不同检测器-顶空气相色谱法测定甲磺酸达比加群酯中的甲磺酸乙酯和甲磺酸异丙酯
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摘要
建立了顶空气相色谱法(HS-GC)测定甲磺酸达比加群酯中的甲磺酸乙酯和甲磺酸异丙酯,对比研究了不同检测器,即氢火焰离子检测器(FID)、电子捕获检测器(ECD)和质谱检测器(MS),主要从灵敏度、空白干扰性和样品测定等方面进行详细比较与评价,以期为不同品种药物活性成分(APIs)中甲磺酸酯含量测定方法的建立提供参考。
ABSTARACT:Headspace GC methods with different detectors were established and compared for the determination of ethyl and isopropyl methanesulfonate in dabigatran etexilate mesylate,including FID,ECD and MS detectors.Detailed comparisons and evaluations were conducted mainly from the sensitivity,interference and sample determination,in order to provide a reference for the establishment of determination methods for methanesulfonates in different APIs.
ABSTARACT:Headspace GC methods with different detectors were established and compared for the determination of ethyl and isopropyl methanesulfonate in dabigatran etexilate mesylate,including FID,ECD and MS detectors.Detailed comparisons and evaluations were conducted mainly from the sensitivity,interference and sample determination,in order to provide a reference for the establishment of determination methods for methanesulfonates in different APIs.
引文
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[12]张萌萌,潘红娟,陈佳,等.盐酸达泊西汀中甲磺酸甲酯、甲磺酸乙酯及甲磺酸异丙酯的顶空毛细管GC-ECD法测定[J].中国医药工业杂志,2015,46(1):55-58.
[2]宫平,贾薇.新型口服抗凝血药物达比加群酯[J].世界临床药物,2008,29(9):544-547.
[3]Jayaraman VR,Patel S,Mistry S,et al.An improved process for the preparation of dabigatran etexilate mesylate:WO,2014020555[P].2014-02-06.
[4]Elder DP,Teasdale A,Lipczynski AM.Control and analysis of alkyl esters of alkyl and arylsulfonic acids in novel active pharmaceutical ingredients(APIs)[J].J Pharm Biomed Anal,2008,46(1):1-8.
[5]Bolt HM,Foth H,Hengstler JG,et al.Carcinogenicity categorization of chemicals-new aspects to be considered in a European perspective[J].Toxicol Lett,2004,151(1):29-41.
[6]European Medicines Agency.CPMP/SWP/5199/02,EMEA/CHMP/QMP/251344/2006.Evaluation of medicines for human use,guideline on the limit of genotoxic impurities[S].2006.
[7]European Medicines Agency.EMEA/CHMP/SWP/431994/2007.Pre-authorisation evaluation of medicines for human use,question&answers on the CHMP guideline on the limits of genotoxic impurities[S].2008.
[8]U.S.Department of Health and Human Services Food and Drug Administration.Guidance for industry:genotoxic and carcinogenic impurities in drug substances and products:recommended approaches(draft guideline)[S].2008.
[9]张园园,李银峰,王杰晶,等.药物中痕量磺酸酯类物质的检测技术研究进展[J].药物评价研究,2012,35(4):304-306.
[10]Lee CR,Guivarch F,van Dau CN,et al.Determination of polar alkylating agents as thiocyanate/isothiocyanate derivatives by reaction headspace gas chromatography[J].Analyst,2003,128(7):857-863.
[11]连小刚,李孝壁,程红艳.衍生气相色谱法测定甲磺酸伊马替尼中甲磺酸烷基酯类[J].中国医药科学,2013,3(17):128-130.
[12]张萌萌,潘红娟,陈佳,等.盐酸达泊西汀中甲磺酸甲酯、甲磺酸乙酯及甲磺酸异丙酯的顶空毛细管GC-ECD法测定[J].中国医药工业杂志,2015,46(1):55-58.