GC-MS测定醋酸卡泊芬净中三氟甲磺酸甲酯与三氟甲磺酸乙酯  

Determination of Meethyl Trifluoromethanesulfonate and Ethyl Trifluoromethanesulfonate in Caspofungin Acetate by GC-MS

作　　者：张晓玲 胡中元 陈婷 俞海荣 ZHANG Xiao-ling;HU Zhong-yuan;CHEN Ting;YU Hai-rong(Research Institute of Chia Tai Tianqing Pharmaceutical Co.,Ltd.,Nanjing 210000,China)

机构地区：[1]正大天晴药业集团股份有限公司研究院,江苏南京210000

出　　处：《精细化工中间体》2025年第1期79-83,共5页Fine Chemical Intermediates

摘　　要：建立了一种气相色谱-质谱联用法(GC-MS)同时测定醋酸卡泊芬净中三氟甲磺酸甲酯与三氟甲磺酸乙酯的方法。方法以6%氰丙基苯基-94%二甲基聚硅氧烷为固定相的毛细管柱进行检测,三氟甲磺酸甲酯与三氟甲磺酸乙酯可完全分离。起始温度40℃,维持10 min,以15℃/min的速率升温至200℃,维持5 min。进样口温度200℃,载气为氦气,柱流速1.5 mL/min,分流比5∶1,进样体积1μL,采集模式为选择离子监测(SIM),离子源温度200℃。通过外标法进行计算,结果显示,三氟甲磺酸甲酯与三氟甲磺酸乙酯分别在0.51~3.03、0.50~3.02μg/mL浓度范围内与峰面积呈良好线性关系。三氟甲磺酸甲酯的定量限、检测限为0.54、0.15μg/mL,三氟甲磺酸乙酯的定量限、检测限为0.17、0.06μg/mL。三氟甲磺酸甲酯与三氟甲磺酸乙酯的平均回收率为85.93%和100.48%,相对标准偏差为4.8%和3.0%。方法专属性强、灵敏度高、准确性好,适用于醋酸卡泊芬净中三氟甲磺酸甲酯与三氟甲磺酸乙酯的检测。GC-MS method was established for the determination of methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate in Caspofungin Acetate.The method was performed on 6% cyanopropylbenzene and 94%dimethylsiloxane capillary column,methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate could be completely separated.The initial column temperature is set to 40 ℃,maintained for 10 minutes,raised to 200 ℃ at15 ℃/min,maintained for 5 minutes.The injection port temperature is set at 200 ℃,The carrier gas is helium,the column flow rate is 1.5 mL/min,the split ratio is 5∶1,injection volume is 1 μL,the acquisition mode was selected ion monitoring(SIM) with an ion source temperature of 200 ℃.The results showed that methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate could be completely separated by external standard method.Methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate showed a good linear relationship with the peak area in the concentration range of 0.51~3.03 μg/mL and 0.50~3.02 μg/mL.The limit of quantification and detection were0.54 μg/mL and 0.15 μg/mL for methyl trifluoromethanesulfonate,and 0.17 μg/mL and 0.06 μg/mL for ethyl trifluoromethanesulfonate,respectively.The average recoveries of methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate were 85.93% and 100.48%,and the relative standard deviations were 4.8% and 3.0%.The method has the advantages of strong specificity,high detection sensitivity,accurate.It can be used for the determination of methyl trifluoromethanesulfonate and ethyl trifluoromethanesulfonate in Caspofungin Acetate.

关 键 词：醋酸卡泊芬净 三氟甲磺酸甲酯 三氟甲磺酸乙酯 气相色谱-质谱联用法 

分 类 号：TQ460.7[化学工程—制药化工]