• Title/Summary/Keyword: Pharmaceutical analysis

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Determination of Thiamine in Pharmaceutical Preparations by Reverse Phase Liquid Chromatography Without Use of Organic Solvent

  • Suh, Joon Hyuk;Kim, Junghyun;Jung, Juhee;Kim, Kyunghyun;Lee, Seul Gi;Cho, Hyun-Deok;Jung, Yura;Han, Sang Beom
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1745-1750
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    • 2013
  • A novel green aqueous mobile phase modified with room temperature ionic liquids (RTILs) was employed in the absence of volatile organic solvents or ion-pairing reagents to analyze thiamine, a very polar compound, by reverse phase high performance liquid chromatography (RP-HPLC). Due to its strongly hydrophilic nature, thiamine was eluted near the column dead time ($t_0$) using a mobile phase without adding RTILs or ion-pairing reagents, even if a 100% aqueous mobile phase, which has weak elution power under reverse phase conditions, was used. Thus, 1-ethyl-3-methyl-imidazolium hexafluorophosphate ([EMIM][$PF_6$]), which has the strongest chaotropic effect, was selected as a mobile phase additive to improve retention and avoid baseline disturbances at $t_0$. Various mobile phase parameters such as cation moiety, chaotropic anion moiety, pH and concentration of RTILs were optimized to determine thiamine at the proper retention time. Method validation was performed to assess linearity, intra- and inter-day accuracy and precision, recovery and repeatability; all results were found to be satisfactory. The developed method was also compared to the current official United States Pharmacopoeia (USP) and Korean Pharmacopoeia (KP) methods using an organic mobile phase containing an ionpairing reagent by means of evaluating various chromatographic parameters such as the capacity factor, theoretical plate number, peak asymmetry and tailing factor. The results indicated that the proposed method exhibited better efficiency of thiamine analysis than the official methods, and it was successfully applied to quantify thiamine in pharmaceutical preparations.

An Analysis on the Determinants of Efficiency of the Pharmaceutical Firms using Stochastic Frontier Analysis (Stochastic Frontier Analysis를 이용한 제약회사의 효율성과 그 결정요인분석)

  • Sakong, Jin;Kim, Jeongkyu
    • Health Policy and Management
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    • v.25 no.2
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    • pp.97-106
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    • 2015
  • Background & Methods: The purpose of this research is to estimate the efficiency of the pharmaceutical firms and the determinants of their efficiency. Stochastic frontier analysis(SFA) and panel study are applied to the data of 60 domestic pharmaceutical firms from 2006 to 2012. Results & Conclusion: First, the result of the stochastic frontier analysis shows that overall efficiency of the pharmaceutical firms is increasing as time goes by. However, if firms are classified by the scale, the larger firms show more efficiency and if classified by the degree of innovativeness, the innovative firms show more efficiency compared to the non-innovative firms. This evidences show that the scale and R&D investment have significant relationships with the efficiency of the pharmaceutical firms. Therefore, it is necessary to increase the national level of investment for the fundamental researches to vitalize R&D of the new drugs. Second, the result of estimation of the determinants of efficiency shows that the firms with larger sales promotion expenses and entertainment expenses have less efficiency compared to the other firms. This can be explained by the structural characteristics of the small generic pharmaceutical firms. Therefore, the government had better make the pharmaceutical firms to reduce sales promotion and entertainment expenses and increase R&D expenses by introducing systems such as global budgeting system on medicine or reference pricing system.

Inhibition of matrix metalloproteinases: a troubleshooting for dentin adhesion

  • de Moraes, Izadora Quintela Souza;do Nascimento, Ticiano Gomes;da Silva, Antonio Thomas;de Lira, Lilian Maria Santos Silva;Parolia, Abhishek;de Moraes Porto, Isabel Cristina Celerino
    • Restorative Dentistry and Endodontics
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    • v.45 no.3
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    • pp.31.1-31.20
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    • 2020
  • Matrix metalloproteinases (MMPs) are enzymes that can degrade collagen in hybrid layer and reduce the longevity of adhesive restorations. As scientific understanding of the MMPs has advanced, useful strategies focusing on preventing these enzymes' actions by MMP inhibitors have quickly developed in many medical fields. However, in restorative dentistry, it is still not well established. This paper is an overview of the strategies to inhibit MMPs that can achieve a long-lasting material-tooth adhesion. Literature search was performed comprehensively using the electronic databases: PubMed, ScienceDirect and Scopus including articles from May 2007 to December 2019 and the main search terms were "matrix metalloproteinases", "collagen", and "dentin" and "hybrid layer". MMPs typical structure consists of several distinct domains. MMP inhibitors can be divided into 2 main groups: synthetic (synthetic-peptides, non-peptide molecules and compounds, tetracyclines, metallic ions, and others) and natural bioactive inhibitors mainly flavonoids. Selective inhibitors of MMPs promise to be the future for specific targeting of preventing dentin proteolysis. The knowledge about MMPs functionality should be considered to synthesize drugs capable to efficiently and selectively block MMPs chemical routes targeting their inactivation in order to overcome the current limitations of the therapeutic use of MMPs inhibitors, i.e., easy clinical application and long-lasting effect.

LC-MS/MS-based Quantification of Ten Neurotransmitters in Rat Limbic System and Serum: Application to Chronic Unpredictable Mild Stress-Induced Depression Rats

  • Mingyan Ma;Qiangxiang Chen;Wen Cao;Yubo Zhou;Aijuan Yan;Yanru Zhu
    • Mass Spectrometry Letters
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    • v.14 no.3
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    • pp.91-103
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    • 2023
  • As one of the most common mood disorders, numerous studies have shown depression is the main risk factor for non-suicidal self-harm. The pathogenesis of depression is complex, and a comprehensive and rapid measurement of monoamine neurotransmitters and their metabolites will be very helpful in understanding the pathogenesis of depression. Therefore, a rapid and sensitive underivatized liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous monitoring of the levels of ten neurotransmitters and their metabolites in rat serum and limbic system and successfully applied to quantify the changes of neurotransmitter levels in chronic unpredictable mild stress-induced rats. The analytes studied were mainly involved in tyrosine metabolism, tryptophan metabolism, and glutamate cycling pathways, which are important in the pathogenesis of depression. It had been verified the method was sensitive and effective, with satisfactory linearity, and met the requirements of biological sample determination. Levels of neurotransmitters in rat serum, hippocampus, amygdala, prefrontal cortex, striatum, and hypothalamus were determined via the method. The results showed serotonin, dopamine, norepinephrine, and their metabolites were decreased, glutamine was increased, and glutamate was disturbed in chronic unpredictable mild stress-induced depression rats. This method provides a new approach to studying the pathogenesis of depression and other neurological disorders.

A Survey on Ochratoxin a Contamination of Commercial Medicinal Herbs in Incheon (인천지역 유통 생약 중 Ochratoxin A 오염실태 조사)

  • Lim, Soo-sun;Joo, Gwang-sig;Choi, Eun-Jeong;Lee, Soo-Yeon;Lim, Yun-sun;Eum, Sun-Ah;Jo, Nam-Kyu;Lee, Sung-Mo
    • Korean Journal of Pharmacognosy
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    • v.48 no.1
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    • pp.56-62
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    • 2017
  • The aim of this study was to screen the contamination by ochratoxin A of mycotoxins in various medicinal herbs. We conducted a survey of ochratoxin A in medicinal herb on the retail market in Incheon in 2016. 116 medicinal herb samples were evaluated for the ochratoxin A contamination. They were analyzed for ochratoxin A using immunoaffinity column and high-performance liquid chromatography(HPLC)-fluorescence detection and the positive samples were confirmed using HPLC-tandem mass spectrometry. Ochratoxin A was detected in 4 medicinal herb samples; the concentrations of ochratoxin A were containing between 20.11 and $372.90{\mu}g/kg$. This study shows that in general, this kind of commodity may be contaminated by mycotoxins. Also this contamination is not limited to only aflatoxin of mycotoxins.

Construction of Database and Analysis of Specifications of Pharmaceutical Agents Listed in Korean Compendiums

  • Cho, Jung-Hwan
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.221.2-221.2
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    • 2003
  • Several Compendia are effective in relation with production and supply of pharmaceutical agents in Korea. Those compendia exists only in printed documents, which are not suitable for the analysis of their contents and inter-relationship among them when they have specifications on the same or related pharmaceutical agents. For the analysis of contents of Korean compendia, database system is desinged and all of the available data are entered into relational database system. Every specification was analyzed into several database tables, fields and relations between tables. (omitted)

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Discrimination between Artemisia princeps and Artemisia capillaris Based on Near Infrared Spectroscopy Combined Multivariate Analysis

  • Lee, Dong-Young;Jeon, Min-Ji;Suh, Young-Bae;Kim, Seung-Hyun;Kim, Young-Choong;Sung, Sang-Hyun
    • Journal of Pharmaceutical Investigation
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    • v.41 no.6
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    • pp.377-380
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    • 2011
  • The Artemisia princeps (Compositae) has been used in traditional Korean medicine for the treatment of microbial infections and inflammatory diseases. Since A. princeps is generally difficult to be discriminated from A. capillaris, A. caplillaris has been misused in place of A. princeps. To solve this problem, a rapid and nondestructive method for discrimination of A. princeps and A. capillaris samples was developed using near infrared spectroscopy (NIRS) in the present study. A principal component analysis (PCA) and a partial least squares discrimination analysis (PLS-DA) were performed to discriminate two species. As a result, with the use of PLS-DA, A. princeps and A. capillaris were clustered according to their genus. These outcomes indicated that the NIRS could be useful for the discrimination between Artemisia princeps and Artemisia capillaris.

Tentative identification of 20(S)-protopanaxadiol metabolites in human plasma and urine using ultra-performance liquid chromatography coupled with triple quadrupole time-of-flight mass spectrometry

  • Ling, Jin;Yu, Yingjia;Long, Jiakun;Li, Yan;Jiang, Jiebing;Wang, Liping;Xu, Changjiang;Duan, Gengli
    • Journal of Ginseng Research
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    • v.43 no.4
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    • pp.539-549
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    • 2019
  • Background: 20(S)-Protopanaxadiol (PPD), the aglycone part of 20(S)-protopanaxadiol ginsenosides, possesses antidepressant activity among many other pharmacological activities. It is currently undergoing clinical trial in China as an antidepressant. Methods: In this study, an ultra-performance liquid chromatography coupled with triple quadrupole time-of-flight mass tandem mass spectrometry method was established to identify the metabolites of PPD in human plasma and urine following oral administration in phase IIa clinical trial. Results: A total of 40 metabolites in human plasma and urine were identified using this method. Four metabolites identified were isolated from rat feces, and two of them were analyzed by NMR to elucidate the exact structures. The structures of isolated compounds were confirmed as (20S,24S)-epoxydammarane-12,23,25-triol-3-one and (20S,24S)-epoxydammarane-3,12,23,25-tetrol. Both compounds were found as metabolites in human for the first time. Upon comparing our findings with the findings of the in vitro study of PPD metabolism in human liver microsomes and human hepatocytes, metabolites with m/z 475.3783 and phase II metabolites were not found in our study whereas metabolites with m/z 505.3530, 523.3641, and 525.3788 were exclusively detected in our experiments. Conclusion: The metabolites identified using ultra-performance liquid chromatography coupled with triple quadrupole time-of-flight mass spectrometry in our study were mostly hydroxylated metabolites. This indicated that PPD was metabolized in human body mainly through phase I hepatic metabolism. The main metabolites are in 20,24-oxide form with multiple hydroxylation sites. Finally, the metabolic pathways of PPD in vivo (human) were proposed based on structural analysis.