• Title/Summary/Keyword: prep-HPLC

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Identification of Volatile Essential Oil, and Flavor Characterization and Antibacterial Effect of Fractions from Houttuynia cordata Thunb -II. Flavor Characterization and Antibacterial Effect of Fraction from Houttuynia cordata Thunb by Prep-HPLC- (어성초 휘발성 정유성분의 동정과 분획물의 향특성 및 항균활성 -II. Prep-HPLC에 의한 분획물의 향특성과 향균활성-)

  • Kang, Jung-Mi;Cha, In-Ho;Lee, Young-Kuen;Ryu, Hong-Soo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.26 no.2
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    • pp.214-221
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    • 1997
  • The volatile essential oil isolated from Houttuynia cordata were separated to 11 fractions by Prep-HPLC, of these, a fraction(Fr. 6) which carried the characteristic Houttuynia cordata flavor(fishy) contained 2-undecanone, ${\beta}-myrcene$, ${\beta}-ocimene$, 1-decanol and decanoyl acetaldehyde, as identified by GC-MS. From this observation, it may be inferred that 2-undecanone and decanoyl acetaldehyde could be the compounds which play a crucial role in flavoring of Houttuynia cordata. In test of antibacterial activity of eleven fractions of volatile essential oil from H.C., the growths of nine Gram negative bacteria were inhibited obviously when treated with and Fr. 6 including 2-undecanone, ${\beta}-myrcene$, ${\beta}-ocimene$, 1-decanol and decanoyl acetaldehyde, and Fr. 5 including decanal, endobornylacetate, fenchene and decanoic acid, respectively.

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Large Scale Purification of KRF-001 on the Preparative HPLC (Preparative HPLC를 이용한 KRF-001의 대량분리정제)

  • 이항우;김무경정태숙복성해
    • KSBB Journal
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    • v.9 no.4
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    • pp.385-394
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    • 1994
  • Large scale purification to get antifungal antibiotic KRF-001 of 90% purity, was investigated using preparative HPLC. Crude KRF-001 was purified by XAD-7 adsorption chromatography, acid precipitation and microfiltration. Microfiltration was the most effective isolation method of crude KRF-001. The purification methods using C18 chromatography was convenient compared with the conventional methods. Delta PAK C18 column and Bonda PAK C18 column were adapted large scale purification of KRF-001. Gradient system of prep HPLC using Delta PAK C18 column was more effective. With these conditions, final recovery of KRF-001 yielded 77%.

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Isolation of Herbicidal Compounds from Pulsatilla koreana Roots (백두옹(Pulsatilia koreana Nakai) 뿌리로부터 제초활성물질의 분리)

  • 정형진
    • Korean Journal of Plant Resources
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    • v.9 no.1
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    • pp.47-54
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    • 1996
  • To search herbicidal compounds in Pulsatilla koreana Nakai, methanol extract of P. koreana roots was purified by sequences of XAD-7 column chromatography, silica gel adsorption column chromatography, silica gel flash column chromatography, preparative layer chromatography and preparative high performance liquid chromatography(Prep, HPLC).The final Prep. HPLC gave two herbicidally-active fractions. These fractions treatment at 100ppm inhibited the root length of Echinochloa crus-galli seedlings by 48% and 60% as compared with the control, respectively. Components in the two active fractions were analyzed by GC-MS Spectrometry. These compounds, which were isolated from P. koreana roots, were identified as several fatty esters, hydrocarbons, squalene, evidonol, and a diazepin analogue.

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New Efficient Method for Isolation and Purification of Ginsenosides (Ginsenoside의 새로운 분리.정제 방법)

  • 김세원;황석연
    • Journal of Ginseng Research
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    • v.22 no.4
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    • pp.284-288
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    • 1998
  • This study was carried out to establish a new efficient method for isolation and purification of ginsenosides. Silica gel column chromatography, having been used for the isolation of ginsenosides, is advantageous to obtain a large amount of ginsenosides. However, it has a disadvantage to isolate ginsenosides to their highest purity. In addition, normal-or reverse-phase HPLC method thus far reported is confined to quantitative analysis. Especially, it has not been possible to isolate racemic 20(S)- and 20(R)-ginsenoside Rg2. In this experiment, isolation and purification of ginsenosides were accomplished by Diaion HP-20 adsorption chromatography, silica gel column chromatography, recrystalization and Prep. HPLC with or without Prep. TLC. From this study, we could establish a new efficient method for isolation and purification of 9 major and/or minor ginsenosides.

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The stability comparison of purified bee venom and bee venom melittin in aqueous solution (수용액에서 정제봉독 (PBV)과 봉독멜리틴 (BVM)의 안정성 비교)

  • Park, Jung Keun;Shen, Chang Zhe;Kim, Choul Goo;Kim, Il Kwang
    • Analytical Science and Technology
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    • v.29 no.4
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    • pp.194-201
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    • 2016
  • The stability comparison tests on purified bee venom (PBV) and bee venom melittin (BVM) in different conditions of temperature, solvent, and concentration were studied. High purity BVM (98.2 %) was separated from PBV by prep-HPLC (column, C4) and used to stability tests in aqueous phase. The stability of the PBV has been increased in the saline solution, while BVM was reduced. In distilled water, the stability of PBV has been reduced, while BVM showed an increasing result. As a result, the appropriate conditions for maintaining the long term stability of BVM were found to be the low temperature (4 ℃), distilled water, and concentration (1.0 mg/mL).

NEAR INFRARED TRANSFLECTANCE SPECTROSCOPY (NIRS) IN PHYTOCHEMISTRY

  • Huck, C.W.;W.Guggenbichler;Bonn, G.K.
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.3114-3114
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    • 2001
  • During the last years phytochemistry and phytopharmaceutical applications have developed rapidly and so there exists a high demand for faster and more efficient analysis techniques. Therefore we have established a near infrared transflectance spectroscopy (NIRS) method that allows a qualitative and quantitative determination of new polyphenolic pharmacological active leading compounds within a few seconds. As the NIR spectrometer has to be calibrated the compound of interest has at first to be characterized by using one or other a combination of chromatographic or electrophoretic separation techniques such as thin layer chromatography (TLC), high performance liquid chromatography (HPLC), capillary electrophoresis (CE), gas chromatography (GC) and capillary electrochromatography (CEC). Both structural elucidation and quantitative analysis of the phenolic compound is possible by direct coupling of the mentioned separation methods with a mass spectrometer (GC-MS, LC-MS/MS, CE-MS, CEC-MS) and a NMR spectrometer (LC-NMR). Furthermore the compound has to be isolated (NPLC, MPLC, prep. TLC, prep. HPLC) and its structure elucidated by spectroscopic techniques (UV, IR, HR-MS, NMR) and chemical synthesis. After that HPLC can be used to provide the reference data for the calibration step of the near infrared spectrometer. The NIRS calibration step is time consuming, which is compensated by short analysis times. After validation of the established NIRS method it is possible to determine the polyphenolic compound within seconds which allows to raise the efficiency in quality control and to reduce costs especially in the phytopharmaceutical industry.

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Fractionation of Angiotensin Converting Enzyme(ACE) Inhibitory Peptides from Soybean Paste (된장으로부터 Angiotensin Converting Enzyme(ACE) 저해 Peptide의 분획)

  • Shin, Zae-Ik;Ahn, Chang-Won;Nam, Hee-Sop;Lee, Hyung-Jae;Lee, Hyung-Joo;Moon, Tae-Hwa
    • Korean Journal of Food Science and Technology
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    • v.27 no.2
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    • pp.230-234
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    • 1995
  • Angiotensin converting enzyme(ACE) inhibitory peptides lowering blood pressure were fractionated from a commercial soybean paste(Doenjang). When the freeze-dried sample of soybean paste was extracted with cold water, the recovery yield of total nitrogen(TN) was shown to be 73.3% in 30 minutes. The cold water extract was filtered through PM-10 membrane(Amicon) for 3 hours in order to remove high molecular weight polypeptides. The TN and salt of ultrafiltrate were recovered to 80.8% and 99.2%, respectively, and its ACE $IC_{50}$ was $41.8{\mu}g/ml$. When the ultrafiltrate was divided into 7 fractions by reverse phase prep-HPLC, F5 fraction showed the highest ACE inhibitory activity ($IC_{50}=6.8{\mu}g/ml$) and salt could be collected into F1 fraction. Subsequently, the F5 fraction was divided into another five fractions by ion exchange prep-HPLC, all of which appeared to be high ACE inhibitory activity($IC_{50}=2.5{\sim}8.3{\mu}g/ml$). Among them, F53 fraction had the highest ACE inhibitory activity, and its main amino acid component was found to be histidine.

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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
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    • v.23 no.4
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    • pp.390-396
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    • 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.

Isolation of Ginsenoside Rh1 and Compound K from Fermented Ginseng and Efficacy Assessment on Systemic Anaphylactic Shock

  • Kim, Mi-Soon;Kwon, Bin;Park, Myeong-Soo;Ji, Geun-Eog
    • Food Science and Biotechnology
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    • v.17 no.4
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    • pp.805-808
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    • 2008
  • Ginsenosides are responsible for the pharmacological and biological activities of ginseng. In this study, ginsenoside Rh1 and compound K were isolated and purified from fermented ginseng substrate and their anti-allergic effects were assessed in compound 48/80-induced anaphylactic shock model. The fermented ginseng substrate was extracted by methanol and ginsenoside Rh1 and compound K were efficiently purified by preparative high performance liquid chromatography (prep HPLC). Their quality and quantity were analyzed by liquid chromatography-mass spectrometer (LC-MS) and HPLC. Ginsenoside Rh1 showed better anti-allergic effects than compound K in compound 48/80-induced anaphylactic shock model. This study suggested that fermented ginseng extracts with enriched Rh1 may be utilized as a potential biomaterial of functional food for the alleviation of allergic symptoms.

Bioactivity of an Extract of Lespedezea Cuneata G. Don to Rabbit Corpus Cavernosum Smooth Muscle Tone (야관문(Lespedezea cuneata G. Don) 추출물이 토끼 음경해면체 평활근에 미치는 생리활성)

  • Chung, Young-Ho;Lim, Chi-Hwan
    • Korean Journal of Agricultural Science
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    • v.32 no.1
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    • pp.63-70
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    • 2005
  • The extracts in n-hexane layer from Lespedezea cuneata G. Don exelled at sexual activity according to in vitro experiment using biopsy of rabbit corpus cavernosum to investigate effects on sexual function. The extracts were injected into 9 samples at $10{\mu}l$. The lowest relaxation was showed at sample C, $4.8{\pm}1.4%$ and the highest relaxation was showed at sample A, $20.2{\pm}6.0%$. The relaxation by every sample, except sample C and G-1, were higher than by $10^{-7}M$ ACh, $7.8{\pm}5.1%$, and their effects were above 10%. Also, the extracts were injected into 9 samples at $15{\mu}l$. The lowest relaxation was showed at sample C, $15.4{\pm}9.7%$ and the highest relaxation was showed at sample J, $54.8{\pm}9.7%$. The relaxation by sample A and D was as much as by $10^{-6}M$ ACh, $28.0{\pm}20.1%$. The relaxation by sample H was $41.9{\pm}7.3%$. The relaxation by sample J was $54.8{\pm}9.7%$ and it was higher than by $10^{-5}M$ ACh, $53.9{\pm}25.9%$. Also, the extracts were injected into 9 samples at $20{\mu}l$. The lowest relaxation was showed at sample E, $28.9{\pm}0.6%$ and it was a little higher than by $10^{-6}M$ ACh. The relaxation by sample G was as much as by $10^{-5}M$ ACh. The two higher relaxation were showed at sample H, $99.4{\pm}16.0%$ and J, $95.7{\pm}7.2%$, and their relaxation against contraction reaction by PhE were near 100%. Experiment by sample I was not performed for lack of sample amount.

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