• Title/Summary/Keyword: Capillary column gas chromatography

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Quantitative Determination of the Marker Components in Pyungwi-San Using LC-ESI-MS/MS (LC-ESI-MS/MS를 이용한 평위산 주요 성분의 함량 분석)

  • Seo, Chang-Seob;Shin, Hyeun-Kyoo
    • Korean Journal of Pharmacognosy
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    • v.49 no.3
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    • pp.270-277
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    • 2018
  • Pyungwi-san has been used to treat the digestive system diseases, physconia, nausea, anorexia, and dyspepsia in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was optimized for simultaneous determination of the 14 marker components, spinosin, liquiritirn apioside, liquiritin, narirutin, 6'''-feruloylspinosin, hesperidin, liquiritigenin, glycyrrhizin, 6-gingerol, atractylenolide III, honokiol, atractylenolide II, magnolol, and atractylenolide I in Pyungwi-san extract. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) with maintained at $45^{\circ}C$. The mobile phase consisted of 0.1% (v/v) aqueous formic acid and acetonitrile. The MS conditions were as follows: capillary voltage 3.3 kV, extractor voltage 3.0 V, RF lens voltage 0.3 V, source temperature $120^{\circ}C$, desolvation temperature $300^{\circ}C$, desolvation gas 600 L/h, cone gas 50 L/h and collision gas 0.14 mL/min. The coefficient of determination of 14 analytes was 0.9989-1.0000. The limits of detection and quantification values of the all analytes were 0.04-2.56 and 0.13-7.69 ng/mL, respectively. As a result of the analysis using the established LC-ESI-MS/MS method, the 5 components, spinosin, 6'''-feruloylspinosin, atractylenolide III, II, and I derived from Zizyphi Fructus and Atractylodis Rhizoma, were not detected in this extract. On the other hand, the 9 components except for the 5 components were 4.15-498.87 mg/kg in lyophilized Pyungwi-san extract. Among these components, glycyrrhizin, marker compound of Glycyrrhizae Radix et Rhizoma, was detected the most amount as a 498.87 mg/kg.

Analysis of Trans Fatty Acid Content in Retort Food, Powdered Milk, Biscuit and Pizza Products (레토르트식품, 분유, 비스킷 및 피자 내에 함유되어 있는 트랜스지방산 함량 분석)

  • Park, Da-Jung;Park, Jung-Min;Shin, Jin-Ho;Song, Jae-Cheol;Kim, Jin-Man
    • Food Science of Animal Resources
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    • v.28 no.2
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    • pp.240-245
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    • 2008
  • The consumption of foods containing trans fatty acids (TFAs) is a matter of concern at present. According to many studies, trans fatty acids (TFAs) may cause illnesses such as the coronary heart disease, diabetes mellitus, large intestine cancer, and breast cancer. They can also raise low density lipoprotein (LDL) cholesterol and reduce high density lipoprotein (HDL) cholesterol. TFAs can also inhibit the synthesis of phospholipids containing polyunsaturated fatty acids in arterial cells. As a consequence the Food and Drug Administration has deemed that saturated fatty acid, cholesterol and trans fatty acid levels be listed on food labels as of 2006. The Korea Food and Drug Administration also has required the listing of trans fatty acid content on food labels since 2007. The aim of this study was to determine the total lipid and trans fatty acid (TFA) contents in retort food, powdered milk, biscuit and pizza products. The number of samples examined were 2 retort food, 6 powdered milk, 7 biscuit and 3 pizza products. The extraction of total lipids in retort food and powdered milk followed the chloroform methanol method. The extraction of total lipids in biscuit and pizza was by the acid digestion method. All samples were analyzed by gas chromatography (GC) using a SP-2560 capillary column and a flame ionization detector. The TFA contents per 100g of sample were 1-2.8% (1.9%) in retort foods, 0.4-2.4% (1.37%) in powdered milk products, 0-2.9% (1.23%) in biscuits, and 2.8-3.45% (3.03%) in pizzas.

Chiral Separation of Derivatized Racemic Alcohols on Substitued Cyclodextrin Stationary Phases by Capillary Gas Chromatography (모세관 기체 크로마토그래피에 의한 치환된 Cyclodextrin 정지상을 이용한 알코올 유도체의 키랄분리)

  • Lee, Sun-Haing;Seo, Yeong-Ju;Lee, Kwang-Pill
    • Journal of the Korean Chemical Society
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    • v.39 no.2
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    • pp.94-102
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    • 1995
  • S-Hydroxypropyl(PH) ${\beta}$-cyclodextrin(hydrophilic), dialkyl(DA)-cyclodextrin(hydrophobic), trifluoroacetyl(TA) ${\gamma}$-cyclodextrin(intermediate) stationary phases were used for gas chromatographic separation of racemic alcohols and their derivatives. All the alcohols used for this experiment were derivatived by using trifluoro acetic anhydride, acetic anhydride, or trichloro acetic anhydride. It is apparent that the enantioselectivity of the enantiomeric pairs was very dependent on the type of acylation reagent. The best experimental condition of optical resolution of the alcohols and their derivatives was different on the polarity of the solute molecules. The chiral separation was also studied depending on temperature, polarity of the column, and hydrogen bonding ability and steric effect between the alchols and CD stationary phase. The chiral recognition mechanism is dependent not upon the kinds of the chiral stationay phases but upon the derivatization of the racemic alchols.

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Optimization of Soybean Oil Fatty Acid Methyl Esters Preparation for Sucrose Polyesters Synthesis (Sucrose polyesters 합성에 사용하는 대두유 지방산 메틸에스테르 제조의 최적화)

  • Chung, Ha-Yull;Kim, Suk-Ju;Yoon, Sung-Woo;Yoon, Hee-Nam;Kong, Un-Young
    • Korean Journal of Food Science and Technology
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    • v.24 no.3
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    • pp.240-246
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    • 1992
  • Preparation of soybean oil fatty acid methyl esters (soybean oil FAME) through the transesterification of soybean oil with alkaline catalyst was optimized in terms of contents of residual free fatty acids (FFA) in soybean oil FAME and yield of soybean oil FAME due to the inhibitory effect of FFA on sucrose polyesters synthesis. Soybean oil FAME and residual FFA were analyzed quantitatively by simultaneous gas chromatography on a fused silica capillary column after converting the FFA in soybean oil FAME to tert.-butyldimethylsilyl (TBDMS) derivatives. Transesterification of soybean oil was successfully performed with alkaline catalyst (NaOH, 95%), which resulted in 99.1% yield of soybean oil FAME and less than 0.1% residual FFA contents under the conditions such as $30^{\circ}C$, 20min. and 6:1 molar ratio of anhydrous methanol to soybean oil.

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Methodological Research on the Instruments of Fatty Acids Determination (지방산의 기기 측정 방법에 관한 연구)

  • 박선미;안명수
    • Korean journal of food and cookery science
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    • v.7 no.1
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    • pp.45-51
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    • 1991
  • In this study, several standard fatty acids were analyzed by three analysis instruments. And also, for the two kinds of soybean oils, fatty acids compositions were determined by three instruments. The results were obtained as follows: 1. In the case of Gas Chromatography (GC), standard fatty acids (Myristic, Stearic, Linoleic, Linolenic, Arachidonic acid) were determined with high reproducibility, but oleic acid/elaidic acid were not seperated. By Capillary Gas Chromatography (CGC), most of standard fatty acids were determined with very high reproducibility than saturated fatty acids, and palmitic acid/oleic acid were not seperated. 2. In the analytical ability of cis-trans fatty acids isomer (oleic acid/elaidic acid), CGC was shown better analytical ability of geometrical isomer than HPLC. Oleic acid/elaidic acid were not seperated by packed column (15% DEGS). The rquire time for standard fatty acids analysis was as follows; GC, 7.21 min., CGC, 9.84 min., HPLC, 24.48 min. 3. The major compositions of fatty acids of each soybean oil (CSOY; refined, DSOY; unrefined) by GC and CGC were linoleic acid, oleic acid, palmitic acid, linolenic acid and stearic acid. But in the case of HPLC, palmitic acid/oleic acid were not seperated. Analytical ability of three instruments on fatty acids composition in each soybean oil was same trend as in the standard fatty acids mixture.

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Improvement of Analysis Methods for Fatty Acids in Infant Formula by Gas Chromatography Flame-Ionization Detector (GC-FID를 이용한 조제유류 중 지방산 분석법 개선 연구)

  • Hwang, Keum Hee;Choi, Won Hee;Hu, Soo Jung;Lee, Hye young;Hwang, Kyung Mi
    • Journal of Food Hygiene and Safety
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    • v.36 no.1
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    • pp.34-41
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    • 2021
  • The purpose of this research is to improve analysis methods of determining the contents of fatty acids in infant formulas and follow-up formulas. A gas chromatography (GC) method was performed on a GC system coupled to flame ionization detector, with a fused silica capillary column (SP2560, 100 m×0.25 mm, 0.20 ㎛). The method was validated using standard reference material (SRM, NIST 1849a). Performance parameters for method validation such as specificity, linearity, limits of detection (LOD) and quantification (LOQ), accuracy and precision were examined. The linearity of standard solution with correlation coefficient was higher than 0.999 in the range of 0.1-5 mg/mL. The LOD and LOQ were 0.01-0.06 mg/mL and 0.03-0.2 mg/mL, respectively. The recovery using standard reference material was confirmed and the precision was found to be between 0.8% and 2.9% relative standard deviation (RSD). Optimized methods were applied in sample analysis to verify the reliability. All the tested products had acceptable contents of fatty acids compared with component specification for nutrition labeling. The result of this research will provide efficient experimental information and strengthen the management of nutrients in infant formula and follow-up formula.

Changes of Volatile Flavor Compounds of Seibel Grape Must during Alcohol Fermentation and Aging (Seibel 포도즙 알코올 발효 및 저장 중 휘발성 향기성분의 변화)

  • 고경희;장우영
    • Microbiology and Biotechnology Letters
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    • v.27 no.6
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    • pp.491-499
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    • 1999
  • A great variety of the volatile metabolic by-products was formed in yeast cell during alcohol fermentation. The seibel grape (Vitis labrasca) which was grown in the Southern Korea used for wines. The objective of this research was to identify the volatile flavor compounds during alcohol fermentation and aging at 12$^{\circ}C$. saccharomyces cerevisiae and Schizosaccharomyces pombe were inoculated and fermented in seibel grape must. The volatile flavor compounds of logarithmic, stationary and death phases were extracted, concentrated and identified by gas chromatography/mass spectrometer (GC/MS). The volatile flavor compounds were determined by a Hewlett-Packard 5890 II Plus GC which was equipped with Supelcowax 10 fused silica capillary column (60m$\times$0.32mm$\times$0.25${\mu}{\textrm}{m}$ film thickness) wall coated with polyethyleneglycerol. The scan detection method allowed the comparison of the spectrum from the chromatogram of volatile flavor compounds to those in data Wileynbs base library. Among the volatile compounds collected by ether-hexane extraction method, the evolution of 20 main compounds, such as 9 esters (ethyl butyrate, isoamyl acetate, ethyl caproate, n-hexyl acetate, ethl caprylate, ethyl caprate, diethy succinate, ethyl hexadecanoate, 2-pheneethyl acetate), 4 alcohols (3-methyl-1-butanol, 1-hexanol, 1-heptanol, benzoethanol), 4 ketones and acids (2-octanone, caproic acid, caprylic acid, capric acid), 2 furan and phenol (2,6-bis(1,1-dimethyl ethyl)phenol, 2,3-dihydrobenzofuran) were observed during alcohol fermentation and aging. The production of the esters during alcohol fermentation with S. cerevisiae was higher than those of Sch. pombe. The sensory scores of the aged wine samples in aroma, taste and overall acceptability were not significantly different(p<0.05).

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Characterization of a lipopolysaccharide-protein complex of type A Pasteurella multocida (Pasteurella multocida type A의 lipopolysaccharide-protein 복합체의 특성)

  • Ryu, Hyo-ik;Kim, Chul-joong
    • Korean Journal of Veterinary Research
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    • v.40 no.1
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    • pp.63-71
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    • 2000
  • An immunogenic, high molecular weight lipopolysaccharide (LPS)-protein complex isolated from a potassium thioncyanate extract of a Pasteurella multocida (P multocida ; strain P-2383, capsular type A and somatic type 3) was characterized. Chemical analysis of the complex by gas chromatography on a capillary column demonstrated that this complex contained most of the chemical constituents characteristic of LPS extracted by the phenol-water methed from the whole bacterium. However, there was proportionately more carbohydrate than fatty acid in the complex in contrast to LPS in which fatty acid seemed to be in excess. When toxicity of the complex was evaluated in 10-day-old chicken embryos, the complex was less toxic ($LD_{50}=12.72{\mu}g$) than the purified LPS ($LD_{50}=0.44{\mu}g$). The $LD_{50}$, of the LPS moiety extracted from the complex was $5.24{\mu}g$. Composition of the complex was analyzed by SDS-PAGE with silver staining and Western immunoblotting. The complex did not migrate through the polyacrylamide gel unless dissociated with SDS. The complex dissociated with SDS contained at least 32 different protein and polysaccharide components: 18 components reacted with an antiserum against the complex. There was no significant compositional variation between the complexes from different strains, but quantitative differences in individual components were noted. When cross-protectivity of the complex was evaluated in mice, this complex provided substantial protection not only against the homologous bacteriun but also against different P multocida strains of the same serotype. LPS-protein complexes isolated by the same method from other strains also induced protection against an challenge with P-2383.

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Development of Biologically Active Compounds from Edible Plant Sources-XI -Analysis of Phytol Content in Several Varieties of Lactuca sativa L. by gas chromatography- (식용식물자원으로부터 활성물질의 탐색-XI -GC를 이용한 상추(Lactuca sativa L.)의 품종별 Phytol 함량 분석-)

  • Song, Myoung-Chong;Lee, Jin-Hee;Bang, Myun-Ho;Kim, Ji-Young;Chung, Dae-Kyun;Pai, Tong-Kun;Kim, In-Ho;Baek, Nam-In
    • Applied Biological Chemistry
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    • v.47 no.4
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    • pp.426-429
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    • 2004
  • An easy, sensitive and rapid method for the analysis of phytol, a strong ACAT (Acyl-CoA: Cholesterol Acyltransferase) inhibitory diterpenoid, was established. The pre-treatment of sample for GC analysis of phytol includes aq. MeOH extraction, partition of the extracts between EtOAc and water, and filtration of organic phase through Supelclean LC-Si SPE tube. The GC analysis of phytol for a variety of Lactuca sativa was carried out on DB-5 capillary column with flame ionization detector (FID). The consistency in phytol contents according to each variety was not shown. Especially, Jeoktoma, as RS-2 type, showed the highest phytol content.

Oxidative Characteristics of Triglyceride Molecular Species in the Presence of Prooxidants (산화촉진제 공존하에서의 트리글리세리드 분자종의 산화특성)

  • Yoon, Hyeung-Sik;Kim, Seon-Bong;Park, Yeung-Ho
    • Korean Journal of Food Science and Technology
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    • v.22 no.1
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    • pp.7-12
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    • 1990
  • The effect of $Fe^{2+}$ and myoglobin on the oxidative stability of triglyceride molecular species was investigated at $25^{\circ}C$. The molecular species of soybean oil triglycerides were analyzed by capillary column gas chromatography and electron impact ionization mass spectrometry utilizing selected ion monitoring. When $Fe^{2+}$ and myoglobin were added to soybean oil triglycerides, the oxidative stability of each molecular species of triglycerides appeared to decrease in proportion to the increase in the number of double bonds present in the acyl residues, and it was affected by degree of unsaturation of fatty acid when the total degree of unsaturation of triglyceride was the same. But the length of the saturated acyl chain had no influence on the stabilization of unsaturated fatty acid present in the same glyceride when prooxidants were added.

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