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.

Solution of false alarm and slow response in flame detector

A new flame detector with one ultraviolet and two infrared detectors is designed. The ultraviolet detector is of rapid response(≤10 μs) while the two infrared detectors usually have a response time of more than 5 ms. The ultraviolet detector is applied to deal with the flame of large scales. When facing the flame of mid or small scales, the three detectors cooperate. Employing the high-order derivatives of the sample data of the infrared circuits to improve the sensitivity, the response speed is greatly improved. The data of the temperature sensor is used to adjust circuit parameters in real time, thus reducing the effect of temperature drift. The flame detectors are tested at different distances and the response time is as rapid as 0.65 ms. The test results show that the new flame detector has the characteristics of high speed and a low rate of false alarms.

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.

Gas Chromatogragh Analysis of Beaver Oil

Eight fatty acids from beaver oil were identified by GC-9A, and their contents were determinded. A simple yet effective method for separation and quantification was described. Contents of the fatty acids were related to their conditions of extraction.

A system consisted of flame ionization detector and sulfur chemiluminescence detector for interference free determination of total sulfur in natural gas

A new detection system consisted of a flame ionization detector（FID） and a sulfur chemiluminescence detector（SCD） was developed for sensitive and interference free determination of total sulfur in natural gas by non-separation gas chromatography. In this system, sulfur containing compounds and hydrocarbons were firstly burned in the FID using oxygen rich flame and converted to SO_2, CO_2 and H_2O, respectively. The products from FID were transported into the SCD with hydrogen rich atmosphere wherein only SO_2 could be reduced to SO and reacted with O_3 to produce characteristic chemiluminescence. Therefore, the chemiluminescence of CO found in conventional SCD were eliminated because CO_2 could not be reduced to CO under these conditions. The experimental parameters were systematically investigated. Limit of detection obtained by the proposed system is better than 0.5 mmol/mol for total sulfur and superior to those previously reported. The proposed method not only retains the advantages of the conventional SCD but also provides several unique advantages including no hydrocarbon interference, better stability, and easier calculation. The utility of this technique was demonstrated by the determination of total sulfur in real samples and two certified reference materials（GBW 06332 and GBW（E） 061320）.

A new analytical method for quantifying of sterane and hopane biomarkers

An analytical method for quantifying biomarker compounds of the sterane and the hopane existing in saturated hydrocarbons has been established by using comprehensive two-dimensional gas chromatography-flame ionization detector(GC×GC-FID) with optimized operating parameters. The new method achieves the quantification by using a GC×GC-FID system which is able to completely separate steranes from hopanes. The data obtained by the new method are of good repeatability and reliability. Compared with the original data, the relative standard deviations(RSDs) of 12 reference compounds are less than 5%. The RSDs of the quantitative results of the biomarkers based on seven separate analyses are also less than 5%. Compared with the traditional method of gas chromatography-mass spectrometry(GC-MS), the new method has a number of advantages, such as common internal standards(ISs), high resolution, no co-eluting peak, and no interference caused by diagnostic ion peaks. The new method provides petroleum geologists with an effective and scientific means in future researches.

Thin layer chromatography performed in stages to identify the presence of aromatic like fraction in chosen bitumen modifiers

The organic modifiers are used to alter the rheology of the binder in the asphalt concrete at an added cost. For quality control purpose, recognizing if such material is present in the final blend is of an interest. The thin layer chromatography(TLC) using a flame photometric detector(FPD), in addition to the typical flame ionization detector, was demonstrated hereby as a potential analytical tool for this problem, differentiating between tall crude oil based anti-aging agent, polymer, oxidized bitumen and gilsonite. Gilsonite and anti-aging agent consists of the material soluble in solvent used in the development of the fraction referred to as aromatics. Due to the hindered mobility of modifier molecules on the stationary phase, the elution of aromatic fraction stops at position convoluted with polars I and polars II fraction regions, colloquially referred to as resins and asphaltenes. However,for the color of this fraction within gilsonite is different. The presence of gilsonite is thus identifiable visually after the second development bath, but also to an extent with FPD from the final chromatogram. The thin layer chromatography-flame ionization detectors(TLC-FID) procedure is suggested to be supplemented by infrared spectroscopy to discriminate between non-bituminous and bituminous modifiers of similar response during fractionation.