• 제목/요약/키워드: reversed phase

검색결과 605건 처리시간 0.027초

대추로부터 베튜리닉 산과 알피톨릭 산의 분리 및 정량 (Isolation and Quantitative Analysis of Betulinic Acid and Alphitolic Acid from Zyziphi Fructus)

  • 배기환;이상명;이은실;이준성;강종성
    • 약학회지
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    • 제40권5호
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    • pp.558-562
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    • 1996
  • Betulinic acid and alphitolic acid, the triterpenoids of Zyziphi Fructus, were isolated with silica gel column chromatography and used as the standard substances for the analysis. The compounds were determined with HPLC and HPTLC. They were separated on reversed phase column (Nova-Pak C18) with 0.05M Na2HPO4-methanol (19:81) in HPLC and detected at 210nm. Separation on HPTLC precoated silica gel F254 plates was carried out with chloroform-methanol (6:1) and the separated compounds were reacted with p-anisaldehyde and detected at 540nm. The contents of betulinic acid and alphitolic acid in Zyziphi Fructus from four different regions in Korea were in the range of 2.9~3.8% and 3.2~3.9%, respectively.

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HPLC를 이용한 목향 및 유사 한약재에 함유된 Costunolide 비교 (Determination of Costunolide from Aucklandiae Radix and Substitutive Herbs by Reversed-Phase HPLC)

  • 오주희;홍선표;최호영;박용기;이제현
    • 대한본초학회지
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    • 제23권3호
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    • pp.61-66
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    • 2008
  • Objecives : Aucklandiae Radix is a root of Aucklandia lappa which has been widely used for regulating the flow of vital energy, invigorating the spleen, alleviating pain. Aucklandiae Radix contains the costunolide which is the main ingredient. The substitutive Aucklandiae Radix are Inulae helenii Radix, Aristolchiae Radix, Vladimiriae Radix, and Inulae racemosi Radix in Korea and China. This paper is analysised and compared the costunolide and HPLC pattern in Aucklandiae Radix and substitute herbs. Methods : Chromatographic separation performed using C18 column(Luna 5 u, 250 mm ${\times}$ 4.6 mm) with a mixture of methanol and water(65:35)(v/v). The analyses detected at UV(210 nm). Results : Optimal extraction condition of costunolide was 100% methanol for 2hr. Costunolide was detected in Aucklandiae Radix and Vladimiriae Radix, but other herbs were not detected. In Korea herbal market, Aristolchiae Radix merchandise was identified as the imported Inulae helenii Radix. Conclusions : According to above results, this method was useful identified to Aucklandiae Radix and substitutive herbs. In Korea herbal market, Aristolchiae Radix was identified as Inulae helenii Radix.

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희토류 원소의 분리 및 정량을 위한 이온회합 크로마토그래피 (The Separation and Determination of Rare Earth Elements by Ion-Association Chromatography)

  • 이승화;이철;정구순
    • 대한화학회지
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    • 제34권1호
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    • pp.69-75
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    • 1990
  • 모자나이트 광물 중에 포함된 각각 희토류 원소를 이온회합 크로마토그래피 방법으로 분리 및 정량하였다. 정량하기 전에 양이온교환수지(Dowex 5OW-X8) 칼럼으로 희토류 원소를 집단 분리하였다. 이 때 수지 칼럼에 의하여 희토류 원소가 정량적으로 회수되며, 시료 중의 공존이온으로부터 깨끗이 분리됨을 방사성 추적자 및 유도쌍 결합 분광-질량분석법(ICP-MS)으로 각각 확인 하였다. 역상 칼럼($\mu$-Bondapak $C_{18}$)에 의하여 미량(ppm)의 희토류 원소를 pH 4.6의 $\alpha$-hydroxyisobutyric acid으로 0.05M부터 0.3M까지 기울기 용출하여 각각 분리하였다. 희토류 원소와 PAR (4-(2-pyridylazo)-resorcinol monosodium salt)과의 포스터 칼럼 착색반응을 통하여 각각의 희토류 원소를 검출하였다.

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쇠비름에서 분리된 2개의 Biophenolic Glycosides (Two Biophenolic Glycosides from Portulaca oleracea)

  • 서영완;신종헌;이범종;이동석
    • 대한화학회지
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    • 제47권1호
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    • pp.43-46
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    • 2003
  • 우리나라에 널리 분포하며 오래 동안 약용으로 사용되어 온 쇠비름으로부터 페놀 글리코시드인 3-hydroxy-1(2-hydroxyethyl)phenyl-4-O-${\beta}$-D-glucopyranoside(1)과 2-(3,4-dihydroxyphenyl)ethyl-O-${\beta}$-D-glucopyranoside (2)를 칼럼 크로마토그래피 및 역상 HPLC로 분리하였으며, NOESY, HMQC, HMBC와 같은 이차원적인 NMR 분광실험에 의해서 이 물질들의 $^{13}C$ NMR 분광 데이터 값의 지정이 수정되었다. DPPH를 이용하여 이 물질들의 항산화 활성을 측정한 결과 주목할 만한 활성을 나타내었다.

기상요인과 채취시기가 옻나무 칠액채취량 및 칠액의 質에 미치는 영향 (Effects of Climatic Factors and Tapping Date on Yield and Quality of Lactree (Rhus verniciflua) Sap)

  • 김만조
    • 한국자원식물학회지
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    • 제11권1호
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    • pp.70-79
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    • 1998
  • This study was conducted to understand the effects of weather and tapping date on yield and quality of lactree(Rhus verniciflua) sap yield showed a significant positive correlation with the minimum temperature of one day before sap collection at 1% level and with theminimum humidity of theday of sap collection at 5% level. However, the differences between the maximum and the minimum temperatures and humidities of the day of sap collection were negatively correlated with the sap yield at 5% level. Multiple regression analysis indicated that the minimum temperature of one day bofore sap collection and the minumum humidity of the day sap collection were important factors for increasing sap yield. The high sap yield of lactree by Japanese tapping method was recorded during mid-July and early August. Seasonal variation in lactree sap constituents was observed. The sap collected on 15th of August contained the highest urushiol content (68.3%) and the lowest water content resulting in high quality of lactree sap. By reversed-phase HPLC analysis, fove urushiol components were separated from each other depending on the number of doulbe bonds in the side-chain , and seaxonal variation of urushiol composition was noticed. The 3-C15 triene content fo the sap collected on 5th of July was the highest(77.56%) indicating the major component of urushiol which affects lactree sap quality.

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Determination of Recombinant Human Epidermal Growth factor (rhEGF) in a Pharmaceutical Formulation by High Performance Liquid Chromatography with Electrochemical Detection

  • Lee, Kang-Woo;Hwang, Kyung-Hwa;Kim, Chang-Soo;Han, Kun;Chung, Youn-Bok;Park, Jeong-Sook;Lee, Yong-Moon;Moon, Dong-Cheul
    • Archives of Pharmacal Research
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    • 제24권4호
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    • pp.355-359
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    • 2001
  • A novel HPLC method with electrochemical detection has been developed for the determination of recombinant human epidermal growth factor (rhEGF) in pharmaceutical products. rhEGF was separated from other components in formulation on a reversed-phase C18 column with 24% acetonitrile in 0.1 M phosphate buffer (pH 4.75). The optimum electrochemical oxidation of EGF was obtained at 0.85 V vs. Ag/AgCl in a glassy carbon working electrode due to electroactive tyrosine, tryptophan, methionine, and arginine residues. The quantitation range was from 1.0 to 200 ng of rhEGF with the linear correlation coefficient greater than 0.999. The method was successfully applied for the quantitation of rhEGF in a pharmaceutical preparation.

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Phosphate and Carbon Source Regulation of Alkaline Phosphatase and Phospholipase in Vibrio vulnificus

  • Oh, Wan-Seok;Im, Young-Sun;Yeon, Kyu-Yong;Yoon, Young-Jun;Kim, Jung-Wan
    • Journal of Microbiology
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    • 제45권4호
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    • pp.311-317
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    • 2007
  • In this study, the effects of phosphate concentration and carbon source on the patterns of alkaline phosphatase (APase) and phospholipase (PLase) expression in Vibrio vulnificus ATCC 29307 were assessed under various conditions. The activities of these enzymes were repressed by excess phosphate (4 mM) in the culture medium, but this repression was reversed upon the onset of phosphate starvation in low phosphate defined medium (LPDM) containing 0.2 mM of phosphate at approximately the end of the exponential growth phase. The expressions of the two enzymes were also influenced by different carbon sources, including glucose, fructose, maltose, glycerol, and sodium acetate at different levels. The APase activity was derepressed most profoundly in LPDM containing fructose as a sole carbon source. However, the repression/derepression of the enzyme by phosphate was not observed in media containing glycerol or sodium acetate. In LPDM-glycerol or sodium acetate, the growth rate was quite low. The highest levels of PLase activity were detected in LPDM-sodium acetate, followed by LPDM-fructose. PLase was not fully repressed by high phosphate concentrations when sodium acetate was utilized as the sole carbon source. These results showed that multiple regulatory systems, including the phosphate regulon, may perform a function in the expression of both or either APase and PLC, in the broader context of the survival of V. vulnificus.

Glioblastoma-Specific Anticancer Activity of Pheophorbide a from the Edible Red Seaweed Grateloupia elliptica

  • Cho, MyoungLae;Park, Gab-Man;Kim, Su-Nam;Amna, Touseef;Lee, Seokjoon;Shin, Woon-Seob
    • Journal of Microbiology and Biotechnology
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    • 제24권3호
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    • pp.346-353
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    • 2014
  • The chlorophyll-related compound pheophorbide a (Pa) was successively purified from an edible red seaweed, Grateloupia elliptica, using silica, octadecyl silica column chromatography and reversed phase-high-performance liquid chromatography, as well as the cell cycle inhibitory and apoptotic effects of Pa being investigated in U87MG glioblastoma cells. The Pa exhibited strong anticancer effects in the absence of direct photo-irradiation against various cancer cell lines, including U87MG, SK-OV-3, and HeLa cells. Among the cancer cells, the strongest anticancer activity of Pa exhibited on U87MG cells with $IC_{50}$ values of 2.8 ${\mu}g/ml$. In addition, Pa specifically had cytostatic activity on glioblastoma cells rather than human umbilical vein endothelial cells. Analysis of the cell cycle distribution showed that Pa induced G0/G1 arrest of U87 MG cells. In addition, arrested cells induced late apoptosis and DNA degradation under dark condition. These results suggest that Pa isolated from G. elliptica is a potential glioblastoma-specific anticancer agent without side effects on normal cells.

Liquid Chromatographic Determination of Etofenprox Residues in Foods with Mass-Spectrometric Confirmation

  • Lee, Young-Deuk;Kwon, Chan-Hyeok;Kwon, Ki-Sung
    • 한국환경농학회지
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    • 제30권4호
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    • pp.432-439
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    • 2011
  • BACKGROUND: An official analytical method was developed to determine etofenprox residues in agricultural commodities using high-performance liquid chromatography (HPLC). METHODS AND RESULTS: The etofenprox residue was extracted with acetone from representative samples of five raw products which comprised rice grain, apple, mandarin, cabbage, and soybean. The extract was then serially purified by liquid-liquid partition and Florisil column chromatography. For rice and soybean samples, acetonitrile/n-hexane partition was additionally coupled to remove nonpolar lipids. Reversed phase HPLC using an octadecylsilyl column was successfully applied to separate etofenprox from co-extractives. Intact etofenprox was sensitively detected by ultraviolet absorption at 225 nm. Recovery experiment at the quantitation limit validated that the proposed method could apparently determine the etofenprox residue at 0.02 mg/kg. Mean recoveries from five crop samples fortified at three levels in triplicate were in the range of 93.6~106.4%. Relative standard deviations of the analytical method were all less than 10%, irrespective of crop types. A selected-ion monitoring LC/mass spectrometry with positive atmospheric-pressure chemical ionization was also provided to confirm the suspected residue. CONCLUSION(s): The proposed method is simple, rapid and sensitive enough to be employed in routine inspection or monitoring of agricultural products for the etofenprox residue.

Antioxidant Activities and Determination of Phenolic Acids from Leaves of Perilla frutescens

  • Lee, Jin-Hwan;Kang, Nam-Suk;Ha, Tae-Joung;Ko, Jong-Min;Han, Won-Young;Suh, Duck-Yong;Park, Ki-Hun;Baek, In-Youl
    • Journal of Applied Biological Chemistry
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    • 제49권1호
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    • pp.11-15
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    • 2006
  • Two catecholic phenolic acids (1 and 2) obtained from 80% methanolic extract of Perilla frutescens var. frutescens leaves through chromatography showed strong DPPH (1: $IC_{50}$ = 15.5 ${\mu}M$, 2: $IC_{50}$ = 11.7 ${\mu}M$) and ABTS (1: $IC_{50}$ = 5.5 ${\mu}M$, 2: $IC_{50}$ = 4.6 ${\mu}M$) radicals scavenging abilities. Antioxidant compounds contents of 1 and 2 as determined by $C_{18}$ reversed phase HPLC coupled with diode-array detector were 2.98 and 2.26 mg/g, respectively.