摘要
目的:建立地西他滨中多种有机溶剂残留量的测定方法。方法:采用顶空气相色谱内标法,色谱柱为DB-624毛细管柱(30 m×0.53 mm,3.0μm),载气为氮气,氢火焰离子化检测器,柱温程序升温(初始柱温40℃平衡8 min,以25℃·min^-1的速率升温至200℃,平衡10 min,再以35℃·min^-1的速率降温至40℃,平衡2 min)。结果:4种组分甲醇、甲酸甲酯、乙腈、对甲基苯甲酸甲酯在此条件下能有效分离,线性范围分别为0.6094~314.8236μg·ml-1(r=0.9998)、0.1614~25.2360μg·ml^-1(r=0.9997)、0.5762~24.8868μg·ml-1(r=0.9996)、2.0304~25.5870μg·ml^-1(r=0.9987),平均回收率分别为102.4%(RSD=1.7%),104.0%(RSD=1.1%),99.7%(RSD=1.8%),101.3%(RSD=1.8%)(n=9),检测限(LOD)分别为:0.2742,0.0726,0.2593,0.9137μg·ml^-1。结论:该方法简单、准确、灵敏度高、重复性好,适合于地西他滨中残留溶剂的检测。
Objective:To establish a headspace gas chromatography method for the determination of residual solvents in decitabine.Methods:A headspace gas chromatography with an internal standard was used with a capillary column DB-624(30 m×0.53 mm,3.0μm),and with nitrogen as the carrier and an FID as the detector.The column temperature was programmed raising(the initial temperature was 40℃,maintaining for 8 min,and rose to 200℃at the rate of 25℃·min^-1,maintaining for 10 min,and then cooling to 40℃at the rate of 35℃·min^-1,maintaining for 2 min).Results:The linear range for methanol,methyl formate,acetonitrile and methyl p-toluate was 0.6094-314.8236μg·ml^-1(r=0.9998),0.1614-25.2360μg·ml-1(r=0.9997),0.5762-24.8868μg·ml^-1(r=0.9996)and 2.0304-25.5870μg·ml-1(r=0.9987),respectively.The average recovery was 102.4%(RSD=1.7%),104.0%(RSD=1.1%),99.7%(RSD=1.8%)and 101.3%(RSD=1.8%)(n=9)with the LOD of 0.2742,0.0726,0.2593 and 0.9137μg·ml-1,respectively.Conclusion:The method is simple,accurate,sensitive and reproducible.It can be used for the determination of various residual solvents in decitabine.
作者
程志刚
王艳平
何思雨
Cheng Zhigang;Wan Yanping;He Siyu(Wuhan Biocause Pharmaceutical Development Co.Ltd.,Wuhan 430056,China)
出处
《中国药师》
CAS
2020年第1期196-198,共3页
China Pharmacist
关键词
地西他滨
顶空气相色谱法
残留溶剂
内标法
Decitabine
Headspace gas chromatography
Residual solvents
Internal standard method
