期刊文献+

GC-MS法测定甲磺酸萘莫司他中的甲磺酸甲酯与甲磺酸乙酯 被引量:5

Determination of Methylmesylate and Ethylmesylate in Nafamostatmesilate by GC-MS
下载PDF
导出
摘要 建立同时测定甲磺酸萘莫司他原料药中潜在的遗传毒性杂质甲磺酸甲酯和甲磺酸乙酯的测定方法。采用气相色谱-质谱联用法,以甲磺酸异丙酯为内标物质,使用二氯甲烷进行提取。色谱柱为HP-5毛细管柱,柱温采用程序升温,进样口温度为240℃,流速为1.5 mL/min,载气为高纯氦气,检测器为MS检测器,离子源温度为230℃,接口温度为260℃,溶剂延迟时间为2.5min,检测器电压为调谐电压,扫描(检测)方式为选择性离子检测(SIM),电子能量70eV,进样量为1μL。2种杂质之间良好分离,在0.01~0.4μg/mL的浓度范围内线性关系良好,平均回收率分别为90.2%和97.0%,检测限分别为5 ng/mL和3 ng/mL,定量限分别为14.8 ng/mL和7.5 ng/mL。该方法简便、灵敏且准确,可用于甲磺酸萘莫司他中潜在的遗传毒性杂质的测定。 To establish a determination method for the potential genotoxic impurities( methyl methanesulfonate and ethyl methanesulfonate) in nafamostatmesylate. GC-MS was conducted,and the potential genotoxic impurities were extracted by dichloromethane with isopropyl methanesulfonate as internal standard. The column was HP-5 capillary column with programmed temperature,the inlet temperature was 240 ℃,the column flow was 1. 5 mL/min and the carrier gas was high purity helium,the detector was a mass spectrometer detector,the ion source temperature was 230 ℃,the interface temperature was 260 ℃,the delay time of solvent was 2. 5 min,the detector voltage was respect to the tuning results,the scanning( detection) method was selective ion monitoring( SIM),the electron energy was 70 eV,and the injection volume was 1. 0 μL. Methyl mesylate and ethyl mesylate could be separated completely with good linear relationship between 0. 01 - 0. 4μg/mL,the average recoveries were 90. 2% and 97. 0%,the limits of detection were 5 ng/mL and 3 ng/mL,the limits of quantitation were 14. 8 ng/mL and 7. 5 ng/mL. The method is simple,sensitive and accurate,and can be used for the potential genotoxic impurities in nafamostatmesylate.
作者 曹卫 郭彦飞 黄志勇 Cao Wei;Guo Yanei;Huang Zhiyong(Nanjing Heron Pharmaceutical Science Technology Co.,Ltd.,Nanjing 211100,China)
出处 《山东化工》 CAS 2018年第9期53-54,59,共3页 Shandong Chemical Industry
关键词 甲磺酸萘莫司他 遗传毒性杂质 甲磺酸甲酯 甲磺酸乙酯 GC-MS nafamostatmesylate genotoxie impurities methyl methanesulfonate ethyl methanesulfonate GC - MS
  • 相关文献

参考文献1

二级参考文献4

  • 1王晓天,张建宾,金汝城.对胍基苯甲酸盐酸盐的制备及衍生物卡莫他特甲磺酸盐的合成[J].精细化工,2004,21(8):597-599. 被引量:8
  • 2陆美贞.胰腺炎药甲磺酸萘莫司他.国外医药:合成药.生化药.制剂分册,1988,9(4):234-235.
  • 3Takuo A,Toshiyuki O,Toyoo N,et al.Synthesis and structure-activity study of protease inhibitors.Ⅳ.Amidinonaphthols and related acyl derivatives[J].Chem Pharm Bull,1985,33 (4):1458-1471.
  • 4Setsure FT,Toshlynkl OT,Toyoo N,et al.Amidine compound:US,4454338[P].1984-12-01; EP,48433[P].1982-03-31.(CA 1982,97:127298m)

共引文献9

同被引文献77

引证文献5

二级引证文献9

相关作者

内容加载中请稍等...

相关机构

内容加载中请稍等...

相关主题

内容加载中请稍等...

浏览历史

内容加载中请稍等...
;
使用帮助 返回顶部