• Title/Summary/Keyword: Bioanalysis

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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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    • v.22 no.2
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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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Simultaneous Determination of α-Amanitin and β-Amanitin in Mouse Plasma Using Liquid Chromatography-High Resolution Mass Spectrometry

  • Bang, Young Yoon;Lee, Min Seo;Lim, Chang Ho;Lee, Hye Suk
    • Mass Spectrometry Letters
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    • v.12 no.3
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    • pp.112-117
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    • 2021
  • α-Amanitin and β-amanitin are highly toxic bicyclic octapeptides responsible for the poisoning of poisonous mushrooms such as Amanita, Galerina, and Lepiota by inhibiting RNA polymerase II, DNA transcription, and protein synthesis. A sensitive, simple, and selective liquid chromatography-high resolution mass spectrometric method using parallel reaction monitoring mode was developed and validated for the simultaneous determination of α- and β-amanitin in mouse plasma to evaluate the toxicokinetics of α- and β-amanitin in mice. Protein precipitation of 5 μL mouse plasma sample with methanol as sample clean-up procedure and use of negative electrospray ionization resulted in better sensitivity and less matrix effect. The calibration curves for α- and β-amanitin in mouse plasma were linear over the range of 0.5-500 ng/mL. The intra- and inter-day coefficient of variations and accuracies for α- and β-amanitin at four quality control concentrations were 3.1-14.6% and 92.5-115.0%, respectively. The present method was successfully applied to the toxicokinetic study of α- and β-amanitin after an oral administration of α- and β-amanitin at 1.5 mg/kg dose to male ICR mice.

Quantification of Fargesin in Mouse Plasma Using Liquid Chromatography-High Resolution Mass Spectrometry: Application to Pharmacokinetics of Fargesin in Mice

  • Lee, Min Seo;Lim, Chang Ho;Bang, Young Yoon;Lee, Hye Suk
    • Mass Spectrometry Letters
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    • v.13 no.1
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    • pp.20-25
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    • 2022
  • Fargesin, a tetrahydrofurofuranoid lignan isolated from Flos Magnoliae, shows anti-inflammatory, anti-oxidative, anti-allergic, and anti-hypertensive activities. To evaluate the pharmacokinetics of fargesin in mice, a sensitive, simple, and selective liquid chromatography-high resolution mass spectrometric method using electrospray ionization and parallel reaction monitoring mode was developed and validated for the quantification of fargesin in mouse plasma. Protein precipitation of 6 µL mouse plasma with methanol was used as sample clean-up procedure. The standard curve was linear over the range of 0.2-500 ng/mL in mouse plasma with the lower limit of quantification level at 0.2 ng/mL. The intra- and inter-day coefficient variations and accuracies for fargesin at four quality control concentrations including were 3.6-11.3% and 90.0-106.6%, respectively. Intravenously injected fargesin disappeared rapidly from the plasma with high clearance values (53.2-55.5 mL/min/kg) at 1, 2, and 4 mg/kg doses. Absolute bioavailability of fargesin was 4.1-9.6% after oral administration of fargesin at doses of 1, 2, and 4 mg/kg to mice.

Profiling Analysis of Sphingolipids in HL-60 Cells by High-Performance Liquid Chromatography-Tandem Mass Spectrometry in combination with Multiple Reaction Monitoring

  • Son, Jung-Hyun;Lee, Jae-Ick;Yang, Ryung;Kim, Dong-Hyun
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.288.3-289
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    • 2003
  • Sphingolipid species are important second messengers due to their role in the mitogenesis, differentiation and apoptosis. We developed a new column liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS) in combination with multiple reaction monitoring (MRM) method for the rapid, simultaneous and quantitative determination of unambiguous detecting sphingolipids in cell culture of human cancer cells (HL-60). (omitted)

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Simultaneous quantitation of enalapril and enalaprilat in human plasma by high-throughput solid phase extraction and liquid chromatography/tandem mass spectrometry

  • Son, Jung-Hyun;Lee, Jae-Ick;Kim, Dong-Hyun
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.401.3-402
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    • 2002
  • Enalapril (ENP) maleate is effective drug for the treatment of renivascular hypertension and heart failure. ENP acts as inhibitor of the enzyme angiotensin-convertase (ACE-inhibitor) and metabolized to enalaprilat (ENPT), which is the active metabolite that is really responsible for the therapeutic action. In the present study, a sensitive and rapid liquid chromatography/ electrospray ion trap tandem mass spectrometry (LC/MS/MS) method combined with high-throughput solid phase extraction (SPE) has been developed and validated for the simultaneous quantitative determination of ENP and ENPT in human plasma. (omitted)

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Inhibition of Angiogenesis by Propolis

  • Song, Yun-Seon;Park, Eun-Hee;Jung, Kyung-Ja;Jin, Changbae
    • Archives of Pharmacal Research
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    • v.25 no.4
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    • pp.500-504
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    • 2002
  • Propolis, obtained from honeybee hives, has been used in Oriental folk medicine as an anti-inflammatory, anti-carcinogenic, and immunomodulatory agent. There is considerable evidence suggesting that angiogenesis and chronic inflammation are codependent. Blockage of angiogenesis results in an anti-inflammatory effect. Ethanol (EEP) and ether extracts of propolis (REP), and caffeic acid phenethyl ester (CAPE), an active component of propolis, were examined for their anti-angiogenic activities using the chick embryo chorioallantoic membrane (CAM), and the calf pulmonary arterial endothelial (CPAE) cell proliferation, assays. The presence of EEP, REP and CAPE inhibited angiogenesis in the CAM assay and the proliferation of CPAE cells. The results suggest that anti-angiogenic activities of EEP, REP and CAPE are also responsible for their anti-inflammatory effect.

Assay of Human Chorionic Gonadotropin in Urine of Athletes and Evaluation of Assay Kit Performance

  • Lee, Jung-Ran;Kim, Myung-Soo;Choi, Myung-Ja
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.406.2-406.2
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    • 2002
  • Special attention has been paid to human chorionic gonadotropin (hCG) for athlete doping control because it stimulates the endogenous production of testosterone and epitestosterone without increasing the T/E ratio which is a doping indicator for the exogenous administration of testosterone. Even though the IOC banned the use of hCG. a detection method has not been decided upon since there are a variety of immunoassay kits available on the market. We evaluated three kits in terms af their performance characteristics. (omitted)

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IN VIVO METABOLISM OF 2-METHYLAMINOETHYL-4,4'-DIMETHOXY-5,6,5',6'-DIMETHYLENEDIOXYBIPHENYL-2'-CARBOXY-2-CARBOXYLATE (DDB-S) BY LC/ESI TANDEM MASS SPECTROMETRY

  • Son, Jung-Hyun;Lee, Jae-Ick;Yang, Ryung;Kim, Dong-Hyun
    • Proceedings of the PSK Conference
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    • 2002.10a
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    • pp.251.2-251.2
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    • 2002
  • 2-Methylaminoethyl- 4,4' -dimethoxy- 5, 5',6,6' -dimethylenedioxybiphenyl- 2' -carboxy- 2-carboxylate (DDB-S) is a synthetic compound derived from DDB. which is protects liver against carbon tetrachloride-, D-galactosamine-, thioacetamine-, and prednisolone- induced hepatic injury in experimental animals. We assessed the use of liquid chromatography/electrospray iontrap tandem mass spectrometry (LC/MS/MS) method to identify and quantify in vivo metabolites and to measure excretion. (omitted)

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Electrospray ionization tandem mass fragmentation pattern of camostat and its degradation product, 4-(4-guanidinobenzoyloxy)phenylacetic acid (Camostat 및 분해산물 4-(4-guanidinobenzoyloxy)phenylacetic acid의 전자분무 이온화 텐덤 질량 fragmentation 패턴)

  • Kwon, Soon-Ho;Shin, Hye-Jin;Park, Ji-Myeong;Lee, Kyoung-Ryul;Kim, Young-Jin;Lee, Sang-Hoo
    • Analytical Science and Technology
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    • v.24 no.2
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    • pp.78-84
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    • 2011
  • The fragmentation patterns of a serine protease inhibitor, camostat, and its degradation product, 4-(4-guanidinobenzoyloxy)phenylacetic acid (GBPA), were for the first time investigated by a triple quadrupole tandem mass spectrometry equipped with an electrospray source (ESI-MS/MS) in positive and/or negative ion mode under collision-induced dissociation (CID). The positive CID spectrum of camostat showed distinctly that the single bond (C-O) cleavage between carbonyl group and oxygen atom of the ester bonds of the compound favorably occurred and then the loss of N,N-dimethylcarbamoylmethyl group was more susceptible than that of guanidine moiety. In the positive ion CID spectrum of GBPA, the initial cleavage between the carbonyl group and oxygen atom of 4-guanidinobenzoyloxy group also occurred, yielding the most abundant fragment ion at m/z 145. On the other hand, the negative CID spectrum of GBPA characteristically showed the occurrence of the most abundant peak at m/z 226 resulting from the sequential neutral losses of $CO_2$ and HN=C=NH from the parent ion at m/z 312.