摘要
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分类
医药卫生
