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
利用气相色谱法(GC),分别采用硫化学发光检测器(SCD)和氢火焰离子化检测器(FID),对纯苯中的痕量噻吩进行了测定。结果表明:2种方法的定量校正曲线的线性相关系数均大于0.999,线性良好;采用不同方法对含噻吩量为1.10μg/g的标准溶液进行...利用气相色谱法(GC),分别采用硫化学发光检测器(SCD)和氢火焰离子化检测器(FID),对纯苯中的痕量噻吩进行了测定。结果表明:2种方法的定量校正曲线的线性相关系数均大于0.999,线性良好;采用不同方法对含噻吩量为1.10μg/g的标准溶液进行了测定,二者相对标准偏差均小于3%,回收率为98.2%~103.5%,表明2种方法的准确度和精密度均较好;另外,GC-FID和GC-SCD对实际样品的检测结果与ASTM D 7435的基本相同,前两者的最低检测限分别0.12,0.04μg/g,满足工业生产对纯苯产品质量监控的要求。展开更多
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.
文摘利用气相色谱法(GC),分别采用硫化学发光检测器(SCD)和氢火焰离子化检测器(FID),对纯苯中的痕量噻吩进行了测定。结果表明:2种方法的定量校正曲线的线性相关系数均大于0.999,线性良好;采用不同方法对含噻吩量为1.10μg/g的标准溶液进行了测定,二者相对标准偏差均小于3%,回收率为98.2%~103.5%,表明2种方法的准确度和精密度均较好;另外,GC-FID和GC-SCD对实际样品的检测结果与ASTM D 7435的基本相同,前两者的最低检测限分别0.12,0.04μg/g,满足工业生产对纯苯产品质量监控的要求。