GC-MS法同时测定阿糖胞苷中氯甲烷、氯乙烷和2-氯丙烷的残留量
Simutaneous Determination of Methychloride、Ethylchloride and 2-Chloropropane in Cytarabine by GC-MS
张欣娜 1邢倩斌 1栗伟娜 1牛亚蒙 1梁敏1
作者信息
- 1. 石药集团中奇制药技术(石家庄)有限公司 新型药物制剂与辅料国家重点实验室,河北 石家庄 050035
- 折叠
摘要
建立了气相色谱-质谱联用法(GC-MS)测定阿糖胞苷原料中潜在基因毒性杂质氯甲烷、氯乙烷和 2-氯丙烷.采用的色谱柱为TRACETM TR-V1 毛细管柱(60 m×0.25 mm,1.4 μm),采用程序升温方式,在选择性离子检测(SIM)模式下,氯甲烷m/z为 50,氯乙烷m/z为 64,2-氯丙烷m/z为 78,采用外标法进行定量.载气为氦气,顶空瓶平衡温度 60℃,平衡时间 30 min,进样口温度 100℃,分流进样,分流比 4∶1.结果表明,氯甲烷、氯乙烷和 2-氯丙烷分别在 125～1000、125～1000 和128～1025 ng/mL范围内线性关系良好(r≥0.999),检测限分别为 37.5、37.5 和 38.4 ng/mL,定量限分别为 125、125 和 128 ng/mL,回收率均在 90.8%～104.8%范围内.建立的GC-MS测定方法专属、准确、灵敏,可用于阿糖胞苷原料药中氯甲烷、氯乙烷和 2-氯丙烷残留量的同时测定.
Abstract
A gas chromatography-mass spectrometry(GC-MS)method was established for the determination of potentially genotoxic impurities such as chloromethane,chloroethane and 2-chloropropane in cytarabine raw materials.TRACETM TR-V1 capillary column(60 m×0.25 mm,1.4 μm)was used.Adopt programmed temperature rise mode,in the mode of selective ion detection(SIM),the m/z of chloromethane was 50,the m/z of chloroethane was 64,and the m/z of 2-chloropropane was 78.The external standard method was used for quantification.The carrier gas is helium,the equilibrium temperature of the headspace bottle is 60℃,the equilibrium time is 30 min,the temperature of the injection port is 100℃,and the split injection is carried out with a split ratio of 4∶1.The results showed that the linear relationships of chloromethane,chloroethane and 2-chloropropane were good in the ranges of 125～1000 ng/mL,125～1000 ng/mL and 128～1025 ng/mL,respectively(r≥0.999).The detection limits were 37.5,37.5 and 38.4 ng/mL,respectively.The quantitative limits were 125,125 and 128 ng/mL,respectively.The recovery rates are all in the range of 90.8%～104.8%.The established GC-MS method is exclusive,accurate and sensitive,and can be used for the determination of chloromethane,chloroethane and 2-chloropropane residues in cytarabine raw materials.
关键词
气相色谱-质谱联用/阿糖胞苷/氯甲烷/氯乙烷/2-氯丙烷/基因毒性杂质Key words
gas chromatography-mass spectrometry/cytarabinel/methylchloride/ethylchloride/2-chloropropane/genotoxic impurity引用本文复制引用
出版年
2024
国家科技期刊平台
NSTL
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