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
A new and simple gas chromatographic (GC) method using flame ionization detector (FID) and mass spectrometry (MS) for the simultaneous determination of eight fatty alcohols in 10 mg policosanol film-coated tablets was...A new and simple gas chromatographic (GC) method using flame ionization detector (FID) and mass spectrometry (MS) for the simultaneous determination of eight fatty alcohols in 10 mg policosanol film-coated tablets was established and applied to the quality control (QC) of policosanol film-coated tablets. A DB-35MS capillary column (30 m × 0.32 mm, 0.25 um) was employed for the separation. GC-FID was used to quantitatively analyze the eight ingredients with 1-eicosanol as internal standard, three of which were identified using GC-MS due to the lack of standard. The linearity, accuracy, precision, stability, robustness and sensitivity within the detection limits were evaluated. The average recovery of the method was 96.3-100.4% and linearity was (R > 0.999). The average drug content was found to be 96.8% of the labeled amount (10 mg).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A new and simple gas chromatographic (GC) method using flame ionization detector (FID) and mass spectrometry (MS) for the simultaneous determination of eight fatty alcohols in 10 mg policosanol film-coated tablets was established and applied to the quality control (QC) of policosanol film-coated tablets. A DB-35MS capillary column (30 m × 0.32 mm, 0.25 um) was employed for the separation. GC-FID was used to quantitatively analyze the eight ingredients with 1-eicosanol as internal standard, three of which were identified using GC-MS due to the lack of standard. The linearity, accuracy, precision, stability, robustness and sensitivity within the detection limits were evaluated. The average recovery of the method was 96.3-100.4% and linearity was (R > 0.999). The average drug content was found to be 96.8% of the labeled amount (10 mg).
