• 제목/요약/키워드: High-Performance Liquid Chromatography

검색결과 2,124건 처리시간 0.029초

HPLC를 이용한 생체 시료중의 새로운 플라보노이드 유도체인 DA-6034의 분석 (Analysis of DA-6034, a New Flavonoid Derivative in Biological Fluids by HPLC)

  • 이종진;손미원;유무희;장민선;김원배;이강춘
    • 약학회지
    • /
    • 제42권2호
    • /
    • pp.149-152
    • /
    • 1998
  • A high performance liquid chromatographic method was developed for the determination of DA-6034 in biological fluids using internal standard. Plasma containing DA-6034 and inter nal standard was extracted by liquid-liquid extraction at an acidic pH. After evaporation of the organic layer, the drug and internal standard were reconstituted with mobile phase and injected into the column. They were separated by high performance liquid chromatography on inertsil ODS II column at 334 nm. The detection limit of DA-6034 in plasma was 0.02 ${\mu}$g/ml. In this method, the range of recovery and coefficients of variation were 96-110% and 0.40-3.78%, respectively. There was no interference from endogenous substances. Urine and bile were analysed using the deproteinization method and the detection limit of DA-6034 was 1${\mu}$g/l.

  • PDF

High performance liquid chromatography에 의한 fructo 및 inulo올리고당의 정량 (Quantitation of fructo- and inulo-oligosaccharides by high performance liquid chromatography)

  • 강수일;한종인;김경연;오선진;김수일
    • Applied Biological Chemistry
    • /
    • 제36권4호
    • /
    • pp.310-314
    • /
    • 1993
  • HPLC를 이용하여 fructose oligomer인 fructo올리고당(GF2-GF7) 및 inulo올리고당(F2-F4)의 분리, 정량을 실시하였다. TSK-gel amide 80 column과 acetonitrile-water(65:35; v/v) 용매를 사용하여 각 표준당들을 효과적으로 분리할 수 있었으며 이들의 retention time은 분석시마다 거의 변하지않아 재현성이 있었다. 각 당의 농도에 따른 peak면적을 이용하여 표준곡선을 작성한 결과 넓은 당량의 범위에 걸쳐 결정계수가 0.9884이상의 값을 보여 본 HPLC방법에 의한 정량법이 타당한 것으로 나타났다. 또한 기울기는 비슷하나 y축 절편 값이 당마다 크게 상이하여 몇가지 표준당들을 기준으로 하여 모든 당을 일률적으로 정량하는 것은 적합하지 않으며 각 당에 대한 표준곡선을 하나씩 작성하여 정량하여야함을 알 수 있었다.

  • PDF

Transformation of dissolved organic matter in a constructed wetland: A molecular-level composition analysis using pyrolysis-gas chromatography mass spectrometry

  • Park, Jongkwan;Choi, Mijin;Cho, Jaeweon;Chon, Kyongmi
    • Environmental Engineering Research
    • /
    • 제23권4호
    • /
    • pp.390-396
    • /
    • 2018
  • This study investigated the transformation of dissolved organic matter (DOM) in a free-water surface flow constructed wetland. Pyrolysis gas chromatography-mass spectrometry (Py-GC/MS) coupled with preparative high-performance liquid chromatography (prep-HPLC) was used to analyze the compositions of biopolymers (polysaccharides, amino sugars, proteins, polyhydroxy aromatics, lipids and lignin) in DOM according to the molecular size at three sampling points of the water flow: inflow, midflow, and outflow. The prep-HPLC results verified the decomposition of DOM through the decrease in the number of peaks from three to one in the chromatograms of the sampling points. The Py-GC/MS results for the degradable peaks indicated that biopolymers relating to polysaccharides and proteins gradually biodegraded with the water flow. On the other hand, the recalcitrant organic fraction (the remaining peak) in the outflow showed a relatively high concentration of aromatic compounds. Therefore, the ecological processes in the constructed wetland caused DOM to become more aromatic and homogeneous. This indicated that the constructed wetland can be an effective buffer area for releasing biochemically stable DOM, which has less influence on biological water quality indicators, e.g., biochemical oxygen demand, into an aquatic ecosystem.

High Performance Liquid Chromatography를 이용한 국내 시판 사과 주스의 Patulin 분석 (Determination of Patulin in Commercial Apple Juice in Korea by High Performance Liquid Chromatography)

  • 조완일;최영붕;문태화
    • 한국식품과학회지
    • /
    • 제29권3호
    • /
    • pp.412-416
    • /
    • 1997
  • 7개의 국내 시판 사과 주스제품에 대해 patulin 오염수준을 분석하였다. Sep-Pak silica cartridge를 이용한 ethyl acetate 추출물의 정제과정은 HPLC 분석시 추출물내의 다른 성분으로부터 patulin의 분리를 용이하게 하였다. Patulin 검출은 J'sphere $4\;{\mu}m$ ODS-H80 column을 사용하여 reverse phase HPLC로 274 nm에서 분석하였다. 분석결과 4개의 제품은 $4{\sim}20\;{\mu}g/L$ 수준으로, 나머지 3개 제품은 $30{\sim}45\;{\mu}g/L$ 수준으로 patulin에 오염되어 있었다. 이 분석방법에서의 검출 한계농도는 $3\;{\mu}g/L$이며 $3.78{\sim}125.9\;{\mu}g/L$ 오염수준에 대해 $80{\sim}90%$의 회수율을 보였다.

  • PDF

Separation and Purification of Lipase Inhibitory Peptide from Fermented Milk by Lactobacillus plantarum Q180

  • Kim, Seulki;Lim, Sang-Dong
    • 한국축산식품학회지
    • /
    • 제40권1호
    • /
    • pp.87-95
    • /
    • 2020
  • In this study, we separated and purified lipase inhibitory peptide from fermented milk by Lactobacillus plantarum Q180 with the aim of developing a new functional anti-lipase activity yogurt product. L. plantarum 180 was inoculated into 10% reconstituted skimmed milk and incubated at 37℃ until the pH of the culture reached pH 4.4. The lipase activity was measured using porcine pancreatic lipase. The lipase inhibitory peptides were gradually isolated by ultrafiltration, reversed phase column chromatography (RPC), reversed phase high-performance liquid chromatography (RP-HPLC), and gel permeation high-performance liquid chromatography (GP-HPLC) from the fermented milk by L. plantarum Q180. An ODS-AQ column was used for the RPC, a Vydac C18 column for the RP-HPLC, and a Superdex Peptide HR column for the GP-HPLC. The peptide was composed of Asp, Thr, Ile, Ser, Ala, and Gln, and the anti-lipase activity (IC50) was 2,817 ㎍/mL.

고속액체크로마토그라피에 의한 은행잎중 Flavonoid Glycoside의 확인 및 정량 (Identification and Quantitative Analysis of Flavonol Glycosides from Ginkgo biloba Leaves by High Performance Liquid Chromatography)

  • 강삼식;김주선;곽의종;김기협
    • 생약학회지
    • /
    • 제21권2호
    • /
    • pp.148-152
    • /
    • 1990
  • Seven flavonol glycosides from the EtOAc fraction of Ginkgo biloba leaves were identified by high performance liquid chromatography. Separation by reversed phase chromatography on $Lichrosorb^{\circledR}$ RP-18 column was achieved by isocratic elution. The content of the major acylated flavonol glycoside, kaempferol 3-0-[$6'-O-{p}-coumaroyl-{\beta}-_D-glucosyl(1{\rightarrow}2)-{\alpha}-_L-rhamnoside$] was about 8.0% and 0.55% for EtOAc fraction and MeOH extract, respectively.

  • PDF

Klebsiella pneumoniae 균주의 세포외막으로부터 2-Furaldehyde Dehydrogenase의 부분정제에 관하여 (Partial Purification of the Outer Membrane-Associated 2-Furaldehyde Dehydrogenase from Klebsiella pneumoniae)

  • 이준우;이병웅;강사욱;하영칠;유병설;한홍의
    • 미생물학회지
    • /
    • 제24권4호
    • /
    • pp.370-376
    • /
    • 1986
  • From the outer membrane portion of Gram-negative Klebsiella pneumoniae, the activity of 2-furaldehyde dehydrogenase depending upon beta-nicotinamide adenine dinucleotide was detected. Cytoplasmic membrane was preferentially extracted from crude membrane with $Mg^{2+}$ and Triton X-100, and then outer membrane was collected by ultracentrifugation. The crude enzyme was obtained by solubilization of outer membrane with lysozyme, ethylene diamine tetraacetate and Triton X-100. Thereafter 2-furaldehyde dehydrogenase was partially purified through column chromatography on QAE-Sephadex Q-50 and Sephadex G-150 and the enzyme activity was analyzed by means of high performance liquid chromatography. The optimal pH for the activity of the enzyme was about 9.5 and the optimal temperature was about $85^{\circ}C$. The partially purified enzyme retained tis activity at $85^{\circ}C$ for 5 hours. The optimal concentration of Triton X-100 for the activity of the enzyme was about 1.5% in the reaction mixture.

  • PDF

Identification of Actinomycins by High Performance Liquid Chromatography and Fast Atom Bombardment Mass Spectrometry

  • Cho, Seong-Eun;Goo, Yang-Mo;Kim, Kyoung-Ja
    • Archives of Pharmacal Research
    • /
    • 제17권6호
    • /
    • pp.424-427
    • /
    • 1994
  • An acinomycin complex isolated from culture broth of a soil microorganism, SNUS 9305-011 has been examined by High performance liquid chromatography (HPLC). From the analysis of the fractions obtained by column chromatography of the ethyl acetate extract, three actinomycin components are confimed . The HPLC analysis is carried out with a CN-bonded nucleosil column. Comparison of the retention times of the components with those of actinomycin D, C complex, $X_{o{\beta}$, and V and suggests that they are different actinomycins. FBA mass spectra fo the coponents also shows different molecular ions from those of standards and other reported actionbmycins. The present work has demonstrated that actinomycin components can be separated by a CN-bonded HPLC column, and that ocmparison of their HPLC chormatograms with authentic smaples and information on their molecular ions can be successfully employed for indentification of actionmycins.

  • PDF

Determination of Fluorescent Whitening Agents in Paper Materials by Ion-Pair Reversed-Phase High-Performance Liquid Chromatography

  • Kim, Jeong Soo;Kim, Do Hwan;Kim, Keon
    • Bulletin of the Korean Chemical Society
    • /
    • 제33권12호
    • /
    • pp.3971-3976
    • /
    • 2012
  • A simple method was developed for the analysis of seven stilbene-type fluorescent whitening agents (FWAs) in paper materials by ion-pair reversed-phase high-performance liquid chromatography with fluorescence detection. These stilbene-type FWAs included two disulfonate, two tetrasulfonate, and three hexasulfonate compounds. After optimization of chromatographic conditions, the FWAs were satisfactorily separated using a reversed-phase column (RP-18) with the following isocratic mobile phase: methanol-water (60:40) containing 17.5 mM TBABr and 10 mM citrate buffer (pH = 7.0). The calibration plot was linear in the range from 5 to 500 ng/mL for two disulfo-FWAs and from 1 to 500 ng/mL for the other five FWAs. Precision levels of the calibration curve as indicated by RSD of response factors were 1.2 and 8.1%. Limits of quantitation (LOQ) ranged from 1.2 to 11 ng/mL.

Identification of Dammarane-type Triterpenoid Saponins from the Root of Panax ginseng

  • Lee, Dong Gu;Lee, Jaemin;Yang, Sanghoon;Kim, Kyung-Tack;Lee, Sanghyun
    • Natural Product Sciences
    • /
    • 제21권2호
    • /
    • pp.111-121
    • /
    • 2015
  • The root of Panax ginseng, is a Korea traditional medicine, which is used in both raw and processed forms due to their different pharmacological activities. As part of a continued chemical investigation of ginseng, the focus of this research is on the isolation and identification of compounds from Panax ginseng root by open column chromatography, medium pressure liquid chromatography, semi-preparative-high performance liquid chromatography, Fast atom bombardment mass spectrometric, and nuclear magnetic resonance. Dammarane-type triterpenoid saponins were isolated from Panax ginseng root by open column chromatography, medium pressure liquid chromatography, and semi-preparative-high performance liquid chromatography. Their structures were identified as protopanaxadiol ginsenosides [gypenoside-V (1), ginsenosides-Rb1 (2), -Rb2 (3), -Rb3 (4), -Rc (5), and -Rd (6)], protopanaxatriol ginsenosides [20(S)-notoginsenoside-R2 (7), notoginsenoside-Rt (8), 20(S)-O-glucoginsenoside-Rf (9), 6-O-[$\alpha$-L-rhamnopyranosyl(1$\rightarrow$2-$\beta$-D-glucopyranosyl]-20-O-$\beta$-D-glucopyranosyl-$3\beta$,$12\beta$, 20(S)-dihydroxy-dammar-25-en-24-one (10), majoroside-F6 (11), pseudoginsenoside-Rt3 (12), ginsenosides-Re (13), -Re5 (14), -Rf (15), -Rg1 (16), -Rg2 (17), and -Rh1 (18), and vinaginsenoside-R15 (19)], and oleanene ginsenosides [calenduloside-B (20) and ginsenoside-Ro (21)] through the interpretation of spectroscopic analysis. The configuration of the sugar linkages in each saponin was established on the basic of chemical and spectroscopic data. Among them, compounds 1, 8, 10, 11, 12, 19, and 20 were isolated for the first time from P. ginseng root.