GC-MS法同时测定阿糖胞苷中四种潜在的硫酸酯类基因毒杂质残留量  

Simutaneous determination of four potential sulfates of genotoxic impurities in cytarabine by GC-MS

作　　者：栗伟娜 牛亚蒙 曹晓绵 张欣娜 褚素霞 LI Weina;NIU Yameng;CAO Xiaomian;ZHANG Xinna;CHU Suxia(CSPC Pharmaceutical Group ZhongQi Pharmacy(Shijiazhuang)Co.Ltd.,State Key Laboratory of Novel Pharmaceutical Preparation and Excipients,Shijiazhuang Hebei 050035,China;Hebei Institute for Drug and Medical Device Control,Shijiazhuang Hebei 050227,China)

机构地区：[1]石药集团中奇制药技术(石家庄)有限公司,新型药物制剂及辅料国家重点实验室,河北石家庄050035 [2]河北省药品医疗器械检验研究院,河北石家庄050227

出　　处：《天津药学》2025年第3期257-261,共5页Tianjin Pharmacy

摘　　要：目的建立阿糖胞苷中四种潜在的硫酸酯类基因毒性杂质(亚硫酸二甲酯、亚硫酸二乙酯、硫酸二甲酯和硫酸二乙酯)残留量的测定方法。方法气相色谱-质谱联用仪(GC-MS),电子轰击离子源(EI),检测器温度为240℃,选择离子监测模式(SIM),毛细管柱为TRACETMTR-V1,规格为60 m×0.25 mm、1.4μm,采用梯度升温,氦气为载气,进样口温度为210℃,并以3∶1的比例分流,使用外标法定量。结果建立了阿糖胞苷中四种潜在的硫酸酯类基因毒性杂质残留量的测定方法。3批阿糖胞苷中四种潜在的硫酸酯类基因毒性杂质均未检出。结论建立的阿糖胞苷中潜在的硫酸酯类基因毒性杂质残留量的测定方法具有较强的专属性、较好的精密度和较高的灵敏度。适用于阿糖胞苷中四种硫酸酯类基因毒杂质的质量控制。Objective To establish a method for determination of potential sulfates of genotoxic impurities(dimethyl sulfite,diethyl sulfite,dimethyl sulfate,and diethyl sulfate)in cytarabine.Methods The method was gas chromatography-mass spectrometry(GC-MS).The ion source was EI source.The detector temperature was 240℃.The acquisition mode was selective ion monitoring(SIM).An TRACETM TR-V1 column(60 m×0.25 mm,1.4μm)was adopted for separation with a injection temperature of 210℃.Helium as used as the carrier gas,and the split ratio was set at 3∶1.The quantity of sulfates of genotoxic impurities by external standard method was calculated.Results A method for determination of four potential sulfates of genotoxic impurities in cytarabine was successfully established.None of these impurities were detected in three batches of cytarabine.Conclusion The method was exclusive,accurate and sensitive,and can be used for the determination of potential sulfates of genotoxic impurities in cytarabine.

关 键 词：气相色谱-质谱联用仪 阿糖胞苷 基因毒性杂质 亚硫酸二甲酯 亚硫酸二乙酯 硫酸二甲酯 硫酸二乙酯 

分 类 号：R917[医药卫生—药物分析学]