气相色谱-质谱法测定沙格列汀中的3种甲磺酸酯类杂质  

Determination of three methanesulfonate impurities in saxagliptin by GC-MS

作　　者：刘小琼 曹杰永 刘春亮 堵伟锋 LIU Xiao-qiong;CAO Jie-yong;LIU Chun-liang;DU Wei-feng(Anhui Center for Drug Evaluation&Inspection,Hefei 230051;Hefei Cosource Pharmaceuticals Inc.,Hefei 230088;Chuzhou Institute for Food and Drug Control,Chuzhou Anhui 239000;Anhui Institute for Food and Drug Control,Hefei 230051)

机构地区：[1]安徽省药品审评查验中心,合肥230051 [2]合肥合源药业有限公司,合肥230088 [3]滁州市食品药品检验中心,安徽滁州239000 [4]安徽省食品药品检验研究院,合肥230051

出　　处：《中南药学》2022年第9期2151-2154,共4页Central South Pharmacy

摘　　要：目的 建立气相色谱-质谱法检测沙格列汀中的甲磺酸甲酯(杂质1)、甲磺酸乙酯(杂质2)、甲磺酸异丙酯(杂质3)的含量。方法 用CP-SIL 8 CB毛细管色谱柱,以氦气作为载气,应用电子轰击离子化离子源(EI)和离子监测模式(SIM),按照设定的气相色谱-质谱参数运行,对原料药沙格列汀中的3种甲磺酸酯类杂质进行检测。结果 3种甲磺酸酯类在0.1~1.0 μg·mL^(-1)内与峰面积线性关系良好。甲磺酸甲酯的检测限为6.21 ng·mL^(-1),平均回收率在96.51%~98.45%;甲磺酸乙酯的检测限为6.14 ng·mL^(-1),平均回收率在95.21%~98.91%;甲磺酸异丙酯的检测限为6.17 ng·mL^(-1),平均回收率在94.48%~96.45%。结论 该方法具有线性好、检测限低、准确度高等优势,可用于原料药沙格列汀中的3种甲磺酸酯类杂质的检测。Objective To establish a GC-MS method for the simultaneous determination of methyl methanesulfonate,ethyl methanesulfonate and isopropyl methanesulfonate in saxagliptin.Methods The chromatographic column was CP-SIL 8 CB capillary column,and the carrier gas was high-purity helium.The ion source was electron impact ion source.The single ion monitor was used.Results At the concentration of 0.1~1.0 μg·mL^(-1),the three methanesulfonate impurities showed a good linearity.Their average recoveries of methyl methanesulfonate,ethyl methanesulfonate and isopropyl methanesulfonate were 96.51%~98.45%,95.21%~98.91% and 94.48%~96.45%,respectively.The limits of detection were 6.21,6.14,and 6.17 ng·mL^(-1),respectively.Conclusion The method is specific,sensitive and accurate,which can be used for the determination of methanesulfonate impurities in saxagliptin.

关 键 词：气相色谱-质谱 沙格列汀 甲磺酸甲酯 甲磺酸乙酯 甲磺酸异丙酯 

分 类 号：R927[医药卫生—药学]