气相色谱-质谱法测定帕瑞昔布钠中3种硫酸酯类基因毒性杂质  

Determination of three sulfates genotoxic impurities in Parecoxib sodium by GC-MS

作　　者：崔萍 曹庆丰 丁逸梅 CUI Ping;CAO Qingfeng;DING Yimei(Jiangsu Provincial Institute of Material Medica,Nanjing 211816,China;School of Pharmaceutical Sciences,Nanjing Tech University,Nanjing 211816,China)

机构地区：[1]江苏省药物研究所有限公司,南京211816 [2]南京工业大学药学院,南京211816

出　　处：《化学分析计量》2024年第8期56-61,68,共7页Chemical Analysis And Meterage

摘　　要：建立气相色谱-质谱法检测帕瑞昔布钠原料药及注射用帕瑞昔布钠中硫酸二甲酯、硫酸二乙酯和硫酸二异丙酯。用Thermo TG-5MS毛细管色谱柱(30 m×0.25 mm,0.25μm)分离,载气为氦气,质谱离子源为电子轰击离子源,采集模式为定时选择性离子监测。3种硫酸酯质量浓度在各自范围内与色谱峰面积线性关系良好,相关系数均大于0.995,平均回收率为95.60%~107.3%,测定结果的相对标准偏差均小于5%(n=6),检出限为20.50~21.88 ng/mL,定量限为61.50~65.64 ng/mL。该法可用于帕瑞昔布钠原料药及注射用帕瑞昔布钠中3种硫酸酯类基因毒性杂质的检测。A method for determining dimethyl Sulfate,diethyl sulfate and diisopropyl sulfate in Parecoxib sodium and Parecoxib sodium for injection was established by gas chromatography-mass spectrometry.The separation was performed on a Thermo TG-5MS(30 m×0.25 mm,0.25μm)capillary column with helium as carrier gas,the detection was performed with electron impact(EI)ion source,the acquisition mode was timed-selective ion monitoring(T-SIM).The mass concentrations of the three types of sulfates showed good linearity with the chromatographic peak area within their respective ranges,the correlation coefficients were all more than 0.995,the average recoveries were 95.60%-107.3%,the relative standard deviations of the measurement results were less than 5%(n=6),the limits of detection were 20.50-21.88 ng/mL,the limits of quantification were 61.50-65.64 ng/mL.This method can be used for the determination of sulfates genotoxic impurities in Parecoxib sodium and Parecoxib sodium for injection.

关 键 词：气相色谱-质谱法 帕瑞昔布钠 注射用帕瑞昔布钠 硫酸酯类 基因毒杂质 

分 类 号：O657.7[理学—分析化学]