• Title/Summary/Keyword: Column extraction

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Pattern Recognition of the Herbal Drug, Magnoliae Flos According to their Essential Oil Components

  • Jeong, Eun-Sook;Choi, Kyu-Yeol;Kim, Sun-Chun;Son, In-Seop;Cho, Hwang-Eui;Ahn, Su-Youn;Woo, Mi-Hee;Hong, Jin-Tae;Moon, Dong-Cheul
    • Bulletin of the Korean Chemical Society
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    • v.30 no.5
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    • pp.1121-1126
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    • 2009
  • This paper describes a pattern recognition method of Magnoliae flos based on a gas chromatographic/mass spectrometric (GC/MS) analysis of the essential oil components. The botanical drug is mainly comprised of the four magnolia species (M. denudata, M. biondii, M. kobus, and M. liliflora) in Korea, although some other species are also being dealt with the drug. The GC/MS separation of the volatile components, which was extracted by the simultaneous distillation and extraction (SDE), was performed on a carbowax column (supelcowax 10; 30 m{\time}0.25 mm{\time}0.25{\mu}m$) using temperature programming. Variance in the retention times for all peaks of interests was within RSD 2% for repeated analyses (n = 9). Of the 74 essential oil components identified from the magnolia species, approximately 10 major components, which is $\alpha$-pinene, $\beta$-pinene, sabinene, myrcene, d-limonene, eucarlyptol (1,8-cineol), $\gamma$-terpinene, p-cymene, linalool, $\alpha$-terpineol, were commonly present in the four species. For statistical analysis, the original dataset was reduced to the 13 variables by Fisher criterion and factor analysis (FA). The essential oil patterns were processed by means of the multivariate statistical analysis including hierarchical cluster analysis (HCA), principal component analysis (PCA) and discriminant analysis (DA). All samples were divided into four groups with three principal components by PCA and according to the plant origins by HCA. Thirty-three samples (23 training sets and 10 test samples to be assessed) were correctly classified into the four groups predicted by PCA. This method would provide a practical strategy for assessing the authenticity or quality of the well-known herbal drug, Magnoliae flos.

Quantification of Entacapone in Human Plasma by HPLC Coupled to ESI-MS/MS Detection: Application to Bioequavalence Study (체외에서 ESI-MS/MS 탐지에 연결된 HPLC에 의한 Entacapon의 수량화: 생물학적 동등성 연구에 적용)

  • Balasekhara Reddy., Ch.;Baburao., Ch.;Chandrasekhar., K.B.;Kanchanamala., K.;RihanaParveen., S.K.;Ravikumar., Konda
    • Journal of the Korean Chemical Society
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    • v.54 no.5
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    • pp.523-532
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    • 2010
  • The proposed method is simple, sensitive and specific Liquid chromatography-tandem mass spectrometry (LCESI-MS/MS) method for the quantification of Entacapone (EA) in human plasma using Entacapone-d10 (EAD10) as an internal standard (IS). Chromatographic separation was performed on Zorbax SB-C18, $2.1{\times}50\;mm$, $5\;{\mu}m$ column, mobile phase composed of 10 mM Ammonium formate (pH 3.0): Acetonitrile (60:40 v/v), with a flow-rate of 0.7 mL/min, followed by Liquid-liquid extraction. EA and EAD10 were detected with proton adducts at m/z $306.1{\rightarrow}233.1$ and $316.3{\rightarrow}233.0$ in multiple reaction monitoring (MRM) positive mode respectively. The method was validated over a linear concentration range of 1.00 - 2000.00 ng/mL with correlation coefficient ($r^2$) $\geq$ 0.9993. Intra and inter-day Precision within 3.60 to 7.30 and 4.20 to 5.50% and Accuracy within 97.30 to 104.20 and 98.30 to 105.80% proved for EA. This method is successfully applied in the bioequivalence study of healthy Indian human volunteers.

A Road Feature Extraction and Obstacle Localization Based on Stereo Vision (스테레오 비전 기반의 도로 특징 정보 추출 및 장애 물체 검출)

  • Lee, Chung-Hee;Lim, Young-Chul;Kwon, Soon;Lee, Jong-Hun
    • Journal of the Institute of Electronics Engineers of Korea SC
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    • v.46 no.6
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    • pp.28-37
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    • 2009
  • In this paper, we propose an obstacle localization method using a road feature based on a V-disparity map binarized by a maximum frequency value. In a conventional method, the detection performance is severely affected by the size, number and type of obstacles. It's especially difficult to extract a large obstacle or a continuous obstacle like a median strip. So we use a road feature as a new decision standard to localize obstacles irrespective of external environments. A road feature is proper to be a new decision standard because it keeps its rough feature very well in V-disparity under environments where many obstacles exist. And first of all, we create a binary V-disparity map using a maximum frequency value to extract a road feature easily. And then we compare the binary V-disparity map with a median value to remove noises. Finally, we use a linear interpolation for rows which have no value. Comparing this road feature with each column value in disparity map, we can localize obstacles robustly. We also propose a post-processing technique to remove noises made in obstacle localization stage. The results in real road tests show that the proposed algorithm has a better performance than a conventional method.

Method Development for the Profiling Analysis of Urine Globotriaosylceramide (Gb3) for the Screening of Fabry Disease by Tandem Mass Spectrometry (ESI-MS/MS를 이용한 소변 중 Globotriaosylceramide(Gb3)의 정량 및 임상 응용; 패브리병(Fabry) 진단)

  • Yoon, Hye-Ran;Cho, Kyung-Hee;Kang, Seung-Woo;Kwon, Young-Joo;Jeong, Choon-Sik;Lee, Yong-Soo
    • YAKHAK HOEJI
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    • v.51 no.2
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    • pp.96-102
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    • 2007
  • Measurement of globotriaosylceramide (Gb3, ceramide trihexoside) in urine has clinical importance for monitoring after enzyme replacement therapy in Fabry disease patients. The disease is an X-linked lipid storage disorder that results from a deficiency of the enzyme ${\alpha}$-galactosidase A (${\alpha}$-Gal A). The lack of ${\alpha}$-Gal A causes an intracellular accumulation of glycosphingolipids, mainly Gb3. A simple, rapid, and highly sensitive analytical method for Gb3 in urine was developed without labor-extensive pre-treatment by electrospray ionization MS/MS (ESI-MS/MS). Only simple 5-fold dilution of urine is necessary for the extraction and isolation of Gb3 in urine. Gb3 in diluted urine was dissolved in dioxane containing C17:0 Gb3 as an internal standard. After centrifugation it was directly injected and analyzed through guard column by in combination with multiple reaction monitoring mode of ESI-MS/MS. Eight isoforms of Gb3 were completely resolved from urine matrix. C24:0 Gb3 occupied 50% of total Gb3 as a major component in urine. Linear relationship for Gb3 isoforms was found in the range of 0.005${\sim}$5.0 ${\mu}$g/ml. The limit of detection (S/N=5) was 0.005 ${\mu}$g/ml and limit of quantification was 0.05 ${\mu}$g/ml for C24:0 Gb3 with acceptable precision and accuracy. Correlation coefficient of calibration curves for 8 Gb3 isoforms ranged from 0.9598 to 0.9975. This method could be useful for rapid and sensitive 1st line Fabry disease screening, monitoring and/or diagnostic tool for Fabry disease.

Studies on the Lipid Components of Potato Tubers - I. Lipid Composition in Free and Bound Lipids - (감자의 지방질(脂肪質) 성분(成分)에 관한 연구(硏究) - 제(第) 1보(報) : 유리(遊離) 및 결합(結合) 지질(脂質)중의 지방질(脂肪質) 조성(組成)에 관하여 -)

  • Lee, Sang-Young;Shin, Hyo-Sun
    • Korean Journal of Food Science and Technology
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    • v.11 no.4
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    • pp.291-297
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    • 1979
  • The experimentally cultivated potatoes of 4 varieties, Irish Cobbler, Warba, Shimabara, and Saco were dried in a frozen state, powdered subsequently and subjected to the extraction of free and bound lipids. Constituents of the prepared lipids were fractionated, quantified, and compared by the methods of column and gas-liquid chromatographies. The results were summarized as follows : 1. The total crude lipid content in potato on a dry weight basis was 0.57 % of which 0.2 % was free lipid and 0.37 % was bound lipid. 2. The neutral lipid content in the free lipid was 14.9 %, approximately 3 times as much as the 4.5 % contained in the bound lipid, whereas the glycolipid content in the free lipid was 15.1 %, slightly less than 22.2 % contained in the bound lipid. However, the phospholipid content was 33.9 % in the bound lipid, approximately 4.5 times as much as the 7.2 % contained in the free lipid. This fact revealed that the bound lipid consisted mainly of polar lipid, while the free lipid consisted of neutral lipids, glycolipids and phospholipids in about the same proportion. 3. The main fatty acids constituting more than 90 % in the free and bound lipids were linoleic, palmitic and linolenic acids. The content of the saturated fatty acid was slightly less in the free lipid than in the bound lipid, whereas the unsaturated fatty acids were more abundant in the free lipid.

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Validation of the LC-MS/MS Method for Ginsenoside Rb1 Analysis in Human Plasma (LC-MS/MS를 이용한 인체 혈장에서 Ginsenoside Rb1의 분석법 검증)

  • Han, Song-Hee;Kim, Yunjeong;Jeon, Ji-Young;Hwang, Minho;Im, Yong-Jin;Lee, Sun Young;Chae, Soo-Wan;Kim, Min-Gul
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.41 no.12
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    • pp.1753-1757
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    • 2012
  • A new liquid chromatographic tandem mass spectrometric (LC-MS/MS) assay for the quantification of ginsenoside Rb1 in human plasma was developed and validated. The separation was performed on a Agilent C18 column ($4.6mm{\times}150mm$, particle size 5 ${\mu}m$) with a gradient elution of 0.1% formic acid in water and 0.1% formic acid in methanol and a flow rate of 0.9 mL/min. The analyte was determined using electrospray positive ionization mass spectrometry in the multiple reaction monitoring (MRM) mode (m/z 1131.714${\rightarrow}$365.303). Human plasma samples were extracted with acetone : water (50:50) by the liquid-liquid extraction method. The method was linear over the dynamic range of 10~500 ng/mL with a correlation coefficient of r=0.9995. The intra-and inter-day precision over the concentration range of ginsenoside Rb1 was lower than 5.8% (correlation of variance, CV), and the accuracy was between 96.0~104.6%. This LC-MS/MS assay of ginsenoside Rb1 in human plasma is applicable for quantification in a pharmacokinetic study.

Purification and Properties of ${\beta}-Mannanases$ from Germinated Guar Bean (${\beta}-Mannanase$ 군(群)의 정제(精製) 및 그들의 성질(性質)에 관(關)한 연구(硏究))

  • Lee, Su-Rae
    • Applied Biological Chemistry
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    • v.7
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    • pp.1-13
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    • 1966
  • 1) Three ${\beta}-1$, 4-mannanases were isolated from germinated guar bean through extraction, ammonium sulfate fractionation, column chromatography on cellulose derivatives and gel filltration on Sephadex G-100. They were designated as ${\beta}-1$, 4-mannanase A,B and C, respectively, in the order of isolation. 2) These enzymes were different in several aspects such as pH optimum, effect of metal ions, adsorbability on cellulose derivatives, molecular weight, Michaelis constant toward reduced ivory nut mannan A, mode of action and extent of hydrolysis of the mannan. 3) ${\beta}-1$, 4-Mannanases A and C were proposed to be two different endo-enzymes of random-splitting type producing a series of oligosaccharides from ${\beta}-1$, 4-mannans. ${\beta}-1$, 4-Mannanase B was suggested to be possibly an exe-type enzyme catalyzing a stepwise splitting from the non-reducing end of ${\beta}-1$, 4-mannans to produce mannose. 4) Guaran was subjected to hydrolysis by the purified enzymes and the consequence was discussed in connection with structural requirements of the enzymes toward substituted ${\beta}-1$, 4-mannans and their role in germinating guar seeds.

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The VHR Dual-Specificity Protein Tyrosine Phosphatase (DS-PTPase) Inhibitor Isolated from Gastrodia elata (천마(Gastrodia elata)로부터 분리한 VHR DS-PTPase 저해 물질)

  • Lee, Myung-Sun;Oh, Won-Keun;Bae, Eun-Young;Ahn, Soon-Cheol;Sohn, Cheon-Bae;Osada, Hiroyuki;Ahn, Jong-Seog
    • Korean Journal of Food Science and Technology
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    • v.34 no.3
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    • pp.505-509
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    • 2002
  • In the course of screening program for VHR DS-PTPase (dual-specificity protein tyrosine phosphatase) from natural sources, Gastrodia elata was selected. One compound showing potent inhibitory activity was isolated by the solvent extraction and column chromatography including silica gel, ODS RP-18, Sephades LH-20, and HPLC. This compound was identified as baicalein by several NMR techniques such as $^1H-NMR$, $^{13}C-NMR$, and DEPT. Baicalein showed selective inhibitory activity against VHR DS-PTPase with $IC_{50}=2.4\;{\mu}M$, and showed cytotoxicity against several human cancer cell lines with an $GI_{50}$ of $5.26{\sim}12.93\;{\mu}g/mL$ range, including, melanoma (LOX-IMVI), lung cancer (NCI H23 and A549), colon cancer (HCT 116 and SW 620), prostate cancer (PC-3), and leukemia (MOLT 4F).

A Method for Simultaneous Analysis of Phthalate Esters and Di-(2-ethylhexyl) Adipate Migrated from PVC Wraps into Fatty Food (PVC Wraps에서 지방함유 식품으로 이행되는 Phthalate esters 및 Di-(2-ethylhexyl) adipate의 동시 분석법)

  • Lee, Kwang-Ho;Jeon, Dae-Hoon;Jeong, Dong-Youn;Choi, Byung-Hee;Kim, Sung-Wook;Lee, Chul-Won
    • Korean Journal of Food Science and Technology
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    • v.32 no.6
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    • pp.1244-1250
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    • 2000
  • A method for simultaneous quantitative determination of plasticizers such as diethyl phthalate(DEP), di-n-propyl phthalate(DprP), di-n-butyl phthalate(DBP), di-n-pentyl phthalate(DPP), butylbenzyl phthalate(BBP), di-(2-ethylhexyl) phthalate(DEHP), dicyclohexyl phthalate(DCHP) and di-(2-ethylhexyl) adipate(DEHA), which are suspected as endocrine disruptors, in food was studied. A analysis method was optimized for the quantification of plasticizers in Jjambbong, which is a kind of fatty noodle, by using GC/FID. The detection limits of DEP, DprP, DBP, DPP, BBP, DEHP, DCHP and DEHA were 3.5, 5.3, 2.2, 2.2, 7.2, 1.7, 1.9 and 3.0 mg/kg, respectively. Much higher recovery was obtained by extraction with acetone/n-hexane(1:1) rather than hexane solvent system. The recovery of DEP, DprP, DBP, DPP, BBP, DEHP, DCHP and DEHA were 72.7, 85.9, 91.4, 97.1, 100.8, 103.2, 104.3 and 95.8% after 4 time extractions, respectively. The migration of plasticizers from PVC wraps into PVC wrap covered Jjambbong was conducted after shaking(120 rpm) for 30min at room temperature with chosen solvent system. It was found that the migration level of DEHA were 577, 706, 770 mg/kg into Jjambbong, respectively, while the other plasticizers were not observed.

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Quantitative Determination of Marker Compounds in the Extracts of Camellia sinensis L. Sub-branches (Residual Products) by HPLC (HPLC에 의한 차나무 잔가지(부산물)의 추출물 내 지표 성분의 정량분석)

  • Lee, Min Sung;Im, Hyeon Jeong;Jeong, Hea Seok;Cho, Hae Jin;Woo, Hyun Sim;Oh, Yu Jin;Lee, Soo In;Kim, Hyun Chul;Ahn, Kyung Wan;Kim, Yeong Su;Kim, Dae Wook
    • Korean Journal of Medicinal Crop Science
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    • v.27 no.1
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    • pp.24-29
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    • 2019
  • Background: Camellia sinensis L.(CS) is a perennial evergreen species of plant whose leaves are used to produce tea. In this plant species, the parts used are the leaves, sub-branch parts are thrown out. Methods and Results: Ethanol extract of sub-branch parts was used for isolation of major compounds by column chromatography. Structures were identified as caffeine (1), (-)-epicatechin (2) and (-)-epicatechin gallate (3) by interpretation of spectroscopic analysis, including $^1H$- and $^{13}C$-NMR. High-performance liquid chromatography (HPLC) method was used to compare the quantitative level of marker compounds in various extraction solvents of sub-branch parts of CS. The content of caffeine, (-)-epicatechin, and (-)-epicatechin gallate in 30% ethanol extract showed higher value with $3.28{\pm}0.57mg/g$, $5.53{\pm}0.88mg/g$, and $1.29{\pm}0.24mg/g$, respectively. Conclusions: These results indicated that not only leaves parts but also sub-branch, could be a good source for the functional material and pharmaceutical industry.