• Title/Summary/Keyword: plasma column

검색결과 236건 처리시간 0.025초

하늘타리(Trichosanthes kirilowii Max) 재분획물이 Steptozotocin 유발 당뇨 흰쥐의 인슐린 활성에 미치는 영향 및 급성독성에 관한 연구 (The Effect of Trichosanithes kirilowii Max. Subfractions on the Insulin Activity in Streptozotocin Induced Diabetic Rats and Their Acute Toxicity)

  • 임숙자
    • Journal of Nutrition and Health
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    • 제30권1호
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    • pp.25-31
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    • 1997
  • The effects of Trichosanthes kirilowii Max. subfractions, which has long been used as a wild vegetable and folk medicine, on insulin activity and acute toxicity were investigated. Diabetes melitus was induced in male Sprague-Dawley rats by the injection of streptozotocin(STZ) into the tail vein at a dose of 45mg/kg. The hexane fraction of the plant was subfractioned by silica gel column chromatography and were administered orally for 14 days and the normal and STZ-control group were orally administered with tween 80. The body weight gain was monitored and plasma levels of glucose, cholesterol, triglyceride, free fatty acid HDL-cholesterol were determined. The plasma activities of aspartate aminotransferase(AST) and alanine aminotransferase (ALT) were analysed. The subjraction A of hexane fraction lowered plasma glucose levels significantly and increased insulin activity compared to that of STZ-control. The activities of AST and ALT were decreased by administration of subfractions A and C of hexane fraction. The intakes of the hexane fraction of Trichosanthes kirilowii Max. did not showed the acute toxicity. It is suggested from the results that the subfraction A of the hexane fraction of Trichosanthes kirilowii Max. showed a hypoglycemic effect on diabetic rats and that the subfraction may be beneficial for insulin secreation.

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A Fast Determination of Globotriaosylsphingosine in Plasma for Screening Fabry Disease Using UPLC-ESI-MS/MS

  • Yoon, Hye-Ran
    • Mass Spectrometry Letters
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    • 제6권4호
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    • pp.116-119
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    • 2015
  • Globotriaosylsphingosine (lyso-Gb3) is considered as one of the biological marker for Fabry disease. To date, a reliable biomarker that reflects disease severity and progression has not been discovered to guide the management of Fabry disease. A new method included a simple protein precipitation with acetonitrile in 100 μL of plasma following analyte separation on an Phenomenex Kintex- C18 column using a gradient elution (0.1% formic acid in 5-90% acetonitrile). Total run time was within 12 min including sample preparation and MS/MS analysis. The limit of detection and limit of quantitation were 1 ng/mL and 2 ng/mL, respectively. The calibration curve was linear over the concentration range of 2.0-200.0 ng/mL (r2 = 0.9999). Inter-day accuracy and precision at 7 level were 93.4-100.7% with RSD of 0.55-5.97%. Absolute recovery was 97.6-98.6%. The method was applied to human and mice plasma, proved the suitability for quantification of lyso-Gb3 for screening, diagnosis and therapeutic monitoring of Fabry disease patients.

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

  • 한건
    • Journal of Pharmaceutical Investigation
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    • 제17권2호
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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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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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    • 제25권5호
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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.

Identification and Purification of a Normal Rat Liver Plasma Membrane Surface Protein which Disappears after Chemical Carcinogenesis

  • Kim, Min-Young;Lee, Myung-Kyu;Hahm, Kyung-Soo
    • BMB Reports
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    • 제28권6호
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    • pp.504-508
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    • 1995
  • The electrophoretic patterns of plasma membrane surface proteins of normal rat liver cells and rat hepatomas were compared in 10% non-denaturing and 7-15% gradient non-denaturing gel. Chemical carcinogens, 2-Me DAB (2-methyl-4-dimethylaminoazobenzene) and DENA (diethylnitrosamine), were used to induce hepatoma in rats. One protein which disappeared in hepatoma was identified in normal rat liver by non-denaturing gel electrophoresis. Rabbit antisera were raised against this specific protein, and the protein was purified by Sephacryl S-200 column and immunoaffinity chromatography using the purified antibody. The purified protein showed two bands of molecular weights approximately 50 $kD_{\alpha}$ and 52 $kD_{\alpha}$ by SDS-polyacrylamide gel electrophoresis, which reacted specifically with the antibody. However only one band was observed in non-denaturing gel and also in isoelectric focusing with a pI value of 6.6. This study showed the existence of an unique protein on the plasma membrane surface of normal rat liver cells which disappeared in rat hepatomas induced by chemical carcinogens.

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인체 혈장에서 염산시프로플록사신(시프로플록사신으로서 250 mg) 정량을 위한 HPLC 분석법의 유효성검토 (Validation of a Simple HPLC Method for Determination of Ciprofloxacin Hydrochloride in Human Plasma)

  • 하용화;조성희;천성국;서성훈;류재환;최영욱;이경태
    • Journal of Pharmaceutical Investigation
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    • 제34권4호
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    • pp.327-331
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    • 2004
  • A simple HPLC method with ultraviolet detection of ciprofloxacin in human plasma was developed and validated. After protein precipitation with trichloroacetic acid, chromatographic separation of ciprofloxacin in plasma was achieved at $50^{\circ}C$ with a $C_{18}$ column and methanol-phosphate mixture (pH 2.5), as mobile phase. Quantitative determination was performed by ultraviolet detection at 278 nm. The method was specific and validated with a limit of quantification of 100 ng/ml. The intra- and inter-day coefficients of variation were between 1.67% and 10.55% and accuracy between 92.01 % and 106.09%. The method has been successfully applied in a bioavailability study of 250 mg ciprofloxacin hydrochloride tablet.

Identification of IY81149 and Its Metabolites in the Rat Plasma Using the On-Line HPLC/ESI Mass Spectrometry

  • Myung, Seung-Woon;Min, Hye-Ki;Jin, Chang-Bae;Kim, Myung-Soo;Lee, Seung-Mok;Chung, Gi-Ju;Park, Seong-Jun;Kim, Dong-Yeon;Cho, Hyun-Woo
    • Archives of Pharmacal Research
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    • 제22권2호
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    • pp.189-193
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    • 1999
  • Reversed-phase high-performance liquid chromatography/mass spectrometry (HPLC/MS) with an eletcrospray ionization (ESI) interface was applied to the identification of metabolites of IY81149 in the rat plasma. Fragments obtained using collision-induced dissociation (CID) in both positive and negative modes were utilized to elucidate the structure of metabolites. The eluent from the conventional HPLC column was split and directly introduced into an ESI-mass spectrometer for the identification of the structures. the CID technique allowed the sensitive identification of sulfonyl-IY81149 and hydroxy-IY81149 from the rat plasma.

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Development of a UPLC-MS/MS method for the therapeutic monitoring of L-asparaginase

  • Jeong, Hyeon-Cheol;Kim, Therasa;Yang, Deok-Hwan;Shin, Kwang-Hee
    • Translational and Clinical Pharmacology
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    • 제26권3호
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    • pp.134-140
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    • 2018
  • This study aimed to develop a UPLC-MS/MS method for determining plasma levels of L-aspartic acid and L-asparagine and the activity of L-asparaginase. L-aspartic acid, L-asparagine, and L-aspartic acid-2,3,3-$d_3$ were extracted from human plasma by protein precipitation with sulfosalicylic acid (30%, v/v). The plasma samples were analyzed using an Imtakt Intrada amino acid analysis column with 25 mM ammonium formate and 0.5% formic acid in acetonitrile as the mobile phase with step gradient method at a flow rate of 0.5 mL/min. The injection volume was $5{\mu}L$, and the total run time was 15 min. Inter- and intra-batch accuracies (%) ranged from 96.62-106.0% for L-aspartic acid and 89.85-104.8%, for L-asparagine, and the coefficient of variation (CV%) did not exceed 7%. The validation results for L-aspartic acid and L-asparagine satisfied the specified criterion, however, the results for L-asparaginase activity assay showed a borderline validity. This study could be a foundation for further development of therapeutic drug monitoring systems using UPLC-MS/MS.

Determination of Eupatilin in Human Plasma by Liquid Chromatography/Electrospray Ionization Tandem Mass Spectrometry

  • Lee, Hye-Won;Ji, Hye-Young;Kim, Hui-Hyun;Kim, Sook-Jin;Kim, Soon-Hoe;Kim, Won-Bae;Lee, Hye-Suk
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2-2
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    • pp.223.2-223.2
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    • 2003
  • A rapid, sensitive and selective liquid chromatography-tandem mass spectrometric (LC/MS/MS) method for the determination of eupatilin in human plasma was developed. Eupatilin and internal standard, (S)-[N-3-(4-(2-(1-methyl-5-tetrazolyl)-pyridine-5-y1)- 3-fluorophenyl)-2-oxo-5-oxazolidinyl]methyl acetamide (DA-7867) were extracted from human plasma by liquid-liquid extraction and analyzed on a phenyl-hexyl column with the mobile phase of acetonitrile-ammonium formate (10 mM, pH 3.0) (60:40, v/v). (omitted)

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Chromatographic Analysis of Cilostazol in Human Plasma with On-Line Column Switching

  • Park, Young-Joon;Park, Kyung-Mi;Eunmi Ban;Chun, Soo-Kyung;Kim, Yang-Bae;Kim, Chong-Kook
    • 한국응용약물학회:학술대회논문집
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    • 한국응용약물학회 2002년도 창립10주년기념 및 국립독성연구원 의약품동등성평가부서 신설기념 국재학술대회:생물학적 동등성과 의약품 개발 전략을 위한 국제심포지움
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    • pp.207-207
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    • 2002
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