【摘要】 目的:建立阿扎胞苷中多种有机溶剂残留量的测定方法。方法:采用项空气相色谱法,色谱柱为VF-624ms毛细管柱（60m×0.25mm,1.4μm）,载气为氮气,氢火焰离子化检测器,柱温程序升温。结果:5种溶剂甲醇、异丙醇、二氯甲烷、甲酸甲酯、乙酸甲酯在此条件下能有效分离,且线性关系良好。甲醇,甲酸甲酯,异丙醇,乙酸甲酯,二氯甲烷的线性范围分别为10.32～127.89μg·ml^-1（r=0.999 8）,1.34～17.08μg·ml^-1（r=0.999 9）,3.44～43.16μg·ml^-1（r=0.9999）,1.47～16.94μg·ml^-1（r=0.999 8）,0.79～8.61μg·ml^-1（r=0.999 4）;平均回收率分别为97.7%（RSD=1.8%,n=6）,100.0%（RSD=1.6%,n=6）,99.3%（RSD=1.2%,n=6）,101.2%（RSD=1.4%,n=6）,99.7%（RSD=4.6%,n=6）;检测限分别为5.16,0.67,1.72,0.74,0.40μg·ml^-1。结论:该方法简单、准确、灵敏度高、重复性好,适合于阿扎胞苷中残留溶剂的检测。更多还原

【Abstract】 Objective:To establish a headspace gas chromatography method for the determination of residual solvents in azacytidine. Method:A capillary column VF-624ms（60 m×0.25 mm,1.4μm） was used with nitrogen as the carrier and FID as the detector,the column temperature was increased by temperature-programming method.Result:The linear range for methanol,methyl formate,2-propanol, methyl acetate and dichloromethane was 10.32-127.89μg·ml^-1（r =0.999 8）,1.34-17.08μg·ml^-1（r =0.999 9）,3.44-43.16μg·ml^-1（r=0.9999）,1.47-16.94μg·ml^-1（r=0.9998） and 0.79-8.61μg·ml^-1（r=0.999 4） with the average recovery of 97.7% （RSD = 1.8%,n =6）,100.0%（RSD = 1.6%,n = 6）,99.3%（RSD = 1.2%,n =6）,101.2%（RSD = 1.4%,n =6） and 99.7%（RSD = 4.6%,n =6）,respectively.The detection limit was 5.16,0.67,1.72,0.74 and 0.40μg·ml^-1,respectively.Conclusion:The method is simple,accurate,sensitive and repeatable.It can be used for the determination of various residual solvents in azacytidine.更多还原