• Title/Summary/Keyword: cyano column

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Determination of Allantoin in Dioscorea Rhizoma by High Performance Liquid Chromatography Using Cyano Columns

  • Yoon, Kee-Dong;Yang, Min-Hye;Chin, Young-Won;Park, Ju-Hyun;Kim, Jin-Woong
    • Natural Product Sciences
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    • v.14 no.4
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    • pp.254-259
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    • 2008
  • An easy and reliable HPLC method was developed to determine allantoin in Dioscorea Rhizoma using cyano columns. Qualitative and quantitative analyses of allantoin were performed successfully by cyano columns (YMC-Pack CN column, Zorbax SB-CN column and Discovery$^{(R)}$ Cyano column). The intraday precision were 0.58 - 3.33% for YMC-Pack CN, 0.41 - 2.20 for Zorbax SB-CN and 0.45 - 1.93% Discovery$^{(R)}$ Cyano columns, while interday variations were 0.09 - 1.84%, 0.04 - 2.59% and 0.87 - 5.18% for YMC-Pack CN, Zorbax SB-CN and Discovery$^{(R)}$ Cyano columns. The recoveries of allantoin were in the range at 98.8 - 102.6% (RSD 1.1 - 1.6%) for YMC-Pack CN column, 99.7 - 110.5% (RSD 1.3 - 4.9%) for Zorbax SB-CN column, and 97.2 - 110.1% (RSD 1.8 - 5.7%) for Discovery$^{(R)}$ Cyano column. The contents of allantoin in four Dioscorea Rhizoma samples were determined by cyano columms and ranged at 4.1-7.1 mg/g dry weight. The present study indicated that HPLC method using cyano column for determining allantoin is a reliable method and this method can be applied to verify allantoin in Dioscorea Rhizoma.

Chromatographic Selectivity of Cyano-Bonded Silica Columns in RPLC Based on the Linear Solvation Energy Relationships

  • Park, Jung-Hag;Jang, Myung-Duk;Kwon, Se-Mok
    • Bulletin of the Korean Chemical Society
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    • v.13 no.1
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    • pp.75-79
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    • 1992
  • Differences in chromatographic properties in RPLC of four brands of cyano bonded silica stationary phases are rationalized in terms of the type and relative strength of the solute-stationary phase interactions, which can be readily inferred from multiple linear regression analyses of retention data for a set of standard compounds on the stationary phases under study based on the linear solvation energy relationships (LSERs). Although four brands of cyano bonded columns studied (CPS-Hypersil, Ultrasphere cyano, Spherisorb-CN and ${\mu}$-Bondapak-CN) have similar bonding density and have been prepared from monofunctional cyanopropylsilane reagents, they possess quite different, relative hydrogen bonding (HB) donor and acceptor strengths. Comparison of the retention behavior on a cyano-bonded silica column with that on an ODS column shows that there are significant differences in the strength of HB interactions between the solute and the stationary phase on the two columns with different functionalities. Information on the differences in the interaction characteristics among brands of the cyano-bonded silica columns and between the ODS and cyano-bonded columns can be utilized to optimize the selectivity for a given separation on these columns.

Determination of Pd(II) and Pt(II) Metal Cyano Complexes Using Capillary Electrophoresis

  • Lee, Hue-Jin;Lee, Sang-Ho;Chung, Koo-Soon;Lee, Kwang-Woo
    • Bulletin of the Korean Chemical Society
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    • v.15 no.11
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    • pp.945-949
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    • 1994
  • Mixtures of cyano complexes of palladium(II) and platinum(II) were separated by capillary electrophoresis using a fused silica capillary as a separation column and 30 mM phosphate buffer (pH 7) containing 15 wt. % acetonitrile as a running buffer. By virtue of the high ionic mobilities of the negatively charged cyano complexes of Pd(II) and Pt(II), they were separated using a cathodic injection and anodic detection scheme. The metal complexes eluted through the capillary were detected by direct UV absorption at 214 nm. A linear relationship between peak area and concentration was obtained for both ions and the detection limit was lower than $10^{-14}$ mole. The proposed method was applied to real sample, e.g., anode slime obtained from an electrolytic copper refinary, as a method for the simultaneous determination of palladium and platinum.

Determination of dextromethorphan and its metabolite dextrorphan in human urine by High-performance liquid chromatography

  • Son, Haeng-Ja;Park, Mee-Jung;Choi, Sang-Kil;Lim, Mi-Ae;Chung, Hee-Sun
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.279.2-280
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    • 2003
  • A simple and accurate reverse-phase high performance liquid chromatography (HPLC) coupled with photodiode array was developed for the determination of dextromethorphan(DM) and its metabolite dextrorphan(DX) in human urine. Chromatographic separation was accomplished on a cyano analytical column at 220 nm using a mobile phase containing 25 mM triethylammonium phosphate buffer(PH 3.0) in a 0-70% ACN gradient and triazolam(TZ) was used as internal standard(I.S). (omitted)

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Simultaneous HPLC Determination of Preservatives in Cosmetics (화장품중 살균ㆍ보존제의 동시분리 및 정량)

  • 양성준;김영옥;손경훈;이정표;정래석;양원준;백옥진;이현경;최상숙
    • YAKHAK HOEJI
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    • v.46 no.4
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    • pp.231-236
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    • 2002
  • A high-performance liquid chromatographic method for the simultaneous quantitative analysis of methylparaben (MP), ethylparaben (EP), propylparaben (PP), butylparaben (BP) and imidazolidinyl urea(IU) or diazolidinyl urea(DU) in cosmetics was studied by using a cyano-propyl column and 0.05M hexanesulfonic acid at 228 nm. Calibration curves were found to be linear in the 60-1000 $\mu\textrm{g}$/mL range (parabens), 100-1,250 $\mu\textrm{g}$/mL range (IU) and the 120-2000 $\mu\textrm{g}$/mL range (DU). Linear regression analysis of the data demonstrates the efficacy of the method in terms of precision and accuracy. An extraction method is developed and validated in order to apply this chromatographic method to a commercial cosmetic cream. The precision of this method, calculated as the relative standard deviation (RSD) of the recoveries (0.46-2.71%) was excellent for all compounds.

An Improved HPLC Assay Using Hg/Au Electrochemical Detector for S-2-(3-aminopropylamino) ethylphosphorothioate and S-2-(3-methylaminopropylamino) ethylphosphorothioate in Human Plasma (사람혈장중 S-2-(3-Aminopropylamino) ethylphosphorothioate 및 S-2-(3-Methylaminopropylamino) ethylphosphorothioate의 수은/금 전기화학검출기를 이용한 고속액체크로마토 그라프법에 의한 분석)

  • Han, Kun;Lin, Emil T.
    • Journal of Pharmaceutical Investigation
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    • v.17 no.2
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    • pp.55-60
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    • 1987
  • WR 2721 (S-2-(3-aminopropylaminoethylphosphorothioate) is a radioprotective drug that is now undergoing clinical trials in the United States and Japan. a liquid chromatographic electrochemical method for the determination of WR 2721 an WR 3689 [S-2-(3-methylaminopropylamino)ethylphorothioate] in human plasma was developed in this study. This method includes the use of a Hg/Au electrochemical detector and a cyano column for the direct measurement of WR 2721 and WR 3689 in plasma. An analog of WR 2721, WR 149846 was used as an internal standard. WR 2721 and WR 3689 could be well separated from the solvent front, with a mobile phase of acetonitrile-water (20:80), 0.1M acetic acid and 1.2 mM sodium octane sulfonate. This method was shown to be precise. Both intra-day and inter-day results were within 10% CV. Also, sample preparation was fairly simple. Since WR 2721 and WR 3689 were unstable at room temperature, it was essential to use an automatic sample processor with a refrigerator, especially for carrying out routine analyses.

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Phytochemical Analysis and Anti-cancer Investigation of Boswellia Serrata Bioactive Constituents In Vitro

  • Ahmed, Hanaa H;Abd-Rabou, Ahmed A;Hassan, Amal Z;Kotob, Soheir E
    • Asian Pacific Journal of Cancer Prevention
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    • v.16 no.16
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    • pp.7179-7188
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    • 2015
  • Cancer is a major health obstacle around the world, with hepatocellular carcinoma (HCC) and colorectal cancer (CRC) as major causes of morbidity and mortality. Nowadays, there isgrowing interest in the therapeutic use of natural products for HCC and CRC, owing to the anticancer activity of their bioactive constituents. Boswellia serrata oleo gum resin has long been used in Ayurvedic and traditional Chinese medicine to alleviate a variety of health problems such as inflammatory and arthritic diseases. The current study aimed to identify and explore the in vitro anticancer effect of B. Serrata bioactive constituents on HepG2 and HCT 116 cell lines. Phytochemical analysis of volatile oils of B. Serrata oleo gum resin was carried out using gas chromatography-mass spectrometry (GC/MS). Oleo-gum-resin of B. Serrata was then successively extracted with petroleum ether (extract 1) and methanol (extract 2). Gas-liquid chromatography (GLC) analysis of the lipoidal matter was also performed. In addition, a methanol extract of B. Serrata oleo gum resin was phytochemically studied using column chromatography (CC) and thin layer chromatography (TLC) to obtain four fractions (I, II, III and IV). Sephadex columns were used to isolate ${\beta}$-boswellic acid and identification of the pure compound was done using UV, mass spectra, $^1H$ NMR and $^{13}C$ NMR analysis. Total extracts, fractions and volatile oils of B. Serrata oleo-gum resin were subsequently applied to HCC cells (HepG2 cell line) and CRC cells (HCT 116 cell line) to assess their cytotoxic effects. GLC analysis of the lipoidal matter resulted in identification of tricosane (75.32%) as a major compound with the presence of cholesterol, stigmasterol and ${\beta}$-sitosterol. Twenty two fatty acids were identified of which saturated fatty acids represented 25.6% and unsaturated fatty acids 74.4% of the total saponifiable fraction. GC/MS analysis of three chromatographic fractions (I,II and III) of B. Serrata oleo gum resin revealed the presence of pent-2-ene-1,4-dione, 2-methyl- levulinic acid methyl ester, 3,5- dimethyl- 1-hexane, methyl-1-methylpentadecanoate, 1,1- dimethoxy cyclohexane, 1-methoxy-4-(1-propenyl)benzene and 17a-hydroxy-17a-cyano, preg-4-en-3-one. GC/MS analysis of volatile oils of B. Serrata oleo gum resin revealed the presence of sabinene (19.11%), terpinen-4-ol (14.64%) and terpinyl acetate (13.01%) as major constituents. The anti-cancer effect of two extracts (1 and 2) and four fractions (I, II, III and IV) as well as volatile oils of B. Serrata oleo gum resin on HepG2 and HCT 116 cell lines was investigated using SRB assay. Regarding HepG2 cell line, extracts 1 and 2 elicited the most pronounced cytotoxic activity with $IC_{50}$ values equal 1.58 and $5.82{\mu}g/mL$ at 48 h, respectively which were comparable to doxorubicin with an $IC_{50}$ equal $4.68{\mu}g/mL$ at 48 h. With respect to HCT 116 cells, extracts 1 and 2 exhibited the most obvious cytotoxic effect; with $IC_{50}$ values equal 0.12 and $6.59{\mu}g/mL$ at 48 h, respectively which were comparable to 5-fluorouracil with an $IC_{50}$ equal $3.43{\mu}g/mL$ at 48 h. In conclusion, total extracts, fractions and volatile oils of B. Serrata oleo gum resin proved their usefulness as cytotoxic mediators against HepG2 and HCT 116 cell lines with different potentiality (extracts > fractions > volatile oil). In the two studied cell lines the cytotoxic acivity of each of extract 1 and 2 was comparable to doxorubicin and 5-fluorouracil, respectively. Extensive in vivo research is warranted to explore the precise molecular mechanisms of these bioactive natural products in cytotoxicity against HCC and CRC cells.