Volume 66 Issue 11
Jan.  2023
Turn off MathJax
Article Contents
WU Xue, BO Meng, SUN Xiaojing, FAN Yanlong, WANG Yajing, DONG Haifeng. Determination of Genotoxic Impurities in Safinamide Mesylate by LC/MS[J]. Metrology Science and Technology, 2022, 66(11): 27-30. doi: 10.12338/j.issn.2096-9015.2021.0632
Citation: WU Xue, BO Meng, SUN Xiaojing, FAN Yanlong, WANG Yajing, DONG Haifeng. Determination of Genotoxic Impurities in Safinamide Mesylate by LC/MS[J]. Metrology Science and Technology, 2022, 66(11): 27-30. doi: 10.12338/j.issn.2096-9015.2021.0632

Determination of Genotoxic Impurities in Safinamide Mesylate by LC/MS

doi: 10.12338/j.issn.2096-9015.2021.0632
  • Accepted Date: 2022-03-31
  • Available Online: 2022-12-01
  • Publish Date: 2023-01-17
  • Safinamide mesylate is mainly used in the treatment of Parkinson's disease. A liquid chromatography-mass spectrometry (LC-MS) method was developed for the determination of genotoxic impurities ((S)-4-((1-amino-1-oxopropane-2-methyl)amino)methyl)benzoate) in safinamide mesylate. The sample was dissolved in methanol, separated by YMC-Triart C18 column (4.6mm×100 mm, 3μm), eluted with 0.1 % formic acid in water and 0.1 % formic acid in methanol gradient, and quantified by positive ion scanning in multiple reaction monitoring (MRM) mode. The method has good specificity, and the target compound has a good linear relationship in the concentration range of 1.53-30.54 ng/mL. Standard recovery rate was 98.5%~99.90% with relative standard deviations of 0.83%~2.10%. The linear response range was between 1.53~30.54 ng/mL (R2 >0.99). The results showed that the method was sensitive, accurate, reliable and suitable for screening of genotoxic impurities ((S) - 4 - ((1-amino-1-oxopropane- 2-methyl) amino) methyl) in safinamide mesylate.
  • loading
  • [1]
    KAKKAR A K, SINGH H, MEDHI B. Old wines in new bottles: Repurposing opportunities for Parkinson’s disease[J]. European Journal of Pharmacology, 2018, 830: 115-127. doi: 10.1016/j.ejphar.2018.04.023
    [2]
    ALDAKHEEL A, KALIA L V, LANG A E. Pathogenesis-targeted, disease modifying therapies in Parkinson disease[J]. Neurotherapeutics, 2014, 11(1): 6-23. doi: 10.1007/s13311-013-0218-1
    [3]
    陈宗元, 黄春丽, 官检发, 等. 帕金森病的流行病学、发病机制及药物的研究进展[J]. 海峡药学, 2018, 30(3): 48-50. doi: 10.3969/j.issn.1006-3765.2018.03.023
    [4]
    SIMONSON W. New drugs for Parkinson’s disease[J]. Geriatric Nursing, 2017, 38: 244-245. doi: 10.1016/j.gerinurse.2017.05.005
    [5]
    CATTANEO C, BARONE P, BONIZZONI E, et al. Effects of safinamide on pain in fluctuating Parkinson’s disease patients: a post-hoc analysis[J]. Journal of Parkinson’s Disease, 2017, 7(1): 95-101. doi: 10.3233/JPD-160911
    [6]
    龙倩, 苑玉和, 张欣, 等. 沙芬酰胺治疗帕金森的研究进展[J]. 中国药理学报, 2019, 35(1): 8-11.
    [7]
    王玲玲, 张阳, 赵倩. 治疗帕金森病新药—沙芬酰胺[J]. 沈阳药科大学学报, 2016, 33(9): 754-758.
    [8]
    CATTANEO C, SARDINA M, BONIZZONI E. Safinamide as add-on therapy to levodopa in mid-to late-stage Parkinson’s disease fluctuating patients: post hoc analyses of studies 016 and SETTLE[J]. Journal of Parkinson’s Disease, 2016, 6(1): 165-173. doi: 10.3233/JPD-150700
    [9]
    杨君义. 一种治疗帕金森病的新型药物—沙芬酰胺[J]. 中国新药与临床杂志, 2016, 35(4): 252-255.
    [10]
    梁瑶, 张蕾, 曾灶昌. 新型抗帕金森病药物沙芬酰胺[J]. 中国新药杂志, 2018(14): 1603-1606.
    [11]
    TEASDALE A. ICH M7: Assessment and control of DNA reactive (mutagenic) impurities in pharmaceuticals to limit potential carcinogenic risk[J]. ICH Quality Guidelines:An Implementation Guide, 2017(1): 667-699.
    [12]
    易可可, 谢洁, 龚晓云, 等. 液相色谱-串联质谱应用研究进展[J]. 计量科学与技术, 2021(2): 7-15,6.
    [13]
    REDASANI V K, MALI B J, SURANA S J. Development and validation of HPTLC method for estimation of safinamide mesylate in bulk and in tablet dosage form[J]. ISRN Analytical Chemistry, 2012(1): 1-4.
    [14]
    陈晓宇, 刘秋叶, 贾少华. 液相色谱法分离测定甲磺酸沙芬酰胺及其有关物质的方法: CN111220715A[P]. 2020-06-02.
    [15]
    刘佳, 邱学艳, 胡素招, 等. 一种沙芬酰胺中甲磺酸异丙酯含量的测定方法: CN109975435A[P]. 2019-07-05.
    [16]
    李蓉, 杨乐婷, 彭雅茹, 等. LC-MS/MS法测定人血浆中沙芬酰胺浓度及其在中国健康人体内的药动学研究[J]. 中国新药杂志, 2019, 28(19): 2375-2379. doi: 10.3969/j.issn.1003-3734.2019.19.013
    [17]
    曹海荣, 薛晓康, 李晓宇. UPLC-MS/MS法测定化妆品中丙烯酰胺的不确定度评定[J]. 计量学报, 2021, 42(8): 1101-1109. doi: 10.3969/j.issn.1000-1158.2021.08.19
    [18]
    邸铮, 贾伯阳, 周荔, 等. 高效液相色谱法测定化妆品中防晒剂奥克立林含量的不确定度评定[J]. 计量学报, 2020, 41(12): 1570-1575. doi: 10.3969/j.issn.1000-1158.2020.12.20
    [19]
    苏福海. 《液相色谱-飞行时间质谱联用仪性能测定方法》国家标准解读[J]. 计量科学与技术, 2020(10): 3-5. doi: 10.3969/j.issn.2096-9015.2020.10.01
  • 加载中

Catalog

    通讯作者: 陈斌, bchen63@163.com
    • 1. 

      沈阳化工大学材料科学与工程学院 沈阳 110142

    1. 本站搜索
    2. 百度学术搜索
    3. 万方数据库搜索
    4. CNKI搜索

    Figures(2)  / Tables(5)

    Article Metrics

    Article views (409) PDF downloads(49) Cited by()
    Proportional views
    Related

    /

    DownLoad:  Full-Size Img  PowerPoint
    Return
    Return