acid（C18：1n-9） decreased while linolenic acid（C18：3n-3） increased significantly（P〈0.05）.These four compounds could be served as biomar-kers in the evaluation of drug efficacy,and their quantitation in plasma may provide additional information for disease progression in DN patients.
文摘该研究采用人工感官评价、顶空气相色谱火焰离子化检测器法(headspace gas chromatography with flame ionization detection,HS-GC-FID)、顶空固相微萃取气相色谱-质谱联用技术(headspace solid phase microextraction gas chromatography-mass spectrometry,HS-SPME-GC-MS)及顶空固相微萃取-全二维气相色谱-飞行时间质谱(headspace solid phase microextraction-comprehensive two-dimensional gas chromatograph-time of flight mass spectrometer,HS-SPME-GC×GC-TOFMS)技术对国内6种品牌的Lager啤酒的特征香气成分进行了分析。通过HS-SPME-GC×GC-TOFMS技术对6种啤酒中的香气化合物进行了全面检测及半定量分析,分别测出520、520、519、522、518、513种物质,并首次在Lager啤酒中测出罗勒烯、白铃兰醇、桃醛等化合物。通过HS-GC-FID及HS-SPME-GC-MS技术共定量了61种香气成分,其中酯类24种、醇类14种、醛类10种、酸类6种、酮类3种、酚类2种、含S及含O杂环化合物各1种。结合多元变量统计分析方法,通过一维色谱发现主要差异物质为异戊醇、苯乙醇、乙酸乙酯等,通过HS-SPME-GC×GC-TOFMS的相对定量结果进一步表明,差异物质还体现在2,3-丁二醇硝酸酯等含N化合物及(E)-β-金合欢烯、罗勒烯等其他共计100种化合物上。此外,通过多元统计学、气味活性值结合皮尔森相关性分析发现,啤酒麦芽香高低与菠萝酮的含量高低相关,酒花香与芳樟醇、乙酸芳樟酯的含量相关,花香、酯香与乙酸乙酯、辛酸乙酯、乙酸苯乙酯等的含量相关,醇香与异丁醇的含量相关,异香与柠檬醛、壬醛的含量相关。通过二维结合正交偏最小二乘-判别分析还发现,麦芽香还与2,3-丁二醇硝酸酯,1,2-丙二醇硝酸酯等含N化合物相关。
