• Title/Summary/Keyword: Chromatographic Analysis

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PMFs Analysis of Krachaidum Products by HPLC and GC

  • Burapan, Supawadee;Kim, Mihyang;Han, Jaehong
    • Journal of Applied Biological Chemistry
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    • v.57 no.3
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    • pp.211-218
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    • 2014
  • Polymethoxyflavones (PMFs) are a group of polymethoxylated bioactive flavones with diverse biological activities, including anticancer, anti-inflammatory, antibacterial, and antiviral activities. PMFs are found from various plants such as orange, tangerine, and krachaidum. To establish the simple quantitative analytical methods for PMFs, chromatographic analysis was applied to the selected krachaidum foods because krachaidum contains diverse PMFs compared to other PMF-containing foods. Krachaidum is the rhizome of Kaempferia parviflora, and many commercial krachaidum products, such as tea, juice and wine, are commercially available and consumed as health functional foods in Asian countries. Apart from the claimed health promoting benefits, reliable quality assurance and legal guideline for the registration of these products are not available yet. Twelve PMFs were analyzed from the commercial krachaidum foods by GC-FID and HPLC-DAD. No single chromatographic method could not analyze 12 PMFs simultaneously. HPLC-DAD method was found more sensitive to detect PMFs. Based on our analysis data, we proposed 5,7-dimethoxyflaone and 5,7,4'-trimethoxyflavone as index components for the food products.

Identification of Xanthium Sibiricum Components using LC-SPE-NMR-MS Hyphenated System

  • Sohn, Ji Soo;Jung, Youngae;Han, Ji Soo;Hwang, Geum-Sook
    • Journal of the Korean Magnetic Resonance Society
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    • v.22 no.2
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    • pp.26-33
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    • 2018
  • Xanthium sibiricum is used as a traditional folk medicine for the treatment of cancer, fever, headache, nasal sinusitis, and skin pruritus. This study aimed to identify components from Xanthium sibiricum extracts using an SPE-800MHz NMR-MS hyphenated system. The simultaneous acquisition of MS and NMR spectra from the same chromatographic peaks significantly increases the depth of information acquired for the compound and allows the elucidation of structures that would not be possible using MS or NMR data alone. LC -NMR analysis was conducted using a HPLC separation system coupled to 800 MHz spectrometer equipped with a cryoprobe, and a SPE unit was used to automatically trap chromatographic peaks using a HPLC pump. LC-MS analysis was conducted with a Q-TOF MS instrument using ESI ionization in the negative ion mode. Using the hyphenated analysis, several secondary metabolites were identified, such as 3',5'-O-dicaffeoylquinic acid, 1',5'-O-dicaffeoyl- quinic acid, and ethyl caffeate. These results demonstrate that the SPE-800MHz NMR-MS hyphenated system can be used to identify metabolites within natural products that have complex mixtures.

Analysis of Volatile Fatty Acids in Air by Dynamic SPME (Dynamic SPME를 이용한 공기 중 지방산 분석)

  • Yu, Mee-Seon;Yang, Sung-Bong;Ha, Nam-Ki
    • Journal of Environmental Science International
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    • v.19 no.12
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    • pp.1447-1454
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    • 2010
  • In this study, the detection limits of lower fatty acids in air were investigated by using Dynamic SPME(Solid Phase Micro-Extraction), i.e. improved Head Space - SPME method(HS-SPME). This Dynamic SPME, called SPDE(Solid Phase Dynamic Extraction), is the analytical method for volatile compounds in air with the extraction by using a stainless steel needle of which inner surface is coated with adsorption material and following the gas chromatographic analysis by inserting the needle into a injection port of GC and subsequently, desorption of the volatile compounds into a gas-chromatographic column. Extraction was carried out by passing the sample air through the needle with a suction pump which has been used for a detection tube. The result of measurement for the 6 lower fatty acids showed that the detection limits ranged from 0.10 ppm to 0.44 ppm and the linear correlation coefficients were over 0.99. Relative standard deviations obtained from 5 analytical repetition of a ca. 1.6 ppm standard mixture were in the range of 1.87%~2.47%. This method has been shown to be a adequate for the measuring C2~C5 fatty acids in air in the concentrations of over several hundreds ppb.

Evaluation of Sigumjang Aroma by Stepwise Multiple Regression Analysis of Gas Chromatographic Profiles

  • Choi, Ung-Kyu;Kwon, O-Jun;Lee, Eun-Jeong;Son, Dong-Hwa;Cho, Young-Je;Im, Moo-Hyeog;Chung, Yung-Gun
    • Journal of Microbiology and Biotechnology
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    • v.10 no.4
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    • pp.476-481
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    • 2000
  • A linear correlation, by the stepwise multiple regression analysis, was found between the sensory test of Sigumjang aroma and the gas chromatographic data which were transformed with logarithm. GC data is the most objective method to evaluate Sigumjang aroma. A multiple correlation coefficient and a determination coefficient of more than 0.9 were obtained at the 9th and 13th steps, respectively. At step 31, the coefficient of determination level of 0.95 was attained. The accuracy of its estimation became higher as the number of the variables entered into the regression model increased. Over 90% of the Sigumjang aroma was explained by 13 compounds indentified on GC. The contributing proportion of the peak 26 was the highest followed by peaks 57 (9.27%), 29 (7.51%), 54 (6.01%), 8 (5.99%), 49 (4.97%), and 13 (4.11%).

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Determination of Ant Repellents Activity of Cineol, α-Terpineol, Linalool, and Piperitone

  • Shim, Jae-Han;Lee, Chang-Joo;Shen, Jing-Yu;Kim, Yong-Du;Kang, Seong-Koo
    • Journal of Applied Biological Chemistry
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    • v.44 no.3
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    • pp.140-142
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    • 2001
  • Quantitative gas chromatographic method for determining the ant repellent activity of cineol, ${\alpha}$-terpineol, linalool, and piperitone which usually found in Chinese Prickly Ash Zanthoxylum piperitum DC. was developed. These monoterpenes showed higher ant repellent activities than DEET due perhaps to their volatility. Gas chromatographic method quantified the volatility of the four monoterpenes and DEET.

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Purification and reaction pattern of cephalexin synthesizing enzyme from Acetobacter turbidans

  • Kang, Sang-Moo;Kim, June-Hoe;Kim, Deog-Jung;Kim, Young-Jun
    • Proceedings of the Korean Society for Applied Microbiology Conference
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    • 1986.12a
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    • pp.525.2-525
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    • 1986
  • Cephalexin synthesizing enzyme (${\alpha}$ amino acid ester hydrolase) was partially purified from the culture broth of Acetobacter turbidans ATCC9325 through ammonium sulfate fractionation, DEAE, CM, and Sephacryl S-200 gel filtration. The enzyme has optimum pH 6.0 and temperature, 40$^{\circ}C$ respectively. From the analysis of reaction mixtures by thin layer chromatographic and high performance liquid chromatographic techniques, it was confirmed this enzyme catalyzed simultaneously the following reactions : 1) Synthesis of cephalexin from D-${\alpha}$-phenylglycine methylester (PGM) and 7-amino 3-deacetoxy-cetoxycephalosporanic acid (7-ADCA) 2) Hydrolysis of cephalexin to form 7-ADCA and phenylglycine (PG) 3) Hydrolysis of PGM to form PG and methanol. Base on the above experimental observations, the reaction model of this enzyme was identical with that of the enzyme from Xanthomonas citri.

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Determination of Mono- and Oligosaccharides Derivatized with p-Aminobenzoic Ethyl Ester by Reverse Phase HPLC

  • Kwon, Hyokjoon;Kim, Joon
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.859-864
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    • 1995
  • Mono- and oligosaccharides are derivatized with p-aminobenzoic ethyl ester (ABEE), strongly absorbs UV light at 254 nm, in the presence of sodium cyanoborohydride. C18-bonded silica column is used for the separation of sugar-ABEE derivatives in an isocratic mode. RP-HPLC conditions are optimized by using ternary mixture as mobile phase and $45^{\circ}C$ as a column temperature. Sugar-ABEE derivatives are separated well within a short run time (ca. 25 min) by reverse-phase partition chromatographic mode. The ($1{\rightarrow}6$) linkage type of dihexose-ABEE derivatives has shorter retention time than ($1{\rightarrow}4$)-linkage type. After acid hydrolysis of glycoproteins with 2M trifluoroacetic acid, monosaccharide composition and contents are determined. This procedure is very useful for the simultaneous analysis of neutral and amino sugars in a single chromatographic step using RP-HPLC without reacetylation of deacetylated amino sugars, which are produced by acid hydrolysis.

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Chemotaxonomic Studies on the Citrus Plants cultivated in Je Ju Island (제주도산 감귤속 식물의 성분 분류학적 연구)

  • 고명자
    • Journal of Plant Biology
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    • v.25 no.1
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    • pp.9-19
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    • 1982
  • A thin-layer chromatographic study was made of the chloroform-soluble and flavonoid fractions from the fruit peels of 16 species, 2 varieties and 5 formas of the Citrus plants cultivated in Je Ju Island for their interspecific relatinships. In addition, 3 hybrids and 9 native plants were also studied for their taxonomic position. Three phenograms were developed from these chromatographic data after cluster analysis via the unweighted paired group method using rithmatic average by Sneath and Sokal. These plants were grouped into 5 alliences based on the phenogram obtained from the chloroform-soluble fracitons, which were nearly identical to the subgenus rank by Tanaka, and rutinoside and neohesperidoside groups by Horowitz. Those from the flavonoid and methanol-soluble fractions were not able to evaluate the morphological classification except for a few cases.

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Chromatographic Separation of Some Phenol Derivatives Using $\alpha$-Cyclodextrin in Mobile Phase ($\alpha$-씨클로덱스트린을 이동상으로 사용한 몇 가지 페놀 유도체들의 크로마토그래피적 분리)

  • 문영자;김봉희
    • Environmental Analysis Health and Toxicology
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    • v.12 no.3_4
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    • pp.75-84
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    • 1997
  • Chromatographic retention behavior and separation of various phenol derivatives on a Partisil 10 ODS 3 column-with mobile phase containing $\alpha$-cyclodextrin-were systematically studied. The decrease in k' values caused by the addition of cyclodextrins in the mobile phase was based on the formation of an inclusion complex, resulting in weakening of the hydrophobic interaction between solutes and the stationary phase. The content of the organic solvent in the mobile phase also influenced k' values of the solutes, and k' values increased with a decrease of the content of organic solvent in the mobile phase. A simple equation has been derived that reveals the hyperbolic dependence of the capacity factor on the total concentration of cyclodextrin. A plot of the reciprocal of the capacity factor against (CD)$_T$ gives a straight line and the dissociation constant, K$_D$, of the inclusion complex can be calculated from the slope. The capacity factor decreased with increasing temperature. The enthalpy was calculated from the slope of van't Hoff plots. Under optimum conditions, some mixtures of phenol derivatives were able to separated successfully.

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Gas Chromatographic Method for Analysis of Fatty Acids in Milk Fat with a Single Injection

  • Hwang, Keum-Taek;Shin, Min-Kyeong
    • Preventive Nutrition and Food Science
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    • v.11 no.3
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    • pp.253-256
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    • 2006
  • The purpose of this study was to develop a gas chromatographic (GC) method to analyze fatty acids in milk fat with a single injection. The single-injection GC method we developed for analyzing fatty acid composition can separate a wide range of fatty acid methyl esters from butyric acid to docosahexaenoic acid. It separated 6 isomers of 18:1 (cis-6, cis-9, cis-11, trans-6, trans-9 and trans-11), 4 isomers of 18:2 (cis-9-cis-12, trans-9-trans-12, cis-9-trans-12 and trans-9-cis-12), and 4 isomers of conjugated 18:2 (cis-9- trans-11, trans-9-cis-11, cis-10-trans-12 and trans-10-cis-12).