顶空+GCMS法检测甲磺酸盐类原料药中甲磺酸烷基酯类杂质  

Determination of alkyl methanesulfonate impurities in methanesulfonate raw materials by GCMSMS combined with headspace injection

作　　者：高洁 田菲菲 李月琪 范军 黄涛宏 GAO Jie;TIAN Feifei;LI Yueqi;FAN Jun;HUANG Taohong(Shimadzu(China)Co.,ltd,Beijing Branch,Beijing,100020,China;Shimadzu(China)Co.,ltd,Shanghai Branch,Shanghai,200233,China)

机构地区：[1]岛津企业管理(中国)有限公司北京分公司,北京100020 [2]岛津企业管理(中国)有限公司上海分公司,上海200233

出　　处：《环境化学》2021年第6期1933-1936,共4页Environmental Chemistry

摘　　要：本文使用岛津公司GCMS-QP2020 NX气质联用仪结合顶空HS-20进样建立了一种检测甲磺酸盐类原料药中甲磺酸甲酯、甲磺酸乙酯、甲磺酸异丙酯与甲磺酸丙酯四种甲磺酸烷基酯杂质的方法.在浓度范围1.0-125 ng线性关系良好,相关系数R2均在0.9999以上,方法检出限(LOD)在0.01-0.10 ng之间.平行检测6份5.0 ng标液,峰面积RSD在2.52%-3.39%之间.使用此方法检测甲磺酸倍他司汀原料药,样品检测出甲磺酸甲酯、甲磺酸乙酯与甲磺酸异丙酯.在此样品中加标5.0 ng与12.5 ng,平均回收率在92.8%-105.4%之间.该方法简单方便,可以很好的满足甲磺酸盐类原料药中甲磺酸烷基酯类杂质的检测.A method for the determination of four alkyl methanesulfonate impurities in methanesulfonate raw materials was established by using Shimadzu GCMS-QP2020 NX combined with headspace injection.In the concentration range of 1.0-125 ng,the linear relationship was good,the correlation coefficient R2 was above 0.9999,and the detection limit(LOD)was between 0.01-0.10 ng.The RSD of the peak area was between 2.52%and 3.39%.Methyl methanesulfonate,ethyl methanesulfonate and isopropyl mesylate were detected in Betahistine mesylate.The average recoveries of 5.0 ng and 12.5 ng were 92.8%-105.4%.The method is simple and convenient,and can meet the requirements of detection of alkyl methanesulfonate impurities in methanesulfonate raw materials.

关 键 词：GCMS-QP2020NX 甲磺酸盐类原料药 甲磺酸烷基酯 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]