• 中国精品科技期刊
  • 中国高校百佳科技期刊
  • 中国中文核心期刊
  • 中国科学引文数据库核心期刊
Advanced Search
DING Xiying, JI Xiaolong, LI Bo, MAO Baiyang, YAN Fang, DI Bin. Determination of potential genotoxic impurity in ecabet sodium active pharmaceutical ingredient by HPLC-MS/MS[J]. Journal of China Pharmaceutical University, 2018, 49(3): 317-321. DOI: 10.11665/j.issn.1000-5048.20180310
Citation: DING Xiying, JI Xiaolong, LI Bo, MAO Baiyang, YAN Fang, DI Bin. Determination of potential genotoxic impurity in ecabet sodium active pharmaceutical ingredient by HPLC-MS/MS[J]. Journal of China Pharmaceutical University, 2018, 49(3): 317-321. DOI: 10.11665/j.issn.1000-5048.20180310
shu

Determination of potential genotoxic impurity in ecabet sodium active pharmaceutical ingredient by HPLC-MS/MS

More Information
    Graphical Abstract
    • Abstract
  • To develop a sensitive analytical method for the determination of the genotoxic impurity mono ethyl ester of ecabet(Imp-I), an HPLC-MS/MS technique was employed. Imp-I was synthesized according to the previous literatures. MS/MS and NMR were used to confirm the structure of Imp-I. A Thermo C18 column was used for chromatographic separations. The mobile phase consisting of A: 5 mmol/L ammonium acetate(pH adjusted to 3. 0 with formic acid)and B: acetonitrile, with a gradient program: 0 min 50%B, 4 min 50%B, 12 min 80%B, 16 min 80%B, 16. 1 min 50%B and 20 min 50%B. The column was maintained at 40 °C throughout the analysis. All measurements were carried out with the mass spectrometer operated under the negative ESI mode. The selective reaction monitor(SRM)transition was used. Good linearity was obtained for Imp-I over the concentration range of 4- 150 ng/mL with the coefficient of determination(r)of 0. 999. And the LOQ was 4 ng/mL. A rapid and sensitive HPLC-ESI-MS/MS method was developed for quantitative analysis of Imp-I in ecabet sodium APIs. This method can be of used for quality assurance of ecabet sodium in bulk commercial drugs.
    • FullText(HTML)
    • References (15)
  • [1]
    Looker AR,Ryan MP,Neubertlangille BJ,et al.Risk assessment of potentially genotoxic impurities within the framework of quality by design[J].Org Process Res Dev,2010,14(4):1032-1036.
    [2]
    Ma L,Ma YN,Chen Z,et al.Structural alerts of genotoxic impurities[J].Chin New Drugs J(中国新药杂志),2014,23(18):2106-2111.
    [3]
    Wu YF,Luan Y,Qi XM,et al.Advance in study on early and rapid assays of genotoxicity[J].Drug Eval Res(药物评价研究),2011,34(4):244-250.
    [4]
    Wang XJ,Ma J.Research advances of new techniques and methods for drug safety evaluation[J].Chin J Pharm(中国医药工业杂志),2017,48(3):341-350.
    [5]
    Wichard JD.In silico prediction of genotoxicity[J].Food Chem Toxicol,2017,106:595-599.
    [6]
    Bhavani KG, Krishna KBM, Srinivasu N, et al. Determination of genotoxic impurity in atazanavir sulphate drug substance by LC-MS[J].J Pharm Biomed Anal,2017,132:156-158.
    [7]
    Wollein U, Schramek N. Simultaneous determination of alkyl mesilates and alkyl besilates in finished drug products by direct injection GC/MS[J].Eur J Pharm Sci,2012,45(1/2):201-204.
    [8]
    Grigori K,Loukas YL,Malenovi'c A,et al.Chemometrically assisted development and validation of LC-MS/MS method for the analysis of potential genotoxic impurities in meropenem active pharmaceutical ingredient[J].J Pharm Biomed Anal,2017,145:307-314.
    [9]
    Zhou J,Xu J,Zheng XY,et al.Determination of methyl methanesulfonate and ethyl methanesulfonate in methanesulfonic acid by derivatization followed by high-performance liquid chromatography with ultraviolet detection[J].J Sep Sci,2017,40(17):3414-3421.
    [10]
    Ito Y,Onoda Y,Nakamura S,et al.Effects of the new anti-ulcer drug ecabet sodium(TA-2711)on pepsin activity.II.Interaction with substrate protein[J].Jpn J Pharmacol,1993,62(2):175-181.
    [11]
    Ito Y,Shibata K,Hongo A,et al.Ecabet sodium,a locally acting antiulcer drug,inhibits urease activity of Helicobacter pylori[J].Eur J Pharmacol,1998,345(2):193-198.
    [12]
    Murata H,Kawano S,Tsuji S,et al.Combination therapy of ecabet sodium and cimetidine compared with cimetidine alone for gastric ulcer:prospective randomized multicenter study[J].J Gastroenterol Hepatol,2003,18(9):1029-1033.
    [13]
    Liu GJ,Pei ZD,Zhang JX,et al.Determination of contents and related substances of ecabet sodium granules by HPLC[J].Chin J Mod Appl Pharm(中国现代应用药学),2012,29(1):70-72.
    [14]
    Zhang D,Du X,Liu M,et al.Determination of ecabet in human plasma by high-performance liquid chromatography-tandem mass spectrometry[J].J Chromatogr B,2008,863(2):223-228.
    [15]
    Ruan XL,Zheng XY,Xu J,et al.Advances in analytical techniques for the determination of genotoxic impurities in pharmaceuticals[J].J China Pharm Univ(中国药科大学学报),2016,47(3):267-274.
    • Related Articles

  • Related Articles

    [1]XU Yuantao, WANG Jundong, GUAN Li, ZHAO Ning, LI Weize. Synthesis and antidiabetic activity evaluation of benzopyrimidine derivatives[J]. Journal of China Pharmaceutical University, 2023, 54(5): 569-576. DOI: 10.11665/j.issn.1000-5048.2023041701
    [2]MEI Yinliu, WU Jie. Application of nanoparticles in wound healing of diabetes[J]. Journal of China Pharmaceutical University, 2022, 53(1): 25-31. DOI: 10.11665/j.issn.1000-5048.20220104
    [3]TAO Yingjun, WU Jie, LIU Chang. Application of proteomics in diabetes and its complications[J]. Journal of China Pharmaceutical University, 2020, 51(3): 368-373. DOI: 10.11665/j.issn.1000-5048.20200315
    [4]LI Yongrong, CHENG Tao, WANG Yongsheng, LI Qin, GAO Bo, HE Yun, BAI Yu. Effect of extract of selenium-enriched Astragalus membranaceus on insulin resistance in streptozotocin-induced diabetic rats[J]. Journal of China Pharmaceutical University, 2018, 49(6): 739-745. DOI: 10.11665/j.issn.1000-5048.20180616
    [5]XU Zhimeng, ZHU Jingjing, JIANG Zhenzhou, LOU Fengchang, WANG Tao. Hypoglycemic effects of terpenes from Fructus Corni on db/db diabetic mice[J]. Journal of China Pharmaceutical University, 2016, 47(3): 337-341. DOI: 10.11665/j.issn.1000-5048.20160315
    [6]HU Mengyue, LIU Can, ZHANG Mian, HU Nan, LIU Li, LIU Xiaodong. Alteration of cytochrome P450s activity under diabetic conditions and its impact on the development of diabetes mellitus[J]. Journal of China Pharmaceutical University, 2014, 45(2): 153-160. DOI: 10.11665/j.issn.1000-5048.20140204
    [7]WANG Xin-ting, ZHANG Mian, GUO Hai-fang, LIU Can, HU Nan, LIU Li, LIU Xiao-dong. Effect and mechanism of atorvastatin on blood glucose of mild diabetic rats[J]. Journal of China Pharmaceutical University, 2012, 43(5): 453-459.
    [8]Effects of Melatonin on the Immune Functions of Diabetic Rats Combined with Injury-induced Stress[J]. Journal of China Pharmaceutical University, 2004, (4): 71-74.
    [9]PREVENTION AND TREATMENT OF ALLOXAN-INDUCED DIABETES IN MICE BY POLYSACCHARIDES ISOLATED RESPECTIVELY FROM BOTH TREMELLA FUCIFORMIS AND AURICULARIA A URICULA[J]. Journal of China Pharmaceutical University, 1989, (3): 181-183.
    [10]PREVENTION AND TREATMENT OF ALLOXAN-INDUCED DIABETES IN MICE BY POLYSACCHARIDES FROM SPORE OF TREMELLA FUCIFORMIS BERK[J]. Journal of China Pharmaceutical University, 1988, (4): 303-304.

  • Cited by

    Periodical cited type(7)

    1. 刘艳，温田田，孙野，陈庆山，张丽莉，匡海学，杨炳友. 白鲜皮化学成分研究. 中成药. 2025(03): 812-821 .
    2. 陈禹竹，徐晓敏，刘树民，卢芳. 白鲜皮及其有效成分的药理作用研究进展. 药物评价研究. 2024(02): 409-418 .
    3. 刘新月，陈乐乐，孙鹏，展照双，王加锋. 白鲜皮化学成分、药理作用和毒性研究进展及质量标志物预测分析. 中国新药杂志. 2023(08): 799-805 .
    4. 牛晨冬，郭丽娜，张金玲，卢宜然，王琳琳，李宗锴. 白鲜属植物化学成分与药理作用研究进展. 中成药. 2022(04): 1231-1238 .
    5. 葛翎，路露，周谦，张秋生，蔡波，黄晓德，张峰伦，钱雪，李海涛，陈斌，曹鹏. 马齿苋醇提物体外生物学活性测定. 中国野生植物资源. 2021(04): 8-14+21 .
    6. 梁郭智，孙淑英. 白鲜研究进展. 时珍国医国药. 2020(02): 408-411 .
    7. 胡玉恒，孙捷，杨洁，王晓静. 3-(4′-苯甲酰基氨基-苯基)-香豆素衍生物的合成及体外降血糖活性. 中国药科大学学报. 2019(02): 168-174 . 本站查看

    Other cited types(4)

Catalog

    Get Citation
    PDF
    XML
    Article views (853) PDF downloads (928) Cited by(11)
    Turn off MathJax
    Article Contents
    Abstract
    References
    Related Articles

    Copyright © Journal of China Pharmaceutical University苏ICP备12050101号-2

    Address：24 Tongjia Lane, Nanjing City, Jiangsu Province （210009）Tel: 025-83271566E-mail: xuebao@cpu.edu.cn

    Supported by: Beijing Renhe Information Technology Co., Ltd.  Baidu Analytics

    Total visits：365847

    /

    DownLoad:  Full-Size Img  PowerPoint
    Return
    Return