• Journal of the Korean Applied Science and Technology
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• v.4 no.1
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• pp.9-18
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• 1987

The effects of procedures for preparation of fatty acid methyl esters for gas chromatography were investigated. A quantitative comparison of four procedures for the preparation of the fatty acid methyl esters from Korean sesame seed lipids which can be representative of fatty acid ranges of Korean vegetable oils has been made. The procedures employed were $BF_3$-methanol, HCI-methanol, sodium methoxide-methanol, and tetramethylammonium hydroxide-methanol. Twelve fatty acids ranged from 14:0 to 24:0 were identified in the lipids from Korean white and black sesame seeds. All four procedures gave similar results for the fatty acids, 16:0, 18:0, 18:1, 18:2, and 18:3 present in the range of $1{\sim}44%$ but only in the HCI-methanol procedure, the fatty acids, 16:1, 20:0, 22:0, 24:0 present in the range of $0.02{\sim}1%$ showed the lowest values. When using tetramethylammonium hydroxide-methanol procedure for determination of total fatty acid composition from white and black sesame seed lipids, unsaponifiable matters including sesamol, sesamolin and sesamin present in the seed lipids are not removed from the resulting reaction mixture. Thus the transesterification mixture is used without further treatment for injection into the gas chromatography. However, the gas chromatographic analysis of the transesterification mixture showed that the unsaponifiable matters had no effect on the fatty acid composition of the seed lipids. From the results, it appears that the $BF_3$-methanol, sodium methoxide-methanol and tetramethylammonium hydroxide-methanol procedures can be used to prepare fatty acid methyl esters from Korean vegetable oils. Among the methods, the tetramethylammonium hydroxide-methanol procedure, which give total fatty acid composition, glyceride fatty acid composition and composition of free fatty acids present, appears to be a simple, convenient and quantitative procedure and applicable to samples containing broad ranges of fatty acids.

• Analytical Science and Technology
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• v.31 no.3
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• pp.112-121
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• 2018

The hydrothermal carbonization method has received great attention because of the conversion process from biomass. The reaction produces various products in hydrochar, bio-liquid, and gas. Even though its yield cannot be ignored in amount, it is difficult to find research papers on bio-liquid generated from the hydrothermal carbonization reaction of biomass. In particular, the heterogeneity of feedstock composition may make the characterization of bio-liquid different and difficult. In this study, bio-liquid from the hydrothermal carbonization reaction of food wastes at $230^{\circ}C$ for 4 h was investigated. Among various products, fatty acid methyl esters were analyzed using two different extraction methods: liquid-liquid extraction and column chromatography. Different elutions with various solvents enabled us to categorize the various components. The eluents and fractions obtained from two different extraction methods were analyzed by gas chromatography with a mass spectrometer (GC/MS). The composition of the bio-liquid in each fraction was characterized, and seven fatty acid methyl esters were identified using the library installed in GC/MS device.

• Applied Biological Chemistry
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• v.9
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• pp.29-33
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• 1968

Through an experiment with gas chromatography carried out using diethylene glycol succinate(DEGS) as the packing material of the column, we have obtained the correction factor between the weight ratio and the peak dimension of the saturated fatty acid methyl esters of C10, C12, C14, C16, and C18 and unsaturated fatty acid methyl esters of oleic acid, linoloic acid, and linolenic acid, employing the detector of thermal conductivity type. Quantitative analysis of the fatty acids contained in rice Bran oil was performed with the above correction factor and the results are as follows; 1. Main components were found to be palmitic acid, oleic acid sand linolenic acid. No trases of capric acid (C10) lauric acid (C10) were found. 2. It was confirmed that there were straight line relation between the logarism retention time of each fatty acid and the number of carbon of saturated fatty acid or the number of double bond of other fatty acids having the same number of carbon. 3. The correction factor became larger as to the number of carbon increased up to C18 in case of saturated fatty acids, end as for other fatty acids, and as for other fatty acids of the same carbon number, it became larger according as the number of double bond increased.

• Mass Spectrometry Letters
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• v.4 no.4
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• pp.75-78
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• 2013

A gas chromatography/mass spectrometric (GC/MS) method was developed as a candidate reference method for the accurate determination of essential fatty acids (linoleic acid, ${\alpha}$- and ${\gamma}$-linolenic acids) in food supplemental oil products. Samples were spiked with three internal standards (stearic acid-$d_{35}$, $^{13}C_{18}$-linoleic acid, and $^{13}C_{18}$-${\alpha}$-linolenic acid). Samples were then subject to saponification, derivatization for methylation, and extraction by organic solvent. For GC/MS measurement, an Agilent HP-88 column, designed for the separation of fatty acid methyl esters, was selected after comparing with other columns as it provided better separation for target analytes. Target analytes and internal standards were detected by selected ion monitoring of molecular ions of their methyl ester forms. The GC/MS method was applied for the measurement of three botanical oils in NIST SRM 3274 (borage oil, evening primrose oil, and flax oil), and measurement results agreed with the certified values. Measurement results for target analytes which have corresponding isotope-labeled analogues as internal standard were calculated based on isotope dilution mass spectrometry (IDMS) approach, and compared with results calculated by using the other two internal standards. Results from the IDMS approach and the typical internal standard approach were in good agreement within their measurement uncertainties. It proves that the developed GC/MS method can provide similar metrological quality with IDMS methods for the measurement of fatty acids in natural oil samples if a proper fatty acid is used as an internal standard.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.45 no.3
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• pp.211-215
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• 2000

Lipid extraction preceding fatty acid methyl esters preparation for gas-liquid chromatography is time-consuming and cumbersome. We performed one-step extraction/methylation method with a mixture of methanol-heptane-benzene-DMP-H$_2$SO$_4$ without prior fat extraction. The simultaneous digestion and lipid transmethylation takes place at 8$0^{\circ}C$ in a single phase. After cooling till room temperature, two phases are formed. The upper one of the phases contains the fatty acid methyl esters ready for GLC. The fatty acid composition of major industrial crops obtained by the one step extraction/methylation method (method 1 and 2) was almost identical with the fatty acid composition of the pure fats extracted with hexane by the Soxtec instrument (method 3). Due to its simplicity, speed, and reduced organic solvent the one-step extraction/methylation method (method 1 and 2) should be useful to determine overall fatty acid composition, especially in situations where many samples have to be analyzed.

• Korean Chemical Engineering Research
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• v.46 no.4
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• pp.747-751
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• 2008

The effect of additives in the synthesis of biodiesel fuel using supercritical methanol was studied in order to examine the possibility of application of spent vegetable oil as a raw material, which has high contents of water or free fatty acid. The experiments were performed by varying the contents of water, free fatty acid or antioxidants respectively in a batch reactor. The contents of fatty acid methyl ester was analyzed by a gas chromatography. As the water contents increased, the contents of fatty acid methyl ester decreased, however, the decrease was very little compared with the alkaline and acid catalyst. The effect of the contents of free fatty acid, vitamin E, and ${\beta}$-carotene was negligible.

• Journal of Nutrition and Health
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• v.11 no.1
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• pp.9-16
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• 1978

A Comparison of the analysis of the green and roast coffee of Arabica and Robusta compositions and regular instant coffee has been investigated by chromatography. The coffee oil were obtained by extracting the green and roast coffee with ethyl ether by soxhlet methood. Instant coffee samples were accurately weighted into 100ml beaker (ca. 0.5g regular coffee and 1.5g decaffeinated coffee) and add ca. 50ml water, heat and boil, remove from heat, and mechanically stried ca. 15min. and filtered of one sample and another sample were without filtrated and proceed with liquid chromatographic separation. The fatty acid compositions of green and roast coffee were compared by gas liquid chromatography and general chemical compositions of sample were analysed. Some similarities between green and roast coffee fatty acids were found in the case of green and roast coffee of both kinds acid methyl esters. They contained stearic, oleic, linoleic, and unknown fatty acid, and palmitic ana linoleic acid were rich.

• Journal of the East Asian Society of Dietary Life
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• v.23 no.4
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• pp.451-460
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• 2013

The purpose of this study is to investigate the volatile compounds of Korean traditional gochujang from various districts. The volatiles from each traditional gochujang are being extracted by simultaneous steam distillation extraction (SDE), and analyzed by gas chromatography (GC) and gas chromatography/mass spectrometry (GC/MS). Twenty compounds are identified as major volatile components which include 8 esters, 4 alcohols and 4 acids. The most traditional gochujang possesses more volatile components rather than commercial gochujang products. Most acids come from fatty acids and the alcohols derive from the oxidative degradation of linolenic acid. The most abundant volatile compounds for both traditional and commercial gochujang include 10 compounds such as 2-methyl-1-propanol, hexanal, 2-methyl-1-butanol, octanoic acid ethyl ester, as well as the various type of acids and esters. They represent most of the total GC peak areas, respectively. From the results, the characteristics of the flavors for traditional gochujang from each district are not clear but have shown various components than the commercial products.

• Korean Journal of Pharmacognosy
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• v.6 no.1
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• pp.15-21
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• 1975

The free fatty acids were prepared from the ethereal fraction of Panax ginseng. The prepared acids were methylated with diazomethzne. The methyl esters of saturated and unsaturated fatty acids were separated by the means of mercuric acetate method and column chromatography. The separated methyl esters were gaschromatographed and analyzed. The obtained conclusions were as follows. 1. The root of six-year old Korean Panax ginseng contains 0.28% of free fatty acids. 2. It was found that 24 kinds of free fatty acids existed in Panax ginseng. Among them, 22 kinds of free fatty acids were indentified by the gas chromatogram and the graphical method but the rest, 2 kinds of them were not identified by the only gas chromatographical data. The amount of each free fatty acid which was not identified was predominant and they were supposed to be unusual free fatty acids which would not commonly exist in nature. These results were shown in Table III. 3. $L_{EE}$ and $L_{EE}$ reported that n18:3 existed in Panax ginseng. However, in this experiment, n18:3 did not exist in Panax ginseng, and instead, peak XVI appeared between n18:2 and n18:3 as shown in Fig. 9.

• Entomological Research
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• v.48 no.6
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• pp.490-498
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• 2018

Ruspolia differens (Serville) (Orthoptera: Tettigoniidae) is a highly valued edible grasshopper species in Africa. However, the effects of plant diets on lipid content and fatty acid composition of R. differens are not well understood. We tested the effects of four diets on the total lipid content and fatty acid composition of R. differens. Sixth instar nymphs of R. differens were reared on one, and mixtures of two, three, and six natural plant inflorescences. Individuals collected from the field constituted a control treatment. We extracted lipids and analyzed the fatty acid methyl esters using gas chromatography-mass spectrometry. We analyzed if the total lipid content, body weight, and fatty acid composition differed among diets and between the sexes using two-way ANOVAs and a PERMANOVA model, respectively. The total lipid content and weight of R. differens did not differ among the diets. The nine common fatty acids were palmitic (mean across treatments, 26%), oleic (22%), palmitoleic (18%), linoleic (13%), stearic (7%), myristic (6%), myristoleic (4%), ${\alpha}$-linolenic (2%) and arachidic acid (1%). The composition of fatty acids and the proportion of essential fatty acids significantly differed among the diets. The proportion of essential fatty acids was highest in the control treatment (21%) but low in less diversified (one to three feed) diets (12-13%). This study demonstrates that the fatty acid composition in R. differens can be influenced through diet. Thus, with dietary manipulations, using local plants in Africa, it is possible to produce R. differens with preferred high quality essential fatty acids for human consumption.