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.

Determination of the volatile fraction of coal tar

The coal tar was qualitative and quantitative anMyzed by gas chromatography （GC） method. 74 components were identified exactly by gas chromatographY-mass spectrometry （GC-MS）. 31 components （37%） were quantitatively analyzed by gas chromatography-flame ionization detector （GC-FID）. The linearity, accuracy, precision, limit of detection （LOD） and limit of quantitative （LOQ） determination were inspected. The scope of quantitative analysis by CC was discussed. The experimental results of thermogravimetric analysis （TGA） proved that GC quantitative analysis of the coal tar was reliable.

Comparison and Analysis of Fabric Deodorization Test Methods

The test methods of deodorization fabric are studied in daily life. In view of different deodorization fabrics and source gases,the detector tube method and gas chromatography-flame ionization detector ( GC-FID ) method were chosen to test the deodorizing rates of fabric and the influencing factors on deodorization test were discussed. Through the two methods,the residual concentration of odorous substance after adsorption can be measured,and the deodorizing rates of deodorization fabric can be got by calculation. The results show that the two test methods are both appropriate for deodorization test of fabric.

Qualitative and Quantitative Assessment of Petroleum Contaminants in Soils under Tropical Weather Conditions

GC-FID methods for the analysis of Petroleum hydrocarbons were developed and optimised. Contamination of soil from the Niger Delta was investigated about 40 days after crude oil spillage from the Shell Petroleum marginal well head. Soil samples and controls were collected at depths of 0 - 15 cm, 15 - 30 cm and 30 - 60 cm. Samples were analysed using gas chromatography fitted with a flame ionisation detector. Penetration and migration of C10-C26 and C26-C34 hydrocarbons through the soil layers were assessed by cluster analysis to determine the spatial distribution, penetration and similarity of these compounds over the contaminated area. The results also indicated elevated levels of total hydrocarbon contents when compared with the reference sites. Recommendations are made to carefully monitor and remediate the environment.

Evaluation of offline sampling for atmospheric C3-C11 non-methane hydrocarbons

The concentration variation of C3-C11 non-methane hydrocarbons(NMHCs)collected in several types of commercial flexible bags and adsorption tubes was systematically inves-tigated using a gas chromatography-flame ionization detector(GC-FID)system.The per-centage loss of each NMHC in the polyvinyl fluoride(PVF)bags was less than 5%during a 7-hr storage period;significant NMHCs loss was detected in aluminum foil composite film and fluorinated ethylene propylene bags.The thermal desorption efficiency of NMHCs for adsorption tubes filled Carbopack B and Carboxen1000 sorbents was greater than 95%at 300℃,and the loss of NMHCs in the adsorption tubes during 20-days storage at 4℃was less than 8%.The thermal desorption efficiency for C11 NMHCs in the adsorption tube filled with Carbograph 1 and Carbosieve SⅢabsorbents was less than 40%at 300℃,and pyrolysis of the absorbents at 330℃interfered significantly with the measurements of some alkenes.The loss of alkenes was significant when NMHCs were sampled by cryo-enrichment at-90℃in the presence of O3 for the online NMHC measurements,and negligible for enrichment us-ing adsorption tubes at 25℃.Although O_(3)scrubbers have been widely used to eliminate the influence of O_(3)on NMHC measurements,the loss of NMHCs with carbon numbers greater than 8 was more than 10%.Therefore,PVF bags and adsorption tubes filled Carbopack B and Carboxen1000 sorbents were recommended for the sampling of atmospheric NMHCs.

Dispersive Liquid-liquid Microextraction for Simultaneous Determination of Six Parabens in Aqueous Cosmetics

A simple and rapid sample preparation method of dispersive liquid-liquid microextraction（DLLME） was applied in the simultaneous determination of six parabens in the aqueous cosmetics. The analysis was performed on gas chromatography coupled with a flame ionization detection（GC-FID）. The mixed solution containing 30 μL of chloroform（extraction solvent） and 300 μL of tetrahydrofuran（dispersive solvent） was rapidly injected into the sample solution for the purpose of microextraction. After that, the solution mentioned above was centrifuged at 4000 r/min for 10 min, and then the organic sediment phase was detected by GC-FID. The effects of experimental parameters, such as the extraction solvent and the volume of it, and the dispersive solvent and the volume of it, on the yield of the extraction were studied in detail. Under the optimum conditions, the enrichment factors of the target analytes range from 87 to 214. Linearity ranges are 0.05-10.0μg/mL for methylparaben and 0.025--5.0 μg/mL for the other five parabens. The relative standard deviations（RSDs） are lower than 8.2%（n=6）. The proposed method was applied to the analysis of six parabens in eleven aqueous cosmetics. The recoveries of the target analytes in the spiked real samples are in the range of 81.0%-103%.