• Title/Summary/Keyword: acidic pharmaceuticals

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Determination of acidic pharmaceuticals in aquatic environmental samples by LC/ESI-MS/MS (LC/ESI-MS/MS를 이용한 수질 환경 시료 중 산성의약물질 분석방법 비교)

  • Sim, Young-Eun;Cho, Hyun-Woo;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.21 no.3
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    • pp.191-200
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    • 2008
  • Pharmaceuticals and personal care products (PPCPs) are emerging contaminants in aquatic environmental samples. Therefore, it required rapidly and certainly analytical method for pharmaceuticals which are existed in environment. In this study, Liquid chromatography/tandem mass spectrometry (LC-MS/MS) with electrospray ionization (ESI) was used to measure the concentrations of 7 pharmaceuticals (quinoxaline-2-carboxylic acid, acetylsalicylic acid, diclofenac-Na, naproxen, ibuprofen, mefenamic acid, talniflumate) from environmental water or aquatic samples simultaneously. Effective sample clean-up by solid-phase extraction (SPE) prior to LC-MS/MS analysis is necessary. For further purification, Mixed Cation eXchange (MCX) and Hydrophilic-Lipophilic Balance (HLB) solid-phase extraction (SPE) cartridges were used to eliminate the remaining interferences. LODs (Limits of Detection) and MDLs (Method Detection Limits) for the spiked sample in fresh water were in the range of 0.05~1.50 pg/mL and 0.17~4.90 pg/mL, respectively. The absolute recovery in the concentration of 1.0 ng/mL were between 81.9 and 116.3%. The acidic pharmaceuticals were detected in concentrations of 0.018~16.925 ng/mL in aquatic environmental samples.

Application of Capillary Electrophoresis for Quality Control Analysis of Complex Medicine (모세관 전기영동 분석법의 복합약물제제의 품질관리 분석에 응용을 위한 연구)

  • Heo, Yoo-Jeong;Lee, Kong-Joo
    • YAKHAK HOEJI
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    • v.41 no.5
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    • pp.539-546
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    • 1997
  • Capillary electrophoresis (CE) is perceived as an attractive tool for the analysis of pharmaceuticals and biological materials because of their high separation efficiency, easy separation and low running cost. New concept of micellar electrokinetic capillary chromatography (MECC) expanded the application of CE to the separation of neutral molecules. Validation of CE as an analytical technique for quality control of pharmaceuticals should be confirmed by quantitative analysis and the peak confirmation. In this study, the quantitative analyses of various types of neutral, acidic and basic components (acetaminophen, caffeine, ascorbic acid, riboflavin, thiamine, chlorpheniramine, phenylpropanolamine, dl-methylephedrine and dextromethorphan) in complex cold medicines have been accomplished using CE. Combined methods of MECC using SDS and capillary zone electrophoresis lowering the pH of running buffer were adopted to determine the ingredients in capsule type or liquid formula complex medicines without particular sample pretreatment. The results indicate that CE is a promising technique for quality control analysis of pharmaceuticals as a validation method.

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Determination of Retinols in Pharmaceutical Preparations by HPLC (HPLC를 이용한 제제중의 레티놀 유도체 정량)

  • 안문규;문현숙;허문회;김대병;박승희
    • YAKHAK HOEJI
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    • v.45 no.4
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    • pp.352-356
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    • 2001
  • A simple and rapid determination of total retinol from various pharmaceuticals containing retinol derivatives was described. Retinol derivatives were hydrolyzed with alcoholic KOH to alcoholic retinol, which was determined by HPLC. Pretreatments and HPLC conditions depend on the kind of retinols and preparation forms. The total amount of alcoholic retinol could be determined with this method from many pharmaceutical preparation of retinol derivatives. Treating time of KOH, acidic reagents and HPLC conditions were investigated.

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In Vitro Assay of Mammary Gland Tissue Specific hEPO Gene Expression (hEPO 유전자의 유선조직 특이적 발현에 대한 In Vitro 검정)

  • Koo, Bon Chul;Kwon, Mo Sun;Kim, Teoan
    • Reproductive and Developmental Biology
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    • v.40 no.1
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    • pp.7-13
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    • 2016
  • Effectiveness of transgene transfer into genome is crucially concerned in mass production of the bio-pharmaceuticals using genetically modified transgenic animals as a bioreactor. Recently, the mammary gland has been considered as a potential bioreactor for the mass production of the bio-pharmaceuticals, which appears to be capable of appropriate post-translational modifications of recombinant proteins. The mammary gland tissue specific vector system may be helpful in solving serious physiological disturbance problems which have been a major obstacle in successful production of transgenic animals. In this study, to minimize physiological disturbance caused by constitutive over-expression of the exogenous gene, we constructed new retrovirus vector system designed for mammary gland-specific expression of the hEPO gene. Using piggyBac vector system, we designed to express hEPO gene under the control of mammary gland tissue specific and lactogenic hormonal inducible goat ${\beta}$-casein or mouse Whey Acidic Protein (mWAP) promoter. Inducible expression of the hEPO gene was confirmed using RT-PCR and ELISA in the mouse mammary gland cells treated with lactogenic hormone. We expect the vector system may optimize production efficiency of transgenic animal and reduce the risk of global expression of transgene.

Effects of Proto-oncogene Protein DEK on PCAF Localization

  • Lee, In-Seon;Lee, Seok-Cheol;Lee, Jae-Hwi;Seo, Sang-Beom
    • Biomolecules & Therapeutics
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    • v.15 no.2
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    • pp.78-82
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    • 2007
  • The proto-oncogene protein DEK is a nuclear binding phosphoprotein that has been associated with various human diseases including leukemia. Histone acetylation is an important post-translational modification which plays important role in transcriptional regulation. Auto-acetylation of histone acetyltransferase PCAF results in increment of its HAT activity and facilitation of its nuclear localization. In this study, we report that DEK inhibits PCAF auto-acetylation through direct interaction. The C-terminal acidic domains of DEK are responsible for the interaction with PCAF. Using confocal microscopy, we have shown that nuclear localization of PCAF is severely inhibited by DEK. Taken together, our results suggest that DEK may be involved in various cellular signal transduction pathways accommodated by PCAF through the regulation of PCAF auto-acetylation.

Synthesis of SATE Prodrug of 6'-Fluoro-6'-methyl-5'-noradenosine Nucleoside Phosphonic Acid as a New Class of Anti-HIV Agent

  • Li, Hua;Yoo, Jin-Cheol;Baik, Young-Chan;Lee, Won-Jae;Hong, Joon-Hee
    • Bulletin of the Korean Chemical Society
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    • v.31 no.9
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    • pp.2514-2518
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    • 2010
  • A very simple synthetic route of a novel SATE prodrug type of 6'-fluoro-6'-methyl-5'-noradeonosine carbocyclic nucleoside phosphonic acid is described. The key fluorinated alcohol intermediate 7 was prepared from the epoxide intermediate 6a via selective ring-opening of epoxide. Coupling of 7 with $N^6$-bis-Boc-adenine under a Mitsunobu reaction followed by phosphonation and deprotection afforded the carbocyclic phosphonic acid. The chemical stability of the bis(SATE) derivative 13 was measured at neutral (pH 7.2) and slightly acidic (Milli-Q water, pH 5.5) pH. The antiviral activity test of the SATE prodrug 13 and its parent nucleoside phosphonic acid 11 were evaluated against HIV-1.

Determination of N-nitrosodimethylamine in zidovudine using high performance liquid chromatography-tandem mass spectrometry

  • Yujin Lim;Aelim Kim;Yong-Moon Lee;Hwangeui Cho
    • Analytical Science and Technology
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    • v.36 no.6
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    • pp.281-290
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    • 2023
  • Zidovudine is an antiretroviral agent prescribed for the prevention and treatment of human immunodeficiency virus/acquired immune deficiency syndrome (HIV/AIDS). It is typically recommended to be used in combination with other antiretroviral drugs. Zidovudine has the potential to generate N-nitrosodimethylamine (NDMA) in the presence of dimethylamine and nitrite salt under acidic reaction conditions during the drug manufacturing process. NDMA is a potent human carcinogen that may be detected in drug substances or drug products. An analytical method was developed to determine NDMA in pharmaceuticals including zidovudine using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The analysis involved reversed-phase chromatography on a Kinetex F5 column with a mobile phase comprising water-acetonitrile mixtures. The detection of positively charged ions was conducted using atmospheric pressure chemical ionization (APCI). The calibration curve demonstrated excellent linearity (r = 0.9997) across the range of 1-50 ng/mL with a highly sensitive limit of detection (LOD) at 0.3 ng/mL. The developed method underwent thorough validation for specificity, linearity, accuracy, precision, robustness, and system suitability. This sensitive and specific analytical method was applied for detecting NDMA in zidovudine drug substance and its formulation currently available in the market, indicating its suitability for drug quality management purposes.

Chiral Mesoporous Silica for Asymmetric Metal-free Catalysis: Enhancement of Chirality thorough Confinement Space by Plug Effect

  • Jeong, Eun-Yeong;Im, Cheong-Rae;Park, Sang-Eon
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.08a
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    • pp.199-199
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    • 2011
  • The addition of a carbanion to ${\yen}{\acute{a}}{\yen}{\hat{a}}$-unsaturated carbonyl compounds is of importance in the C-C bond formation reactions for modern pharmaceuticals and organic synthesis. Recently, heterogeneous asymmetric catalysis became more attractive area of research because of the easy recovery and separation of the catalyst from the reaction system. Most of synthetic methods for heterogeneous catalysts were grafting or immobilization of homogeneous catalyst onto the solid supports. Trans-1,2-Diaminocyclohexane(DACH) and L-proline ligands have been enormously used as chiral ligands in several catalytic transformation under homogenous conditions. Our group prepared l-proline functionalized mesoporous silica was synthesized under acidic condition using a poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) triblock copolymer template (EO20PO70EO20, Pluronic P-123, BASF). Furthermore, we successfully directly synthesized trans-1,2 diaminocyclohexane functionalized mesoporous silica by using microwave method. The direct functionalization of chiral ligand into the framework of mesoporous materials is expected to be useful for the heterogeneous asymmetric catalysis. So, we adopt the direct synthesis of chiral ligand functionalized mesoporous silica by using thermal and microwave irradiation. Then, chiral ligand functionalized mesoporous silicas were applied to enantioselective asymmetric catalytic reactions.

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