• Title/Summary/Keyword: solvent mixture

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Isolation and Identification of Antimicrobial Active Substances from Rhodiola sachlinensis (홍경천(Rhodiola sachlinensis)에서 항균성 물질의 분리 및 동정)

  • 심창주;이규희;정재홍;이상덕;김영호;오만진
    • Food Science and Preservation
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    • v.11 no.1
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    • pp.63-70
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    • 2004
  • The antimicrobial substances from Rhodiola sachalinensis were extncted, isolated and identified. The highest level of antimicrobial activity and its yield were obtained in methanol extract. The minimum inhibition concentrations of the methanol extract were 500 $\mu\textrm{g}$mL on agar plate and 100 $\mu\textrm{g}$mL in broth media for four gram positive and four gram negative microbials. The methanol extract was fractionated by n-hexane, chloroform, ethyl ether, ethyl acetate, and butanol, orderly. The separate was developed on the TLC plate with different solvent system ratio of chloroform and methanol. Nine substances were isolated from chloroform and methanol mixture(9:1, v/v). Among them, three isolates showed antimicrobial activity. Three substances separated by HPLC were identified by GC/MS(EI) spectrum and $^1$H, /sup13/C-NMR spectrum. They were gallic acid, (-)-epicatechin and kaempferol. The antimicrobial activities of each substances were shown gallic acid, (-)-epicatechin, kaempferol orderly.

A Study on the Comparison of Chemical Characterization and Ellagic Acid Content Between Distribution Bokbunja and Korean Native Bokbunja (국내유통 복분자와 토종복분자의 이화학적 특성과 엘라그산 함량 비교연구)

  • Jung, Sung Hee;Yu, Hye Young;Seo, Ji Ho;Lee, Yong Jae;Han, Min Woo
    • Korean Journal of Plant Resources
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    • v.34 no.2
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    • pp.177-185
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    • 2021
  • The purpose of this study was to compare the chemical properties of the bokbunja distributed in Korea with the content of the bioactive substance ellagic acid. The bokbunja was Rubus coreanus group and Rubus occidentalis group were compared, domestic bokbunja and import bokbunja were compared. In bokbunja, free sugar was 30.89 ± 0.7 mg/g of Rubus coreanus and 29.05 ± 0.87 mg/g of Rubus occidentalis. and 27.28 ± 7.4 mg/g of domestic bokbunja and 21.58 ± 6.73 mg/g of import bokbunja. The free amino acids was 4.50 ± 0.08 mg/g of Rubus coreanus and 5.05 ± 0.08 mg/g of Rubus occidentalis. and 4.13 ± 1.09 mg/g of domestic bokbunja and 3.75 ± 0.31 mg/g of import bokbunja. Validation of the ellagic acid method was confirmed by comparing the retention time and spectrum of the standard and extract using HPLC. The calibration curve (R2) showed linearity of 0.9999. As a result of analyzing the ellagic acid content of each extraction solvent, DMSO and methanol mixture extracts were high, and Rubus coreanus was 2.56 mg/g and Rubus occidentalis was 3.16 mg/g, which was not significantly different (p < 0.05) In addition, the ellagic acid content of domestic bokbunja and import bokbunja was 2.83 mg/g and 2.99 mg/g, which was not significantly different (p < 0.05).

Bioactive Materials and Biological Activity in the Extracts of Leaf, Stem Mixture and Root from Angelica gigas Nakai (참당귀 잎, 줄기혼합물과 뿌리 추출물의 생리활성물질 및 그 활성작용)

  • Heo, Jin-Sun;Cha, Jae-Young;Kim, Hyun-Woo;Ahn, Hee-Young;Eom, Kyung-Eun;Heo, Su-Jin;Cho, Young-Su
    • Journal of Life Science
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    • v.20 no.5
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    • pp.750-759
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    • 2010
  • The bioactive materials (phenolic compounds, flavonoids, minerals, decursin and decursinol angelate) and biological activities (DPPH [$\alpha,\alpha$'-diphenyl-$\beta$-picrylhydrazyl] free radical scavenging capability, reducing power, and tyrosinase activity) in the extracts of leaf, stem mixture (AGLS), and root (AGR) from Angelica gigas Nakai were examined by using water, hot water and ethanol solvent. The highest extract yield (21.89%) was found in the water extract of AGR. The highest concentrations of phenolic compounds and flavonoids in the ethanol extracts of AGLS and AGR were 14.99% and 14.79%. Major minerals of AGLS and AGR were K, Mg, Fe, Na and Ca. Decursin and decursinol angelate were the major ingredients of Angelica gigas, detected at 18.71 and 18.89 min of retention time by HPLC analysis, respectively. The highest concentrations of decursin and decursinol angelate in the Angelica gigas ethanol extract were found in root ($41.7\;{\mu}g/g$) and leaf ($34.04\;{\mu}g/g$). The highest free radical scavenging activity was found in the hot water extracts of AGLS and AGR, and its activity was stronger in all extracts of AGLS than AGR. The highest reducing power was found in the ethanol extracts of AGLS and AGR and this was dependent on the sample concentration. The hot water extracts of AGLS and AGR revealed the highest inhibition activity on tyrosinase. Overall, these results may provide the basic data needed to understand the biological activities of bioactive materials derived from Angelica gigas.

Radiosynthesis of $[^{11}C]6-OH-BTA-1$ in Different Media and Confirmation of Reaction By-products. ($[^{11}C]6-OH-BTA-1$ 조제 시 생성되는 부산물 규명과 반응용매에 따른 표지 효율 비교)

  • Lee, Hak-Jeong;Jeong, Jae-Min;Lee, Yun-Sang;Kim, Hyung-Woo;Lee, Eun-Kyoung;Lee, Dong-Soo;Chung, June-Key;Lee, Myung-Chul
    • Nuclear Medicine and Molecular Imaging
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    • v.41 no.3
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    • pp.241-246
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    • 2007
  • Purpose: $[^{11}C]6-OH-BTA-1$ ([N-methyl-$^{11}C$]2-(4'-methylaminophenyl)-6-hydroxybenzothiazole, 1), a -amyloid imaging agent for the diagnosis of Alzheimer's disease in PET, can be labeled with higher yield by a simple loop method. During the synthesis of $[^{11}C]1$, we found the formation of by-products in various solvents, e.g., methylethylketone (MEK), cyclohexanone (CHO), diethylketone (DEK), and dimethylformamide (DMF). Materials and Methods: In Automated radiosynthesis module, 1 mg of 4-aminophenyl-6-hydroxybenzothiazole (4) in 100 l of each solvent was reacted with $[^{11}C]methyl$ triflate in HPLC loop at room temperature (RT). The reaction mixture was separated by semi-preparative HPLC. Aliquots eluted at 14.4, 16.3 and 17.6 min were collected and analyzed by analytical HPLC and LC/MS spectrometer. Results: The labeling efficiencies of $[^{11}C]1$ were $86.0{\pm}5.5%$, $59.7{\pm}2.4%$, $29.9{\pm}1.8%$, and $7.6{\pm}0.5%$ in MEK, CHO, DEK and DMF, respectively. The LC/MS spectra of three products eluted at 14.4, 16.3 and 17.6 mins showed m/z peaks at 257.3 (M+1), 257.3 (M+1) and 271.3 (M+1), respectively, indicating their structures as 1, 2-(4'-aminophenyl)-6-methoxybenzothiazole (2) and by-product (3), respectively. Ratios of labeling efficiencies for the three products $([^{11}C]1:[^{11}C]2:[^{11}C]3)$ were $86.0{\pm}5.5%:5.0{\pm}3.4%:1.5{\pm}1.3%$ in MEK, $59.7{\pm}2.4%:4.7{\pm}3.2%:1.3{\pm}0.5%$ in CHO, $9.9{\pm}1.8%:2.0{\pm}0.7%:0.3{\pm}0.1%$ in DEK and $7.6{\pm}0.5%:0.0%:0.0%$ in DMF, respectively. Conclusion: The labeling efficiency of $[^{11}C]1$ was the highest when MEK was used as a reaction solvent. As results of mass spectrometry, 1 and 2 were conformed. 3 was presumed.

Characterization of a Psychrophilic Metagenome Esterase EM2L8 and Production of a Chiral Intermediate for Hyperlipemia Drug (메타게놈유래의 저온성 에스터라제 EM2L8의 효소적 특성과 이를 활용한 고지혈증 치료제 키랄소재의 생산)

  • Jung, Ji-Hye;Choi, Yun-Hee;Lee, Jung-Hyun;Kim, Hyung-Kwoun
    • Microbiology and Biotechnology Letters
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    • v.37 no.2
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    • pp.118-124
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    • 2009
  • Esterase EM2L8 gene isolated from deep sea sediment was expressed in Escherichia coli BL21 (DE3) and the esterase activity of the cell-free extract was assayed using p-nitrophenyl butyrate-spectrophotometric method. Its optimum temperature was $40-45^{\circ}C$ and 45% activity of the maximum activity was retained at $15^{\circ}C$. The activation energy at $15-45^{\circ}C$ was calculated to be 4.9 kcal/mol showing that esterase EM2L8 was a typical cold-adapted enzyme. Enzyme activity was maintained for 6 h and 4 weeks at $30^{\circ}C$ and $4^{\circ}C$, respectively. When each ethanol, methanol, and acetone was added to the reaction mixture to 15% concentration, enzyme activity was maintained. In the case of DMSO, enzyme activity was kept up to 40% concentration. (S)-4-Chloro-3-hydroxy butyric acid is a chiral intermediate for the synthesis of Atorvastatin, a hyperlipemia drug. When esterase EM2L8 (40 U) was added to buffer solution (1.2 mL, pH 9.0) containing ethyl-(R,S)-4-chloro-3-hydroxybutyrate (38 mM), it was hydrolyzed into 4-chloro-3-hydroxy butyric acid with a rate of $6.8\;{\mu}mole/h$. The enzyme hydrolyzed (S)-substrate more rapidly than (R)-substrate. When conversion yield was 80%, e.e.s value was 40%. When DMSO was added, hydrolysis rate increased to $10.4\;{\mu}mole/h$. The plots of conversion yield vs e.e.s in the presence or absence of DMSO were almost same, implying that the reaction enantioselectivity was not changed by the addition of DMSO. Taken together, esterase EM2L8 had high activity and stability at low temperatures as well as in various organic solvents/aqueous solutions. These properties suggested that it could be used as a biocatalyst in the synthesis of useful pharmaceuticals.

Changes in Cordycepin and Liquiritigenin Content and Inhibitory Effect on NO Production in Fermented Licorice and Dongchunghacho (동충하초균주로 발효한 감초의 주요성분 함량 변화 및 NO 생성 억제 효과)

  • Wang, Ziyu;Li, Mei;Li, Ke;Son, Beung Gu;Kang, Jum Soon;Park, Young Hoon;Lee, Yong Jae;Kim, Sun Tae;Jung, Jae-Chul;Lee, Young Guen;Choi, Young Whan
    • Journal of Life Science
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    • v.27 no.1
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    • pp.57-66
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    • 2017
  • Traditional Korean fermented herbal plants are potential sources of new food that promote health, but they are still produced by yeast, fungi or bacteria fermentation. In the present work, mushroom (Paecilomyces tenuipes and Cordyceps militaris) fungal dongchunghacho were used to fermented Glycyrrhiza uralensis Fischer (licorice) or mixed with pupa. The pupa were tested as solid substrates for the production of corcycepin, liquiritin, and liquiritigenin. The fermented substrates were analyzed the content of cordycepin, liquiritin, liquiritigenin, and glycirrhizin productivity and inhibitory activity of NO. The cordycepin content of 70% EtOH extract from the fermented mixture of licorice and 50% pupa with C. militaris increased maximum at 33 times. Pupa was very excellent for the production of cordycepin. The liquiritin content was decreased in all the assays inoculated with P. tenuipes and C. militaris dongchunghachos. The liquiritigenin content was higher when fermented with P. tenuipes than C. militaris. The addition of pupa significantly reduced the liquiritin content and glycyrrhizin production. As a result, the liquiritigenin content increased in fermented P. tenuipes and C. militaris, and liquiritin and glycyrrhizin decreased. The inhibition of NO production in the different ethanolic extracts fermented with licorice and pupa was also significantly increased and higher than that of a nonfermented extract in higher polar solvent extracts. The contents of cordycepin and biological active compounds were altered in accordance with the concentration of pupa and fungi. This study provides basic data for use in developing dongchunghacho fungi as a functional food resource.

The Dynamic and Histologic Changes of Variously Fixed Bovine Pericardiums Specimens after Mechanical Fatigue Stimuli (다양한 고정 처리법을 이용한 소 심낭의 기계적 피로 자극 후 역학적 및 조직학적 변화)

  • Chang, Hyoung-Woo;Kim, Yong-Jin;Kim, Soo-Hwan;Park, Ji-Eun;Park, Chun-Soo;Kim, Woong-Han;Kim, Kyung-Hwan
    • Journal of Chest Surgery
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    • v.42 no.2
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    • pp.148-156
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    • 2009
  • Background: As cardiovascular operations become more complex and sophisticated, there is an increasing need for various bioprostheses for use as components of blood vessels and heart valves. We developed a fatigue stimuli test instrument to objectively evaluate the mechanical durability of a bioprosthesis, and we tested several currently known processing methods for bovine pericardium and we then compared the results. Material and Method: Fresh bovine pericardium was collected at the butcher shop with using aseptic technique, and each piece of pericardium was fixated and/or decellularized by 16 representative methods. We measured the permeability and compliance of the processed bovine pericardium samples, and measured them again after exposure to the fatigue stimuli. All the pieces of pericardium underwent microscopic examinations before and after the fatigue stimuli. Result: A mixture of glutaraldehyde and solvent treatment showed better mechanical durability than did the single glutaraldehyde treatment. High concentration glutaraldehyde treatment showed equal or no worse results than did low concentration glutaraldehyde treatment. After SDS (sodium dodecylsulfate) decellularization, the mechanical property of the bioprosthesis became much worse ($20{\sim}190$ times) and the mechanical durability to the fatigue stimuli was also very poor. Conclusion: We obtained the basic durability data after various fixation methods with using a home-made fatigue test instrument.

Preparation and Properties of Crosslinked Thermo-responsive Poly(N-isopropylacrylamide) Gel Materials For Smart Windows - Effect of Glycerol Content in Water/Glycerol Solvent - (스마트 윈도우용 가교 열감응성 폴리(N-이소프로필아마이드) 겔 소재의 제조 및 특성 - 물/글리세롤 혼합용매 중의 글리세롤 함량의 영향 -)

  • Park, Jae-Hyong;Kim, Il-Jin;Lee, Dong-Jin;Sim, Jae-Hak;Song, Min-Seop;Lee, Young-Hee;Yoo, Jung-Whan;Kim, Han-Do
    • Clean Technology
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    • v.24 no.2
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    • pp.112-118
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    • 2018
  • Thermo-responsive polymers that exhibit phase transition in response to temperature change can be used as materials for smart windows because they can control solar light transmission depending on the outside temperature. The development of thermo-responsive polymers for smart windows that can be used over a wide temperature range is desirable. To obtain high performance smart windows materials, three-dimensional thermo-responsive poly(N-isopropylacrylamide) (PNIPAm) gels were prepared by free radical polymerization from monomer N-isopropylacrylamide, N, N'-methylenebis acrylamide (MBAm) as a crosslinking agent, ammonium persulfate (APS) as a strong oxidizing agent/tetramethylene diamine as a catalyst, and a mixture of two solvents (water/glycerol). This study examined the effect of glycerol content on the lower critical solution temperature (LCST), freezing temperature and the solar light transmittance of crosslinked PNIPAm gel films. The LCST and freezing temperature of PNIPAm gel films were found to be significantly decreased from 34.3 and $6.3^{\circ}C$ to 28.2 and $-6.5^{\circ}C$ with increasing glycerol content from 0 wt% to 10 wt%, respectively. It was found that the transparent PNIPAm gel films at $25^{\circ}C$ (temperature < LCST) were converted to translucent gels at higher temperature ($45^{\circ}C$) (temperature > LCST). These results suggested that the crosslinked PNIPAm gel materials prepared in this study could have high potential for application in smart glass materials.

Stereospecific Analysis of the Molecular Species of the Triacylglycerols Containing Conjugate Trienoic Acids by GLC-Mass Spectrometry in Combination with Deuteration and Pentafluorobenzyl Derivatization Techniques (중수소화(重水素化), Pentafluorobenzyl화(化)와 GLC-Mass Spectrometry에 의한 Conjugate Trienoic Acid함유(含有) Triacylglycerol 분자종(分子種)의 입체특이적 분석(分析))

  • Woo, Hyo-Kyeng;Kim, Seong-Jin;Joh, Yong-Goe
    • Journal of the Korean Applied Science and Technology
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    • v.18 no.3
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    • pp.214-232
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    • 2001
  • CTA ester bonds in TG molecules were not attacked by pancreatic lipase and lipases produced by microbes such as Candida cylindracea, Chromobacterium viscosum, Geotricum candidium, Pseudomonas fluorescens, Rhizophus delemar, R. arrhizus and Mucor miehei. An aliquot of total TG of all the seed oils and each TG fraction of the oils collected from HPLC runs were deuterated prior to partial hydrolysis with Grignard reagent, because CTA molecule was destroyed with treatment of Grignard reagent. Deuterated TG (dTG) was hydrolyzed partially to a mixture of deuterated diacylglycerols (dDG), which were subsequently reacted with (S)-(+)-1-(1-naphthyl)ethyl isocyanate to derivatize into dDG-NEUs. Purified dDG-NEUs were resolved into 1, 3-, 1, 2- and 2, 3-dDG-NEU on silica columns in tandem of HPLC using a solvent of 0.4% propan-1-o1 (containing 2% water)-hexane. An aliquot of each dDG-NEU fraction was hydrolyzed and (fatty acid-PFB ester). These derivatives showed a diagnostic carboxylate ion, $(M-1)^{-}$, as parent peak and a minor peak at m/z 196 $(PFB-CH_{3})^{-}$ on NICI mass spectra. In the mass spectra of the fatty acid-PFB esters of dTGs derived from the seed oils of T. kilirowii and M. charantia, peaks at m/z 285, 287, 289 and 317 were observed, which corresponded to $(M-1)^{-}$ of deuterized oleic acid ($d_{2}-C_{18:0}$), linoleic acid ($d_{4}-C_{18:0}$), punicic acid ($d_{6}-C_{18:0}$) and eicosamonoenoic acid ($d_{2}-C_{20:0}$), respectively. Fatty acid compositions of deuterized total TG of each oil measured by relative intensities of $(M-1)^-$ ion peaks were similar with those of intact TG of the oils by GLC. The composition of fatty acid-PFB esters of total dTG derived from the seed oils of T. kilirowii are as follows; $C_{16:0}$, 4.6 mole % (4.8 mole %, intact TG by GLC), $C_{18:0}$, 3.0 mole % (3.1 mole %), $d_{2}C_{18:0}$, 11.9 mole % (12.5 mole %, sum of $C_{18:1{\omega}9}$ and $C_{18:1{\omega}7}$), $d_{4}-C_{18:0}$, 39.3 mole % (38.9 mole %, sum of $C_{18:2{\omega}6}$ and its isomer), $d_{6}-C_{18:0}$, 41.1 mole % (40.5 mole %, sum of $C_{18:3\;9c,11t,13c}$, $C_{18:3\;9c,11t,13r}$ and $C_{18:3\;9t,11t,13c}$), $d_{2}-C_{20:0}$, 0.1 mole % (0.2 mole % of $C_{20:1{\omega}9}$). In total dTG derived from the seed oils of M. charantia, the fatty acid components are $C_{16:0}$, 1.5 mole % (1.8 mole %, intact TG by GLC), $C_{18:0}$, 12.0 mole % (12.3 mole %), $d_{2}-C_{18:0}$, 16.9 mole % (17.4 mole %, sum of $C_{18:1{\omega}9}$), $d_{4}-C_{18:0}$, 11.0 mole % (10.6 mole %, sum of $C_{18:2{\omega}6}$), $d_{6}-C_{18:0}$, 58.6 mole % (57.5 mole %, sum of $C_{18:3\;9c,11t,13t}$ and $C_{18:3\;9c,11t,13c}$). In the case of Aleurites fordii, $C_{16:0}$; 2.2 mole % (2.4 mole %, intact TG by GLC), $C_{18:0}$; 1.7 mole % (1.7 mole %), $d_{2}-C_{18:0}$; 5.5 mole % (5.4 mole %, sum of $C_{18:1{\omega}9}$), $d_{4}-C_{18:0}$ ; 8.3 mole % (8.5 mole %, sum of $C_{18:2{\omega}6}$), $d_{6}-C_{18:0}$; 82.0 mole % (81.2 mole %, sum of $C_{18:3\;9c,11t,13t}$ and $C_{18:3 9c,11t,13c})$. In the stereospecific analysis of fatty acid distribution in the TG species of the seed oils of T. kilirowii, $C_{18:3\;9c,11t,13r}$ and $C_{18:2{\omega}6}$ were mainly located at sn-2 and sn-3 position, while saturated acids were usually present at sn-1 position. And the major molecular species of $(C_{18:2{\omega}6})(C_{18:3\;9c,11t,13c})_{2}$ and $(C_{18:1{\omega}9})(C_{18:2{\omega}6})(C_{18:3\;9c,11t,13c})$ were predominantly composed of the stereoisomer of $sn-1-C_{18:2{\omega}6}$, $sn-2-C_{18:3\;9c,11t,13c}$, $sn-3-C_{18:3\;9c,11t,13c}$, and $sn-1-C_{18:1{\omega}9}$, $sn-2-C_{18:2{\omega}6}$, $sn-3-C_{18:3\;9c,11t,13c}$, respectively, and the minor TG species of $(C_{18:2{\omega}6})_{2}(C_{18:3\;9c,11t,13c})$ and $ (C_{16:0})(C_{18:3\;9c,11t,13c})_{2}$ mainly comprised the stereoisomer of $sn-1-C_{18:2{\omega}6}$, $sn-2-C_{18:2{\omega}6}$, $sn-3-C_{18:3\;9c,11t,13c}$ and $sn-1-C_{16:0}$, $sn-2-C_{18:3\;9c,11t,13c}$, $sn-3-C_{18:3\;9c,11t,13c}$. The TG of the seed oils of Momordica charantia showed that most of CTA, $C_{18:3\;9c,11t,13r}$, occurred at sn-3 position, and $C_{18:2{\omega}6}$ was concentrated at sn-1 and sn-2 compared to sn-3. Main TG species of $(C_{18:1{\omega}9})(C_{18:3\;9c,11t,13t})_{2}$ and $(C_{18:0})(C_{18:3\;9c,11t,13t})_{2}$ were consisted of the stereoisomer of $sn-1-C_{18:1{\omega}9}$, $sn-2-C_{18:3\;9c,11t,13t}$, $sn-3-C_{18:3\;9c,11t,13t}$ and $sn-1-C_{18:0}$, $sn-2-C_{18:3\;9c,11t,13t}$, $sn-3-C_{18:3\;9c,11t,13t}$, respectively, and minor TG species of $(C_{18:2{\omega}6})(C_{18:3\;9c,11t,13c})_{2}$ and $(C_{18:1{\omega}9})(C_{18:2{\omega}6})(C_{18:3\;9c,11t,13c})$ contained mostly $sn-1-C_{18:2{\omega6}$, $sn-2-C_{18:3\;9c,11t,13t}$, $sn-3-C_{18:3\;9c,11t,13t}$ and $sn-1-C_{18:1{\omega}9}$, $sn-2-C_{18:2{\omega}6}$, $sn-3-C_{18:3\;9c,11t,13t}$. The TG fraction of the seed oils of Aleurites fordii was mostly occupied with simple TG species of $(C_{18:3\;9c,11t,13t})_{3}$, along with minor species of $(C_{18:2{\omega}6})(C_{18:3\;9c,11t,13t})_{2}$, $(C_{18:1{\omega}9})(C_{18:3\;9c,11t,13t})_{2}$ and $(C_{16:0})(C_{18:3\;9c,11t,13t})$. The sterospecific species of $sn-1-C_{18:2{\omega}6}$, $sn-2-C_{18:3\;9c,11t,13t}$, sn-3-C_{18:3\;9c,11t,13t}$, $sn-1-C_{18:1{\omega}9}$, $sn-2-C_{18:3\;9c,11t,13t}$, $sn-3-C_{18:3\;9c,11t,13t}$ and $sn-1-C_{16;0}$, $sn-2-C_{18:3\;9c,11t,13t}$, $sn-3-C_{18:3\;9c,11t,13t}$ are the main stereoisomers for the species of $(C_{18:2{\omega}6})(C_{18:3\;9c,11t,13t})_2$, $(C_{18:1{\omega}9})(C_{18:3\;9c,11t,13t})_{2}$ and $(C_{16:0})(C_{18:3\;9c,11t,13t})$, respectively.