Detection of Tocopherol in Oilseed Rape (Brassica napus L.) Using Gas Chromatography with Flame Ionization Detector

The variation among Chinese genotypes of Brassica napus L. for seed tocopherols content and their analysis using gas chromatography has not been comprehensively reported till to date. In the present study, the tocopherol contents of four Chinese genotypes of Brassica napus L., namely, Gaoyou 605, Zhejiang 619, Zheshuang 758, and Zheshuang 72, were evaluated using three modified sample preparation protocols （P1, P2, and P3） for tocopherol extraction. These methods were distinguished as follows. Protocol one （P1） included the evaporation of solvent after extraction without silylation. Protocol two （P2） followed the direct supernatant collection after overnight extraction without drying and silylation. Protocol three （P3） included trimethylsilylation with N,O-bis（trimethylsilyl） trifluoroacetamide. Genotypic comparison of tocopherol and its isoforms revealed that Gaoyou 605 was dominant over the other genotypes with （140.5＋ 10.5）, （316.2＋ 9.2）, and （559.1＋ 24.3） ~tg g-~ of seed meal ct-, 7-, and total （T-） tocopherol, respectively, and a 0.44＋0.04 ^- to 7-tocopherol ratio. The comparison of the sample preparation protocols, on the other hand, suggests that P3 is the most suitable method for the tocopherol extraction from Brassica oilseeds and for the analysis of tocopherols using gas chromatography flame ionization detector （GC-FID）. Trimethylsilylation is the key step differentiating P3 from P1 and P2. Variations detected in tocopherol contents among the Chinese rapeseed （B. napus） genotypes signify the need to quantify a wide range of rapeseed germplasm for seed tocopherol dynamics in short and crop improvement in long.

Pharmaceutical Applications of Gas Chromatography

Gas chromatography is an analytical tool for the separation of compounds in complex mixtures based on the polarity of compounds. Separation is achieved only for compounds that are volatile or that can be made volatile on derivatization of the compound using derivatizing agents. This is one of the widely accepted tools for the separation of compounds because of its simplicity, sensitivity, and effectiveness. The principle of separation of compounds depends on the partitioning behaviour difference between mobile and stationary phase, the sample is carried by a moving gas stream through a tube packed with a finely divided solid or may be coated with a film of a liquid. Different types of columns having a various composition of stationary phase are been used for the separation of different classes of compounds mixture or sample in a suitable solvent is introduced through the injector maintained at higher temperature which is capable of volatilizing the compound into the column.

Determination of Di-n-Butyl Phosphate in Organic Streams of FBTR Mixed Carbide Fuel Reprocessing Solution by Gas Chromatographic Technique

The present work describes the amount of Di-n- butyl phosphate (DBP) produced when PUREX solvent (30%tri-n-butyl phosphate (TBP) mixed with 70% hydrocarbon diluent) is exposed to intensive radiolytic and chemical at- tack during the separation of uranium and plutonium from fission products of FBTR mixed carbide fuel reprocessing solution. DBP is the major degradation product of Tri-n-butyl phosphate (TBP). Amount of DBP formed in the lean organic streams of different fuel burn-up FBTR carbide fuel reprocessing solutions were analyzed by Gas Chromatographic technique. The method is based on the preparation of diazo methane and conversion of non-volatile Di-n-butyl phosphate in to volatile and stable derivatives by the action of diazomethane and then determined by Gas Chromatography (GC). A calibration graph was made for DBP over a concentration in the range from 200 to 1800 ppm with correlation coefficient of 0.99587 and RSD 1.2%. The degraded 30% TBP-NPH solvent loaded with heavy metal ions like uranium was analyzed after repeated use and results are compared with standard ion chromatographic technique. A column comparison study to select of proper gas chromatographic column for the separation of DBP from other components in a single aliquot of injection is also examined.

基于GC-FID、HS-SPME-GC-MS与电子鼻技术评价不同水果发酵酒的香气特征

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。

Development of a Derivatization-free GC-FID Method for Evaluation of Free Fatty Acid Levels in Plasma of Diabetic Nephropathy Patients

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.