• Title/Summary/Keyword: High performance Liquid Chromatography

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A Study on the Elution Behavior of some Metal-N-Alkylisonitrosoacetylacetone imine Chelates by Reversed Phase High Performance Liquid Chromatography (역상 액체 크로마토그래피에 의한 몇 가지 금속-N-Alkylisonitrosoacetylacetone imine 킬레이트의 용리거동에 관한 연구)

  • Kim, Yong Jun;Kewon, Ji Hae;Lee, Won
    • Analytical Science and Technology
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    • v.5 no.1
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    • pp.63-71
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    • 1992
  • Liquid chromatographic behavior of Pd(II), Ni(II) and Co(III) in N-Alkylisonitrosoacetylacetone imine(HIAA-NR) chelates was investigated by reversed phase high perfomance liquid chromatography. The optimum conditions for the separation of IAA-NR-metal chelates were examined respect to the flow rate and mobile phase strength. The metal-N-Alkylisonitrosoacetylacetone imine chelates in solution were successfully separated on Novapak $C_{18}$ column using acetonitrile/water mixture as mobile phase. The elution order of chelates is methyl>ethyl>propyl>butyl as N-alkyl group for ligand is varied. It was found that all IAA-NR-metal chelates were eluted in an acceptable range of capacity factor value($0{\leq}log\;k^{\prime}{\leq}1$). The dependence of log k' on the volume fraction of water in the binary mobile phase was examined. Also, the dependence of k' on the liquid-liquid extraction distribution ratio(Dc) in acetonitrile-water-alkane extraction system was investigated for IAA-NR-metal chelate. Both kinds of dependence are linear, which suggests that the retention of the electroneutral metal chelates on Novapak $C_{18}$ column is largely due to the hydrophobic effect.

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Phytoecdysones from the Roots of Achyranthes japonica Nakai and their Anti-atopy Activity (우슬의 뿌리로부터 Phytoecdysones의 분리와 항 아토피 효과)

  • Kim, Ki Ohk;Ku, Chang-Sub;Kim, Min-Jin;Park, Yhun Jung;Ryu, Hyung Won;Song, Hyuk-Hwan;Kim, Jung Hee;Oh, Sei-Ryang
    • Journal of Applied Biological Chemistry
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    • v.58 no.1
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    • pp.13-19
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    • 2015
  • The roots of Achyranthes japonica Nakai were extracted with 100% aqueous and concentrated subfraction was separated with ultra-performance liquid chromatography-based activity profiling. Three compounds were isolated from the subfraction 5 through the repeated prep- high performance liquid chromatography column chromatography. According to the results of physico-chemical and spectroscopic data including NMR and MS, the chemical structures of the compounds were determined as ecdysterone (1), 25S-inokosterone (2), and 25R-inokosterone (3). Three phytoecdysones were showed weak inhibitory activity for thymus and activation-regulated chemokine expression levels in tumor necrosis factor (TNF)-${\alpha}$ plus IFN-${\gamma}$ induced HaCaT cells, respectively. However, those compounds 1-3 were exhibited the most potent inhibition (80-95% at $200{\mu}g/mL$) against TNF-${\alpha}$ expression levels in A23187 plus phorbol-myrisrate acetate-induced RBL-2H3 cells. As result, 100% aqueous extract of A. japonica has an excellent anti-atopy activity. It could be used to a large range of functional anti-atopy cosmetics.

Development of high performance liquid chromatography assay method of diosmin capsules (디오스민 캡슐의 HPLC 분석법의 개발)

  • Shim, Dae Hyun;Shin, Dong Han;Truong, Quoc Ky;Mai, Xuan Lan;Kang, Jong-Seong;Woo, Mi Hee;Na, Dong-Hee;Chun, In-Koo;Kim, Kyeong Ho
    • Analytical Science and Technology
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    • v.29 no.6
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    • pp.277-282
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    • 2016
  • British Pharmacopoeia (BP 2013), the United States Pharmacopoeia (USP 39) and the Korean Pharmacopoeia (KP XI) contain monographs for the quality control of raw diosmin using high performance liquid chromatography (HPLC). However, official monographs detailing pharmaceutical formulations for diosmin are not available in foreign pharmacopoeias. In the KP XI, ultraviolet-visible (UV-Vis) spectroscopy-which is less specific than HPLC-is reported for the testing of diosmin capsules. In this study, we present an alternative HPLC assay for such testing that is more specific than UV-Vis methods. Method validation was performed to determine linearity, precision, accuracy, system suitability, and robustness. The linearity of calibration curves in the desired concentration range was high ($r^2$>0.999), while the RSDs for intra- and inter-day precision were 0.15-0.29 % and 1.05-1.74%, respectively. Accuracies ranged from 101.2-103.2 %, while the retention time and peak area RSDs were 0.37 % and 0.06 %, respectively. Additionally, the plate number and asymmetry factor values for diosmin were 3591.293 and 1.35, respectively. Since the intermediate-precision and robustness of the assay were satisfactory, this method will be a valuable addition to the Korean Pharmacopoeia (KP XI).

Biosynthesis of $17\alpha-hydroxy$, $20\alpha-dihydroprogesterone$ by Ovaries of the Spotted Flounder (Verasper variegatus)

  • Baek Hea-Ja
    • Fisheries and Aquatic Sciences
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    • v.4 no.2
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    • pp.70-74
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    • 2001
  • To examine the production of steroids with potential oocyte maturation-inducing activity in the spotted flounder, Verasper variegatus, we have incubated post-vitellogenic oocytes (0.82­0.95mm in diameters) with radiolabeled pregnenolone and $17\alpha-hydroxyprogesterone$. The resulting metabolites were analyzed by thin layer chromatography (TLC) and high performance liquid chromatography (HPLC). The two main metabolites (progestogens) found in both incubations co-migrated with $17\alpha-hydroxy$, $20\alpha-dihydroprogesterone$ $(17\alpha, 20\alpha OHP)$ and $17\alpha-hydroxy,\;$20\beta-dihydroprogesterone$ (17 a20{30HP). Additional chromatography by HPLC and TLC confirmed the presence of radioactive $17\alpha, 20\alpha OHP$ and a large amount of unknown metabolite. The present study did not reveal in vitro formation of $l7\alpha 20\beta OHP$. Although 1$l7\alpha 20\beta OHP$ was found in a small amount, the synthesis of this steroid suggests that it may play a role in regulating the oocyte maturation process in the spotted flounder.

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Identification of Antimutagenic Compound from Kale by High Performance liquid Chromatography and Mass Spectrometry

  • Lee, Seon-Mi;Rhee, Sook -Hee;Yoo, Jong-Shin;Park, Kun-Young
    • Preventive Nutrition and Food Science
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    • v.3 no.4
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    • pp.334-338
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    • 1998
  • Kale(Brassica oleracea var. acephala) is one of Cruciferous vegetables that is closely related to the wild ancestral form of cabbabe. The ethanol extract of kale which contains the active compoundsss under Salmonella assay system was fractionated with chloroform to collect the nonpolar solvent soluble compounds, and then further fractionation was carried out by silica gel column chromatography. Among kale extracts separated by silical gel column chromatography, the fractions of 4, 5 and 6 exhibited strong antimutagenic activities. The major active compounds from the fraction were identified as chlorophyll derivatives by the analysis with HPLC-fritp-MS. The molecular weights of each chlorophyll derivatives in the sample were acquired from the peaks of positive ion atomosphere pressure chemical ionization (APCI) mas spectrometry.

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Separation and identification of selenoproteins in selenium-enriched yeast (셀레늄이 강화된 이스트에서 셀레늄 단백질의 분리 및 확인)

  • Kim, Kyong-Mi;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.26 no.6
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    • pp.357-363
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    • 2013
  • Selenium-containing proteins were separated from selenium-enriched yeast (SEY) using Trizol$^{(R)}$ reagent followed by anion exchange (AE) chromatography. This method is simpler and less time consuming than electrophoresis. Five selenium containing proteins were identified by on-line AE HPLC-ICP/MS (high performance liquid chromatography-inductively coupled plasma/mass spectrometry). Each protein was enzymatically hydrolyzed to seleno-amino acids and separated with RP (reverse phase) HPLC for the identification of selenoproteins.

A Study On Chemical Composition of Saururaceae Growing in Korea(5) On Flavonoid Constituents of Saururus Chinensis (한국에서 자생하는 Saururaceae의 성분에 관한 연구(5) Saururus chinensis의 Flavonoid 성분)

  • Choe, Koang-Hoon;Yoon, Chun-Hee;Kwon, Shoon-Ja
    • Analytical Science and Technology
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    • v.7 no.1
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    • pp.11-15
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    • 1994
  • From the aerial parts of Saururus chinensis growing in Korea, four flavonoids (hyperin, isoquercitrin, quercitrin and rutin) were isolated and identified by high performance liquid chromatography, gas chromatography and thin layer chromatography. However, avicularin, which was known as one of the main constituents of flavonoid, was not detected.

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Compositional Sugar Analysis of Antitumor Polysaccharidees by High Performance Liquid Chromatography and Gas Chromatography

  • Kim, Yeong-Shik;Park, Kyung-Shin;Park, Ho-Koon;Kim, Sung-Whan
    • Archives of Pharmacal Research
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    • v.17 no.5
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    • pp.337-342
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    • 1994
  • Carbohydrate analysis is important in studying structure and activity of complex polysaccharides. New analytical method was applied to get an information on the composition of polysaccharides showing antitumor activity. Monosaccharides were labeled with 7-amino-1, 3-naph-thalenedisulfonic acid (7-AGA) by reductive amination and separated by HPLC. Five kinds of polysaccharides from Basidiomycetes were hydrolyzed and analyzed in combination with electrophresis and HPLC. At the same time, alditol acetate derivatives were prepared and analyzed by gas chromatography. Two different techniques using different derivatization methods showed very similar results. The monosaccharides from Coriolus versicolor and Cordyceps militaris were glucose and galactose. Phellinus linteus composed of glucose, glactose, mannose, arabinose and fucose. The HPLC method with fluorescence detector was very sensitive compared to other methods.

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Analysis of flavonoids in the mature fruit of Vaccinium uliginosum L. of China

  • Hua, Lian Li;Yoshitama, Kunijiro
    • Advances in Traditional Medicine
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    • v.6 no.1
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    • pp.65-67
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    • 2006
  • In this study, a new extraction method was developed and two kinds of flavonoids were extracted from the mature fruit of Vaccinium uliginosum L. of China. These two kinds of flavonoids were analyzed by spectral and identified by high-performance liquid chromatography (HPLC) and UV/Vis. The extract of the fruit was total acid hydrolyzed. TLC chromatography was subsequently employed to identify the hydrolysate. Two kinds of aglycone flavonoids, quercetin and myricetin, were identified. At the same time PC chromatography was used to identify the monomer sugar in the flavonoids and it was verified as glucose. HPLC, UV/Vis, and Mass spectrum analyses revealed that the flavonoids were quercetin 3-monoglucosides and myricetin 3-monoglucosides.

Physico-chemical and Antagonistic Properties of Antibiotics Produced by Actinomycetes Isolate G-37 (방선균 분리주 G-37이 생산하는 항생물질의 물리.화학적 특성과 항균활성)

  • 여운형;김영호;채순용;박은경
    • Journal of the Korean Society of Tobacco Science
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    • v.17 no.2
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    • pp.103-108
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    • 1995
  • Antibiotic and physico-chemical properties of an active compound from actinomycetes isolate G-37, of which the culture filtrate had an inhibitory effect against tobacco mosaic virus(W) infection, were examined. The active compound, which was purified by ethylacetate extraction, silica gel column chromatography, preparative thin layer chromatography, and high performance liquid chromatography, showed strong antibacterial activities especially against Gram-positive bacteria including Bacillus subtillis, Sarcina lutea and Staphylococcus aureus. From the IH-NMR, FAB/RfS, UV spectral data, and physicochemical properties, the active compound of G-37 appears to belong to a peptide antibiotic group. Among the known peptide antibiotics in the antibiotic group, No. 280, A-30912, and Taitomycin showed molecular weights and ultra violet spectrum similar to those of the active compound from G-37, but was not identical to the compound, which suggests that it may be a new peptide antibiotics.

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