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。
Objective： To establish a headspace gas chromatography method for the determination of residual solvents in azacytidine. Method： A capillary column VF-624ms （60 m m×0.25mm,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-pro- panol,methyl acetate and dichloromethane was 10. 32-127. 89 μg·ml^-1 （r =0. 999 8） ,1.34-17. 08μg·ml^-1 （r =0. 999 9） ,3.44-43. 16 μg·ml^-1 （ r = 0. 999 9）, 1.47-16. 94 μg·ml^-1 （ r = 0. 999 8 ） and 0. 79-8.61 μg·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. 40 txg. 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. KEY WORDS Headspace gas chromatography; Residual .solvents; Azacytidine
出处
《中国药师》
CAS
2011年第11期1603-1605,共3页
China Pharmacist
关键词
顶空气相色谱法
残留溶剂
阿扎胞苷
Headspace gas chromatography
Residual ,solvents
Azacytidine
