• 제목/요약/키워드: HPLC Chromatography

검색결과 2,217건 처리시간 0.031초

2'-deoxyribonucleosides의 단일 및 다성분계의 비선형 흡착평형식 (Nonlinear Adsorption Isotherm of Single and Multi-Components of 2'-Deoxyribonucleosides)

  • 김룡매;한순구;최대기;노경호
    • Korean Chemical Engineering Research
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    • 제43권2호
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    • pp.230-235
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    • 2005
  • 2'-deoxyribonucleosides중에서 dUrd(2'-deoxyuridine), dGuo(2'-deoxyguanosine), dAdo(2'-deoxyadenosine)의 단일 및 다성분계의 흡착평형식을 동적방법으로 구하기 위해 물과 메탄올(90/10, vol%)을 이동상으로 하는 역상 액체 크로마토그래피를 사용하였다. 시료의 주입부피가 증가함에 따라서 체류시간이 짧아지고 피크가 삼각형 모양을 보여서, Langmuir 흡착평형식으로 가정하였다. PIM (pulsed-input method)에 의해서 Langmuir 흡착평형식의 매개변수를 구하고, 경쟁적인 다성분계의 흡착평형식을 사용하였다. 체류시간이 짧은 dUrd와 dGuo의 경우에서는 단일 및 다성분계에서 실험값과 계산값이 잘 일치하였지만, 가장 늦게 용출되는 dAdo에서는 비이상 비선형적인 특성으로 인해서 약간의 오차가 있었다.

국내 시장에서 유통되는 국내·외 초콜릿의 지방산 조성 및 triacylglycerol 조성 분석 (Fatty acid composition and triacylglycerol species of the domestic and foreign chocolates collected from the market)

  • 현진우;신정아;이기택
    • 농업과학연구
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    • 제40권1호
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    • pp.35-45
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    • 2013
  • The fat content, fatty acid composition, trans fatty acid content and triacylglycerol (TAG) composition of 22 chocolates (domestics 8, foreigns 14) collected from the Korea distribution markets were investigated. The crude fat was extracted by acid hydrolysis method and analyzed by gas chromatography (GC) and reversed-phase HPLC for fatty acid and TAG compositions, respectively. The crude fat content of all chocolates varied between 30.11% and 49.59%. The major fatty acids in most of the chocolates were palmitic acid (19.36~31.15 wt%), stearic acid (5.11~36.32 wt%) and oleic acid (18.77~36.68 wt%). Whereas lauric acid (approximately 35.43 wt%) was detected in chocolate fat of sample No. 18. High oleic acid content was observed for the sn-2 position fatty acid with a range from 64.91% to 86.93%. Trans fatty acid contents in domestic chocolates (sample No. 1~8) and foreign chocolates (sample No. 9~22) were 0.03~0.59 wt% (0.01~0.19 g/100g chocolate) and 0.05~6.32 wt% (0.02~1.99 g/100g chocolate), respectively. In TAG composition, TAGs such as POP/PPO(1,3(2)-palmitoyl-2(3)-oleoyl glycerol, PN=48), POS/PSO(palmitoyl-oleoyl-stearoyl glycerol or palmitoyl-stearoyl-oleoyl glycerol, PN=50), SOS/SSO(1,3(2)-stearoyl-2(3)-oleoyl glycerol, PN=50) were mainly detected in most of the chocolates. The peaks of TAG with low PN (ex, 32-34, 36-38, and 40-42) were detected in No. 18 chocolate fat because of containing short chain fatty acid such as lauric acid.

Evidence for Existence of a Water-Extractable Anticoagulant in an Earthworm, Lumbricus rubellus

  • Woo, Jeong-Im;Bahk, Yun-Kyung;Yu, Kyoung-Hee;Paik, Seung-R.;Chang, Chung-Soon
    • BMB Reports
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    • 제29권6호
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    • pp.500-506
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    • 1996
  • We have isolated a water-extracted novel regulator for blood coagulation from an earthworm, Lumbricus rubellus. As a folk remedy, the earthworm has been known to facilitate blood circulation. After complete heat inactivation of endogenous proteases in the earthworm, an anticoagulant(s) was purified through ammonium sulfate fractionation and three consecutive gel permeation chromatography of Sephacryl S-300, Sephadex G-75, and G-150 by measuring activated partial thromboplastin time (APTT) The anticoagulant was further purified to 2,800 fold with a C4 reversed-phase HPLC This activity was stable under heat ($100^{\circ}C$ for 30 min) and acidic conditions (0.4 N HCl). The effects of this partially purified anticoagulant on thrombin were observed with various substrates such as N${\alpha}$-benzoyl-DL-arginine-p-nitroanilide (BApNA), H-D-phenylalanyl-L-pipecoyl-L-arginine-p-nitroanilide (S-2238), N${\alpha}$-p-tosyl-L-arginine methyl ester (TAME), and fibrinogen as a natural substrate. Only TAME hydrolysis, due to an esterase activity of the enzyme, was inhibited among the chromogenic substrates. In addition, the anticoagulant not only inhibited the conversion of fibrinogen to fibrin but also prolonged the fibrin clot formation monitored with the in vitro coagulation test. Based on these observations, we suggest the significance of measuring the ability of antithrombotic drugs to inhibit the esterase activity of thrombin. In this report, it was also shown that the earthworm indeed contained a water-extractable, heat- and acid-stable anticoagulant which could be used as a novel antithrombotic agent.

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수치에 의한 황금의 성분변화 (Change of Flavonoid Composition in Scutellaria baicalensis by Processing)

  • 김장희;양기숙;김태희
    • 약학회지
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    • 제43권1호
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    • pp.16-22
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    • 1999
  • Scutellaria baicalensis Georgi (Labiatae) has been extensively used in treatment of diarrhea, conjunctivitis, gastritis, enteritis and skin disease. As instructed in old description, the Scutellariae Radix should sometimes be processed before use. To 노디 light on the changes of chemical compositions by processing as well as processing method-activity relationships, Scutellariae Radix was heated at 16$0^{\circ}C$-20$0^{\circ}C$ for 30 min. in furnace or soaked with 20% EtOH (SPE) and boy's urine(SPU), respectively, which are one of processing methods and then heated at 17$0^{\circ}C$ for 30 min. To isolate the chemical components, Scutellariae Radix with/without processing were extracted with EtOH and EtOH extract was fractionated with ether, ethyl acetate and butanol to give respective fractions. Ether and EtOAc fractions obtained from the processed drug with urine (SPU) were subjected to chromatography to obtainsix components, oroxylin A, Wogonin, chrysin, baicalein, baicalein 7-O-$\beta$-D-glucopyranoside and $\beta$-sitosterol 3-O-$\beta$-D-glucopyranoside. All the isolated compounds were identified by means of physicochemical and spectroscopic methods (IR, $^1H-NMR,{\;}^13C-NMR$, Mass). By HPLC determination, the changes of the contents for each isolated components from SPE and SPU samples were observed. It was found that the content of nonglycosidic flavones such as oroxylin A, wogonin, chrysin and baicalein was increased markedly, whereas the content of baicalin and baicalein 7-O-$\beta$-D-glucopyranoside was significantly decreased in both samples as compared with those of Scutellariae Radix. When the sample was soaked with boy's urine, the total amount of nonglycosidic flavones was higher than that of processing with 20% EtOH.

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Evaluating Plant Uptake of Veterinary Antibiotics with Hydroponic Method

  • Park, Saet Byel;Kim, Sun Ju;Kim, Sung Chul
    • 한국토양비료학회지
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    • 제49권3호
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    • pp.242-250
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    • 2016
  • Veterinary antibiotics (VAs) has been used to treat animal disease and to increase animal weight as growth promoter. However, abused usage of VAs can cause production of antibiotic resistance genes (ARGs) in the environment and additionally, residual of VAs in soil can be transferred into crops. Therefore, main objective of this research was to examine bioaccumulation of VAs in sprouts (red cabbage, Brassica Olearacea L. var. Capitata f. rubra and red radish, Raphanus sativus) with hydroponic method. Total of 7 VAs in 2 different classes of VAs (tetracyclcines: tetracycline, oxytetracycline, chlortetracycline, sulfonamides: sulfamethoxazole, sulfamethazine, sulfamethiazole, macrolides: tylosin) were evaluated and experiment was conducted with solid phase extraction (SPE)/high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS). Initial spiked concentration of 7 VAs was $5mg\;L^{-1}$ and cultivation period was 8 days. Result showed that growth of sprouts was inhibited about 23-27% when VAs was introduced. Amount of bioaccumulated VAs was also differed depending on class of VAs. The highest amount of bioaccmulated VAs was tetracycline and sulfamethoxazole in each class with a concentration of 4.05, $7.73mg\;kg^{-1}$ respectively. Calculated transfer ratio of VAs into crops was also ranged 0.38-54.27%. Overall, bioaccumulation of VAs in crops can be varied depending on crop species and class of VAs. However, further research should be conducted to verify bioaccumulation of VAs in crops in the soil environment.

LC/ESI-MS/MS를 이용한 식육(소, 돼지)중 잔류 phoxim 분석 (Analysis of Phoxim Residue in Animal Food Production (Cattle and Pig) by LC/ESI-MS/MS)

  • 박미선;이진주;명승운
    • 대한화학회지
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    • 제55권4호
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    • pp.626-632
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    • 2011
  • 폭심(phoxim)은 널리 사용되고 있는 구충제인 동물용의약품이다. 본 논문에서는 소와 돼지 근육에 잔류하는 폭심을 분석하기 위해서, 실리카 고체상과 아세토니트릴을 사용하여 추출/정제하였다. 분석을 위해서 LC/ESI-MS/MS 방법이 사용되었다. HPLC에서 $C_{18}$ 컬럼($2.1{\times}100\;mm$, $3.5\;{\mu}m$)이 사용되었으며, 이동상으로는 0.1% formic acid와 물이 사용되었다. 소(0.0048~2.0 mg/kg)와 돼지(0.0055~2.0 mg/kg)에 소량첨가하여 얻은 검정곡선은 좋은 직선성($r^2$=0.995)을 나타내었다. 소와 돼지의 매트릭스에 대해서 0.0048~0.2 mg/kg범위에서 68.2~106.9%의 정확도를 나타내었으며, LOD는 0.0014~0.0017 mg/kg, LOQ는 0.0048~0.0055 mg/kg범위에 있었으며, 11.2%의 상대표준편차를 나타내었다.

Liquid Chromatographic Resolution of N-(3,5-Dinitrobenzoyl)-α-amino Acids on a New Chiral Stationary Phase: the First Liquid Chromatographic Utilization of a Double-Ureide Pocket for the Recognition of Chiral Carboxylate Anions

  • Hyun, Myung-Ho;Kim, Seung-Nam;Choi, Hee-Jung;Sakthivel, Pachgounder
    • Bulletin of the Korean Chemical Society
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    • 제28권11호
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    • pp.1980-1984
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    • 2007
  • An HPLC chiral stationary phase (CSP) which has only two ureide functional groups was prepared starting from (1S,2S)-1,2-diaminocyclohexane. The CSP was successful in the resolution of various N-(3,5- dinitrobenzoyl)-α-amino acids, the separation (α) and the resolution factors (RS) being within the range of 1.11-1.35 and 2.19-5.17, respectively with the use of 20% 2-propanol in hexane containing 0.1% trifluoroacetic acid as a mobile phase. However, ethyl esters of N-(3,5-dinitrobenzoyl)-α-amino acids were not resolved or resolved with only marginal separation and resolution factors on the CSP under the identical mobile phase condition. From these results, the complexation of the carboxylate anions of analytes inside the double-ureide pocket of the CSP was expected to play some important role for the chiral recognition. In contrast, N-(3,5- dinitrobenzoyl)-α-amino acid N-propylamides were resolved on the CSP with reasonable separation and resolution factors. Enantioselective hydrogen bonding interactions between analytes and the CSP were presumed to be responsible for these resolutions.

High Performance Liquid Chromatographic Analysis of a New Proton Pump Inhibitor KR60436 and Its Active Metabolite O-Demethyl-KR60436 in Rat Plasma Samples Using Column-Switching

  • Lee, Hyun-Mee;Lee, Hee-Yong;Choi, Joong-Kwon;Lee, Hye-Suk
    • Archives of Pharmacal Research
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    • 제24권3호
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    • pp.207-210
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    • 2001
  • A fully automated high performance liquid chromatography with column-switching was developed for the simultaneous determination of KR60436, a new reversible proton pump inhibitor, and its active metabolite O-Demethyl-KR60436 from rat plasma samples. Plasma sample (50$\mu$l) was directly introduced onto a Capcell Pak MF Ph-1 column ($10{\times}4$ mm I.D.) where primary separation was occurred to remove proteins and concentrate target Substances Using acetonitrile-Potassium Phosphate (PH 7, 0.1 M) (2 : 8, v/v). The drug molecules eluted from MF Ph-1 column were focused in an intermediate column ($10{\times}2$ I.D.) by the valve switching step. The substances enriched in intermediate column were eluted and separated on a Vydac 218MR53 column ($250{\times}3.2$ I.D.) using acetonitrilepotassium phosphate (pH 7, 0.02 M) (47:53, v/v) at a flow rate of 0.5 ml/min when the valve status was switched back to A position. The method showed excellent sensitivity (detection limit of 2 ng/ml) with small volume of samples ($50{\mu}$l), good precision and accuracy, and speed (total analysis time 24 min) without any loss in chromatographic efficiency. The response was linear ($r^2{\geq}0.797$) over the concentration range of 5-500 ng/ml.

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Ginkgo Terpene의 Candidate albicans로 인한 관절염에 대한 치료효과 (Therapeutic Anti-inflammatory Effect of Ginkgo Terpene on Arthritis due to Candida albicans)

  • 이순현;이주희;한용문
    • 약학회지
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    • 제49권2호
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    • pp.140-146
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    • 2005
  • Candida albicans, a polymorphic fungus, causes systemic and local infections. Recent reports show that the fungus is a main etiological agent for the arthritis. For trea tment, antifungal drugs and/or rheumatoid drugs are used, but resistance and side effects limit application of the drugs. In search of new sources for treatment of the fungal arthritis, we choose Egb 761 (extract of Ginkgo leaves 761), one of the most popular over-the-counter herbal medicines. The Egb 761 contains two major ingredients such as terpene and flavonoid. In the present study, we examined if the terpene portion of Egb 761 had anti-inflammatory activity against C.albicans-caused arthritis. The terpene was extracted with combination of methanol and water from the Egb 761, followed by gel-permeation chromatography. Presence of terpene was determined by the Salkowski colorimetric method and HPLC analysis. For an animal model of inflammation induction, mice were given an emulsion form of C.albicans cell wall mixed with Complete Freund's Adjuvant (CFA) by footpad-injection. Results showed that intraperitoneal administration of the water-soluble portion that contained terpene and flavonoid reduced the inflammation. Whereas the terpene had anti-inflammatory activity, flavonoid portion had no such activity, For determination of possible mechanism of the activity, the terpene seemed to be suppression of nitric oxide (NO) production from LPS-treated macrophages. Taken together the Ginkgo terpene may have anti-inflammatory effect against C.albicans-caused arthritis, possibly by blocking NO production.

Anthocyanins in 'Cabernet Gernischet' (Vitis vinifera L. cv.) Aged Red Wine and Their Color in Aqueous Solution Analyzed by Partial Least Square Regression

  • Han, Fu-Liang;Jiang, Shou-Mei;He, Jian-Jun;Pan, Qiu-Hong;Duan, Chang-Qing;Zhang, Ming-Xia
    • Food Science and Biotechnology
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    • 제18권3호
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    • pp.724-731
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    • 2009
  • Anthocyanins are considered one of the main color determinants in aged red wine. The anthocyanins in aged red wine made from 'Cabernet Gernischet' (Vitis vinifera L. cv.) grape were investigated by high performance liquid chromatography- electronic spray ionization- mass spectrometry (HPLC-ESI-MS) and their color presented in aqueous solution were evaluated using partial least square regression (PLS). The results showed that there were 37 anthocyanins identified in this wine, including 22 pyranoanthocyanins. The analysis of PLS indicated that different anthocyanins showed distinct color values: malvidin 3-O-(6-O-acetyl)-glucoside-4-vinylguaiacol (Mv3-acet-glu-vg) presented the highest color values, while malvidin 3-O-glucoside (Mv3-glu) showed least. Among the free non-acylated anthocyanins, peonidin 3-O-oglucoside (Pn3-glu) showed the highest color values; the coumarylated anthocyanins presented higher color values than their corresponding acetylated anthocyanins and parent anthocyanins; pyranoanthocyanins presented also higher color values than their original anthocyanins; the color of anthocyanins depended on their structure. This work will be helpful to reveal evolution in aged red wine.