• Title/Summary/Keyword: reverse-phase high performance liquid chromatography

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Studies on the Triglyceride Composition of Job's Tears (율무 지질의 Triglyceride 조성에 관한 연구)

  • Lee, Hee-Ja;Cho, Kwang-Yun;Bae, Jung-Surl;Jang, Soon-Wook
    • Korean journal of food and cookery science
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    • v.6 no.4 s.13
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    • pp.27-32
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    • 1990
  • Lipids of Job's tears (Yullmoo) were extracted by the mixture of chloroform: methanol (2:1, v/v) and from these lipids, triglycerides were separated by column chromatography (Sephadex G-25 column) and then confirmed by thin layer chromatography (TLC) and reconfirmed by gas chromatography (GC). The triglycerides were fractionated into 6 groups on the basis of their partition numbers (PN) by reverse phase high performance liquid chromatography (HPLC) on a column Shimpack CLC-ODS using tetrahydrofuran-acetonitril (25:75) mixture as a solvent. Each of these collected fractions gave one to two peaks in the GC chromatograms according to the acyl carbon number (CN) of the triglyceride and fatty acid composition of the triglycerides were also analyzed by GC. From the results, the major triglycerides of Job's tears lipids were estimated to be C18:1 C18:2 C18:2 (OLL, 38.2%), C16:0 C18:2 C18:3 (PLLn, 15.7%), C18:1 C18:1 C18:2 (OOL, 12.6%).

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Simultaneous Determination of the Novel Neuroprotective Agent KR-31378 and its Metabolite KR-31612 Using High Performance Liquid Chromatography with Tandem Mass Spectrometry in Human Plasma

  • Kim, John;Ji, Hye-Young;Yoo, Sung-Eun;Kim, Sun-Ok;Lee, Dong-Ha;Lim, Hong;Lee, Hye-Suk
    • Archives of Pharmacal Research
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    • v.25 no.5
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    • pp.647-651
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    • 2002
  • An LC/MS/MS method for the simultaneous determination of a neuroprotective agent for ischemia-reperfusion damage, KR-31378 and its N-acetyl metabolite KR-31612 in human plasma was developed. KR-31378, KR-31612 and the internal standard. KR-31543 were extracted from human plasma by liquid-liquid extraction. A reverse-phase HPLC separation was performed on Luna phenylhexyl column with the mixture of acetonitrile-5 mM ammonium formate (55:45, v/v) as mobile phase. The detection of analytes was performed using an electrospray ionization tandem mass spectrometry in the multiple reaction monitoring mode. The lower limits of quantification for KR-31378 and KR-31612 were 2.0 ng/ml. The method showed a satisfactory sensitivity, precision, accuracy, recovery and selectivity.

Determination of Putrescine, Spermidine and Spermine in urine by HPLC (HPLC법에 의한 뇨 중의 Putrescine, Spermidine 및 Spermine의 정량)

  • Shin, Tae-Yong;Lee, Seok-Bong;Kim, Hyung-Min
    • Analytical Science and Technology
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    • v.10 no.6
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    • pp.445-452
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    • 1997
  • A simple and sensitive high performance liquid chromatography for analysis of Putrescine, Spermidine and Spermine in urine is described. The benzoyl chloride derivatives of Putrescine, Spermidine and Spermine are separated on a ${\mu}$ Bondapak $C_{18}$ reverse-phase column with methanol/$H_2O$(50/50v/v) as the mobile phase. The results show that the mean level of polyamines in uterine cancer patients urine is much higher than in normal human urine.

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Quantitative Analysis of chiisanoside in Acanthopanax Species by HPLC

  • Lee, Jeong-Min;Kim, Hye-Min;Lee, Sang-Hyun
    • Natural Product Sciences
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    • v.13 no.2
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    • pp.148-151
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    • 2007
  • High performance liquid chromatography (HPLC) was used for the analysis of chiisanoside in Acanthopanax species. A reverse-phase system using a gradient of H$_2$O and acetonitrile as the mobile phase was developed and a wavelength of detection was at 210 nm. The analysis was successfully carried out for 30 min. Chiisanoside was measured in the fruit, stem and root of A. sessiliflorus, A. koreanus, A. divaricatus and A. senticosus.

Purification of 4-Methylthio-3-butenyl isothiocyanate the Pungent Principle in Radish Roots by RP-HPLC (RP-HPLC법에 의한 무우의 매운 성분인 4-methylthio-3-butenyl isothiocyanate의 분리 및 정제)

  • Kim, Mee-Ree;Rhee, Hei-Soo
    • Korean journal of food and cookery science
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    • v.2 no.2
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    • pp.16-20
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    • 1986
  • The major pungent component from Korean radish roots was purified by reverse phase high performance liquid chromatography (RPHPLC), and characterized as 4-methylthio-3-butenyl isothiocyanate on the basis of the sensory test (pungency), UV spectrum and mass spectrum analysis. The purified isothiocyanate moved as a single peak(retention time, 5.2 min) in RP-HPLC analysis, and as a single spot(Rf, 0.9) in TLC analysis.

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Detection of Undeclared Betamethasone Derivatives in Cosmetic Products Labeled to Contain Zinc Pyrithione as the Active Ingredient (아연피리치온을 유효성분으로 표기한 화장품류에서 미표기 성분인 베타메타손 유도체의 검출)

  • Lee, Jeong-Pyo;Park, Sung-Hwan;Yang, Seong-Jun;Kim, Sun-Mi;Son, Kyung-Hun;Yun, Mi-Ok;Choi, Sang-Sook
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.35 no.1
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    • pp.11-17
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    • 2009
  • Betamethasone propionate, an anti-inflammatory glucocorticosteroid, was detected in cosmetics with no indication on the label of this compound as an ingredient. The product was formulated as a topical spray or shampoo and labeled to contain zinc pyrithione as the active ingredient. A thin-layer chromatographic analysis was carried out on silica gel plates to provide a first indication about the presence of a compound with steroid structure and reactivity; then high-performance liquid chromatography (HPLC) separation allowed the identification of the corticosteroid agent and its quantification. To identify the corticosteroid agent from these commercial samples we collected the fractions suspected to have ketol steroids by prep HPLC and identified the compound as betamethasone propionate by NMR and MS spectrometry. Then we synthesized the standard for the betamethasone 17-propionate and 21-propionate and quantitate the corticosteroids from the sample by HPLC with that standards. By this method we identified the corticosteroid compounds from some commercial cosmetics such as zinc pyrithione sprays. The finding of betamethasone propionate in the products was shown by comparison to an authenticated standard of betamethasone propionate by retention time on reverse-phase HPLC. Two of the tested products contained betamethasone propionate at the levels of 0.005 ${\sim}$ 0.02% and the others were free of betamethasone propionate.

Pharmacokinetic Analysis of Montelukast in Healthy Korean Volunteers by High Performance Liquid Chromatography-Tandem Mass Spectrometry

  • Jo, Min-Ho;Park, Mi-Sun;Seo, Ji-Hyung;Shim, Wang-Seob;Yim, Sung-Vin;Lee, Kyung-Tae
    • Journal of Pharmaceutical Investigation
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    • v.41 no.5
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    • pp.289-294
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    • 2011
  • A rapid and specific high performance liquid chromatography-tandem mass (LC/MS/MS) method for the analysis of montelukast in human plasma has been developed and validated. After cold acetonitrile-induced precipitation of the plasma samples, montelukast and glipizide (internal standard, IS) were eluted on a reverse-phase $C_{18}$ column by isocratic mobile phase consisted of 10 mM ammonium formate buffer (adjusted to pH 3.5 with formic acid) and acetonitrile (3:97, v/v). Acquisition was performed with multiple reaction monitoring (MRM) mode by monitoring the transitions: m/z 587.2${\rightarrow}$ 423.2 for montelukast and m/z 446.0${\rightarrow}$321.2 for IS. Ranges of concentration for calibration curves (10-1000 ng/mL) showed correlation coefficients ($r^2$) were better than 0.9948. Precision of intra- and inter-day ranged from 3.70 to 11.68% and from 3.04 to 12.95%, accuracy of intra-day and inter-day ranged from 93.34 to 102.75% and from 100.79 to 107.63%, respectively. The described method provides a fast and sensitive analytical tool for determining montelukast levels in plasma, and was successfully applied to a pharmacokinetic study in 16 healthy human subjects after oral administration of 10mg tablet formulation of montelukast sodium under fasting conditions.

Simultaneous Determination of Vitamin A and E in Infant Formula by HPLC with Photodiode Array Detection

  • Lee, Hong-Min;Kwak, Byung-Man;Ahn, Jang-Hyuk;Jeong, Seung-Hwan;Shim, Sung-Lye;Kim, Kyong-Su;Yoon, Tae-Hyung;Leem, Dong-Gil;Jeong, Ja-Young
    • Food Science of Animal Resources
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    • v.31 no.2
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    • pp.191-199
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    • 2011
  • The objective of this study was to develop a method to simultaneously quantify vitamins A and E in infant formula. To determine the vitamin A and E content, vitamin A and four different vitamin E isomers (${\alpha}$-, ${\beta}$-, ${\gamma}$-, and ${\delta}$-tocopherol) were separated by high performance liquid chromatography with a photodiode array detector using a Develosil RPAQUEOUS RP-$C_{30}$ column ($4.6{\times}250$ mm, 5 ${\mu}M$). The vitamin A and E contents in the certified reference material determined using this method were within the certified range of standard values. The limits of detection (LODs) and limits of quantitation (LOQs) for vitamin A were 0.02 and 0.06 ${\mu}g/L$, respectively. LODs and LOQs for the vitamin E isomers ranged from 0.20 to 0.55 and from 0.67 to 1.81 ${\mu}g/L$, respectively. Linear analyses indicated that the square of the correlation coefficient for the vitamin A and E isomers was 0.9997-0.9999. The recovery of vitamins ranged from 96.69 to 97.79%. The results demonstrate that this novel method could be used to reliably analyze vitamin A and E content in infant formula.

High-performance liquid chromatographic assay and oral pharmacokinetics of new anti-HIV uracil derivatives, KR-V analogues, in rats

  • Lee, Youngmi;Heeok Shim;Seoungryong Yu;Hochul Shin;Moonkoo Chung;Jungkoo Roh
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1998.11a
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    • pp.123-123
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    • 1998
  • A number of uracil derivatives have been developed as anti-AIDS drugs having a mechanism of inhibiting cellular reverse transcriptase. A simple and rapid assay technique for recently synthesized KR-V analogues was developed using a high-performance liquid chromatography, and oral pharmacokinetics was examined for assessing their oral bioavailabilites. Plasma samples were analyzed by reversed-phase HPLC using an ODS column with an ultraviolet detection system. All the analogues were eluted within 12 min and the LOQ was 15-30 ng/$m\ell$. The extraction recoveries were higher than 85%, except KR-V1039, 1068 and 1720 having ester group. This chromatic method was well applied to the kinetic studies for KR-V analogues. Among 16 analogues tested in the present work, the 6 compounds including KR-V1123, 1122, 1784, 1783, 1736 and 1700 were found to be bioavailable for oral administration to rats.

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DERIVATIZATION OF FATTY ACIDS WITH 2-BROMOACETYLTRIPHENYLENE FOR HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

  • Ryu, Jae-Ha;Park, Man-Ki
    • Analytical Science and Technology
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    • v.6 no.4
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    • pp.411-415
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    • 1993
  • A method for UV labeling of fatty acids with 2-bromoacetyltriphenylene using 18-crown-6-ether as a catalyst is described. The procedure is rapid, simple, quantitative and applicable to the HPLC analysis of fatty acids with UV detector. They have high molar absorptivity and their detection limit was about 1ng level. Nine derivatives of saturated fatty acid($C_{12}-C_{22}$) were separated on reverse-phase column(${\mu}$-Bondapak C-18) using acetonitrile-water gradient.

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