• Title/Summary/Keyword: gas-liquid chromatography

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Studies on the Lipid Composition in Three Species of Shellfish (3종(種) 패류(貝類)의 지질조성(脂質組成)에 관한 연구(硏究))

  • Son, Young Ock;Ha, Bong Seuk
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.12 no.4
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    • pp.407-419
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    • 1983
  • In this study, the lipid components of three species of shellfish included oyster(Crassostrea gigas), top shell(Turbo cornutus) representing salt water shellfish and corb shell(Corbicula fluminea producta) representing flesh water shellfish were analysed and nutriontional significances were discussed. Analysed the total lipid composition, and the fatty acid and sterol composition of total lipid were determined. The lipid was fractionated into three lipid classes neutral, glyco and phospholipid by column chromatography. The fatty acid composition of each lipid class and sterols were determined by gas liquid chromatography. The lipid components of total lipid and neutral lipid were estimated by thin layer chromatography and TLC scanner. The results were as follows: Total lipid contents of shellfish were 1.8% in oyster, 0.4% in top shell and 4.0% in corb shell. The contents of total fatty acid in total lipid were 80.7, 71.2 and 73.2%; and the contents of unsaponifiable matters were 15.4, 18.1 and 23.1% respectively. Total lipids were mainly composed of triglycerides, polar lipid-pigments and sterols as major component, and hydrocarbon-esterified sterols were determined in each sample. The major fatty acids in total lipid were palmitic(37.0%), eicosapentaenoic(13.5%) and linoleic acid(11.2%) in oyster, Octadecatetraenoic(15.8%), palmitic(11.2%), oleic(8.6%) and linoleic acid(8.1%) in top shell, but palmitic(34.0%), linoleic(12.3%) and paimitoleic acid(9.8%) in corb shell. Particularly, the contents of eicosapentaenoic acid of oyster and top shell were higher than those of corb shell. Sterol composition from three species of shellfish were mainly consisted of cholesterol (42.7~64.0%), brassicasterol(15.6~24.7%) and 24-methylenecholesterol (4.7~21.9%). But sitosterol (5.3%) was detected only in oyster and 22-dehydrocholesterol(12.9%) was only in top shell. The contents of fractionated neutral lipid was commonly higher than that of polar lipid in each sample. Glycolipid and phospholipid in polar lipid showed similar in quantity. The neutral lipids were composed of triglycerides(33.0~36.7%), free sterols(25.7~31.2%), esterified sterol(12.4~23.7%) and free fatty acids(5.1~11.7%). The contents of triglycerides and free sterols were higher than those of free fatty acids and esterified sterols. The major fatty acids in neutral lipid were palmitic(28.4~26.4%) eicosapentaenoic(18.6~21.9%) and linoleic acid(9.0~5.4%) in oyster and corb shell but octadecatetraenoic(14.5%), eicosapentaenoic (13.5%) and palmitic acid(12.3%) in top shell. The major fatty acids in glycolipid were eicosenoic(10.2%), palmitic(12.1%) and linolenic acid (10.2%) in oyster, Eicosenoic(26.0%), octadecatetraenoic(14.6.%) and eicosadienoic acid(12.9%) in top shell. But eicosadienoic(21.4%) stearic(14.6%), octadecatetraenoic(8.5%) and eicosenoic acid(8.5%) in corb shell. The major fatty acids in phospholipid were myristic(16.0%), stearic(10.6%), eicosenoic(10.5%) and palmitic acid(10.3%) in oyster, Oleic(22.2%), stearic(20.7%) and linolenic acid (11.8%) in top shell but eicosapentaenoic(25.1%), myristic(8.7%) and arachidonic acid(8.3%) in corb shell.

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Isolation and In Vitro Antimicrobial Activity of Low Molecular Phenolic Compounds from Burkholderia sp. MP-1 (Brukholderia sp. MP-1 에서의 페놀화합물의 분리와 항균활성의 측정)

  • Mao, Sopheareth;Jin, Rong-De;Lee, Seung-Je;Kim, Yong-Woong;Kim, In-Seon;Shim, Jae-Han;Park, Ro-Dong;Kim, Kil-Yong
    • Korean Journal of Soil Science and Fertilizer
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    • v.39 no.4
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    • pp.195-203
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    • 2006
  • An antagonistic strain, Burkholderia MP-1, showed antimicrobial activity against various filamentous plant pathogenic fungi, yeasts and food borne bacteria (Gram-positive and Gram-negative). The nucleotide sequence of the 16S rRNA gene (1491 pb) of strain MP-1 exhibited close similarity (99-100%) with other Burkholderia 16S rRNA genes. Isolation of the antibiotic substances from culture broth was fractionated by ethyl acetate (EtOAc) solvent and EtOAc-soluble acidic fraction. The antibiotic substances were purified through a silica gel, Sephadex LH-20, ODS column chromatography, and high performance liquid chromatography, respectively. Four active substances were identified as phenylacetic acid, hydrocinnamic acid, 4-hydroxyphenylacetic acid and 4-hydroxyphenylacetate methyl ester by gas chromatographic-mass spectrum analysis. The minimum inhibition of concentration (MIC) of each active compound inhibited the growth of the microorganisms tested at 250 to $2500{\mu}g\;ml^{-1}$. The antimicrobial activity of crude acidic fraction at 1 mg of dry weight per 6 mm paper disc was more effective than authentic standard mixture (four active substances were mixed with the same ratio as acidic fraction) over a wide range of bacterial test.

Comparative Evaluation of the Analytical Methods used to Determine Pesticide Residues in Milk via Dispersive Solid Phase Extraction (Dispersive Solid Phase Extraction을 사용한 우유 내 잔류농약 다성분 동시 분석법 비교연구)

  • Oh, Nam Su;Shin, Yong Kook;Lee, Ji Young;Baick, Seung Chun
    • Journal of Dairy Science and Biotechnology
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    • v.33 no.1
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    • pp.27-34
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    • 2015
  • The aim of this study was to optimize a simple, fast, and economic analytical method for the simultaneous determination of various pesticides (aldrin, p,p'-DDT, o,p'-DDT, p,p'-DDE, ${\alpha}$-endosulfan, ${\beta}$-endosulfan, dieldrin, heptachlor, permethrin, chlordane, deltamethrin, diazinon, bifenthrin, methoprene, propargite, fenpropathrin, cypermethrin, fenvalerate, and fenpropathrin) in milk by using dispersive solid phase extraction (SPE). In this study, two different extraction methods (low temperature cleanup and liquid-liquid partitioning), which were followed by a cleanup process based on dispersive-SPE, were evaluated and compared for the 19 pesticides. The results for all the pesticides were determined by gas chromatography mass spectrometry (GC/MS) with selected-ion monitoring mode, and the matrix effect of the method was evaluated. Comparison of these approaches yielded higher and more consistent recoveries of most pesticides at fortification levels of $1{\mu}g/mL$ using low-temperature fat precipitation, followed by cleanup process based on dispersive-SPE with PSA and C18 as sorbents, than other preparation process. The relative standard deviation was <20 % and the combination of this method were very effective for the cleanup.

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Quantitative Determination of Phenol in Water Using GC-MS after Liquid-Liquid Extraction and Acetylation (액-액 추출과 아세틸화 후 GC-MS를 이용한 물 중 phenol의 분석)

  • Park, Sunyoung;Kim, Yunjeong;Jung, Sungjin;Kim, Hekap
    • Korean Journal of Environmental Agriculture
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    • v.36 no.1
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    • pp.63-66
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    • 2017
  • BACKGROUND: The phenol concentrations in water samples were determined using gas chromatography after derivatization of the analyte to phenyl acetate followed by extraction using a large volume of solvent. However, this procedure requires an additional purification step and is not analytically efficient. METHODS AND RESULTS: In this study, phenol was first extracted from an acidified water sample using ethyl acetate and then acetylated using acetic anhydride in the presence of a small amount of water and $K_2CO_3$. The derivative was extracted using 1mL of n-butyl acetate. One microliter of the extract was analyzed by GC-MS without further purification. The calibration curve showed good linearity with the $r^2$ value of 0.9968. The method detection limit and the limit of quantitation were estimated to be $0.18{\mu}g/L$ and $0.56{\mu}g/L$, respectively. Repeatability (RSD, n=3) and recovery (n=3) were 9.1%-4.3% and 90.6%-110.5%, respectively. The concentrations of phenol in a few samples of stream water were distributed in the range of $2.51-7.51{\mu}g/L$. CONCLUSION: This method is simpler and faster to implement than those currently utilized and shows high analytical reliability. It can be applied to the quantitative determination of phenol concentrations in surface water and groundwater samples.

Optimum Extraction Methods of Volatile Compounds in Beef Extract Powder (쇠고기 엑기스 분말 휘발성 성분의 최적 추출방법에 관한 연구)

  • Kim Hun;Cho Woo-Jin;Jeong Eun-Jeong;Ahn Jun-Suck;Lim Chi-Won;Yoo Young-Jae;Kim Kwang-Ho;Cha Yong-Jun
    • The Korean Journal of Food And Nutrition
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    • v.17 no.4
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    • pp.412-419
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    • 2004
  • In odor to select optimum extraction methods of volatile compounds in beef extract powder(BEP) as basic data for the development of a new detection method of irradiated BEP, four extraction methods, such as solid phase microextraction with polar fiber(S-PD) and non-polar fiber(S-CD), purge and trap(P&T) and liquid liquid continuous extraction(LLCE) methods, were tested with gas chromatography/mass spectrometry method. A total of 106 volatile compounds including 22 hydrocarbons, 7 aldehydes, 6 ketones, 13 alcohols, 6 sulfur-containing compounds, 19 nitrogen-containing compounds, 6 aromatic compounds, 17 terpenes, 8 furans and 2 miscellaneous compounds were detected in BEP by four detection methods. The most compounds(62 compounds) were detected by S-PD method, followed by P&T(43), LLCE(38) and S-CD method(30). Among these methods, S-PD and P&T methods showed a complementary interrelationship to detect volatile compounds as S-PD method showed high detectabiltiy to all compound groups except hydrocarbons and ketones, which had high volatility and low molecular weight(less than RI 1200), but P&T method showed the contrary pattern to that of S-PD method. Moreover, the most of volatile compounds detected by S-CD and LLCE methods were also detectable by S-PD or/and P&T methods. Therefore, the simultaneous application of S-PD and P&T methods were selected as the optimum volatile extraction methods of BEP.

Determination of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCCOOH) in human urine by solid-phase extraction and GC/MS (고체상 추출과 GC/MS를 이용한 소변 중 대마 대사체 (THCCOOH) 분석)

  • Cheong, Jae Chul;Kim, Jin Young;In, Moon Kyo;Cheong, Won Jo
    • Analytical Science and Technology
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    • v.19 no.5
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    • pp.441-448
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    • 2006
  • 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THCCOOH) is the major metabolite of tetrahydrocannabinol (THC) which is the primary psychoactive component of marijuana. It is also the target analyte for the discrimination marijuana use. A method using solid-phase extraction (SPE) and gas chromatography/mass spectrometry (GC/MS) was developed for the determination of THCCOOH in human urine. Urine samples (3 mL) were extracted by SPE column with a cation exchange cartridge after basic hydrolysis. The eluents were then evaporated, derivatized, and injected into the GC/MS. The limits of detection (LOD) and quantitation (LOQ) were 0.4 and 1.2 ng/mL, respectively. The response was linear with a correlation coefficient of 0.999 within the concentration range of 1.2 (LLE 1.3)~50.0 ng/mL. The precision and accuracy were stable within 1.20% and the recovery was 83.6~90.7%. The recovery of SPE method was lower than that of liquid-liquid extraction (LLE), but there were no apparent differences in LOD, LOQ, precision and accuracy between the two methods. While SPE method is used as a very effective and rapid procedure for sample pretreatment, and clean extracts, LLE method was not suitable for the extraction procedure of THCCOOH in urine. The applicability of the method was proven by analyzing a urine samples from a marijuana abusers.

Isolation and Chemical Analysis of Potent Anti-Complementary Polysaccharides from Fruiting Bodies of the Fomes fomentarius (말굽버섯 자실체에서 분리한 항보체 활성 다당체의 화학적 분석)

  • Park, Jung-Keun;Park, Kwe-Won;Shin, Kwang-Soon;Lee, Chang-Muk;Seok, Soon-Ja;Kim, Jeong-Bong;Koo, Bon-Sung;Han, Bum-Soo;Yoon, Sang-Hong
    • Microbiology and Biotechnology Letters
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    • v.41 no.2
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    • pp.198-206
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    • 2013
  • The five anti-complementary polysaccharides (MFKF-NP, MFKF-AP1${\alpha}$, ${\beta}$, and MFKF-AP2${\alpha}$, ${\beta}$) were separated from hot water extracts of fruiting bodies of Fomes fomentarius by two subsequent column chromatography using DEAE-sepharose FF and Concanavalin A-sepharose 4B. The order of anti-complementary activity was MFKF-AP1${\beta}$ > MFKF-AP1${\alpha}$ > MFKF-AP2${\alpha}$ > MFKF-AP2${\beta}$ > MFKF-NP > Polysaccharide Krestine (PSK). Especially, MFKF-AP1${\beta}$ among those showed the most excellent anti-complementary activity (70% of ITCH50 value at $20{\mu}g/ml$). The monosaccharide composition analysis by gas chromatography indicates that MFKF-AP1${\alpha}$ and ${\beta}$ are a kind of homoxylan consisted mainly of xylose above 97%. Molecular weight of MFKF-AP1${\beta}$, major anti-complementary polysaccharide, was estimated to be about 12,000 by high performance liquid chromatography (HPLC). After the incubation of the serum with MFKF-AP1${\beta}$ in the presence or absence of $Mg^{++}$ and $Ca^{++}$ ions, its anti-complementary activity was investigated. This result indicated that MFKF-AP1${\beta}$ seems to be activator both on the classical and the alternative pathway of complement activation.

Comparision of Chemical Compositions between Cultured and Wild Fishes (1) Comparision between Cultured and Wild Eel Lipids (양식 및 천연산 어류의 화학성분에 관한 연구 1) 양식 및 천연산 뱀장어의 지질성분)

  • KIM Kyong-Sam;OK Kwans-Soo;LEE Eung-Ho
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.17 no.6
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    • pp.506-510
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    • 1984
  • The muscle lipids of cultured and wild eel, Anguilla japonica, were analysed by gas chromatography for fatty acid compositions of total lipid(TL), neutral lipid(NL), phospholipid(PL) and glycolipid(GL). And high performance liquid chromatography(HPLC) patterns of NL were analysed by HPLC. The lipid contents of dorsal muscle of cultured fish are slightly lower than that of wild fish. The contents of TL, NL and PL of wild fish were similar to those of cultured fish, while GL content of wild fish was higher than that of cultured one. In the fatty acid compositions of TL, NL and PL, percentages of $C_{16:0},\;C_{18:1}\;and\;C_{22:6}$ in cultured fish are higher than these in wild one, while percentage of $C_{16:1}$ is lower. Elution patterns in HPLC of NL of wild and cultured eel were slightly different.

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A Comparative Study on the Lipid Components of Barley and Malt -I. Composition of Neutral Lipids- (보리와 맥아(麥芽)의 지방질(脂肪質) 성분(成分)에 관한 비교(比較) 연구 -제(第)1보(報) : 중성지질(中性脂質)의 조성(組成)-)

  • Shin, Hyo-Sun;Lee, Kang-Hyon;Lee, Sang-Young
    • Korean Journal of Food Science and Technology
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    • v.13 no.1
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    • pp.30-36
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    • 1981
  • Neutral lipids of the total lipid extracted from 4 representative varieties of barley grown in Korea and their corresponding malt were studied. Total lipids of barley and malt were solvent extracted with chloroform:methanol:water (1.0 : 1.0 : 0.9, v/v), The total lipids were fractionated into neutral and polar lipids by silicic acid column chromatography, and neutral lipids fraction was separated by thin layer chromatography and quantitated by TLC scanner. The fatty acid compositions was determined by gas liquid chromatography. The average content of total lipid in the 4 barleys and their malts were 3.3 and 2.9%, and average of neutral lipids content in the barley and malt lipids were 73.8 and 68.5%, respectively. Among the neutral lipids, triglycerides and free fatty acids were the major components, and triglycerides content decreased and free fatty acids content increased during malting. Sterol esters, free sterols, 1,3-and 1,2-diglycerides were the minor components of the neutral lipids, and contents of those components showed increasing tendency during malting. The major fatty acid composition of the total lipids were linoleic, palmitic and oleic acids, and in general, the malts had lower amounts of unsautrated fatty acids and high amounts of saturated fatty acids. Fatty acid composition of neutral lipids was of almost the same pattern as that of the total lipids.

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Studies on the Lipids Composition of Korean Edible Mushrooms (한국산 식용버섯의 지방질 성분에 관한 연구)

  • Hong, Jai-Sik;Kim, Young-Hoi;Kim, Myung-Kon;Kim, Tae-Young;Kim, Keum-Jae
    • Journal of the Korean Society of Food Culture
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    • v.5 no.4
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    • pp.437-442
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    • 1990
  • Three fractions-neutral lipids, glycolipids and phospholipids were obtained from total lipids in cultivated mushrooms(Pleurotus ostreatus and Pleurotus sajor-caju) and wild mushrooms (Ramaria botrytis and Lactarius volemus), and their lipid compositions and fatty acid compositions were determined by means of silicic acid column chromatography, thin layer chromatography and gas liquid chromatography. The total lipid contents in mushrooms were $0.32{\sim}0.39%$(wet basis). It was found that the contents of phospholipids$(19.4{\sim}47.4%)$ and neutral lipids$(32.1{\sim}51.9%)$ were high, while that of glycolipids$(14.8{\sim}28.7%)$ were low. The main lipid in neutral lipids was triglyceride$(21.2{\sim}38.2%)$ followed by free sterol$(21.0{\sim}21.9%)$, sterol ester$(10.3{\sim}18.6%)$, but the main lipid in neutral lipid of Pleurotus sajor-caju was free fatty acid(34.1%). The main lipid in glycolipids was steryl glycoside$(15.6{\sim}29.4%)$ followed by esterified steryl glycoside$(13.4{\sim}23.9%)$, monogalactosyl diglyceride$(15.6{\sim}24.6%)$. Among the phospholipids, phosphatidyl choline$(36.7{\sim}49.5%)$, phosphatidyl ethanolamine$(20.9{\sim}29.7%)$, phosphatidyl inositol$(18.4{\sim}26.1%)$ were the major components. The major fatty acid of total lipids was linoleic acid followed by palmitic acid, oleic acid. Fatty acid composition was not significantly different among total lipids, neutral lipids, glycolipids and phospholipids contained in tested mushrooms but the main fatty acid in neutral lipid of Ramaria botrytis was oleic acid(48.7%).

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