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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 method for the determination of azacitidine residue in a variety of organic solvents. Methods: The chromatographic column was VF-624ms capillary column (60m × 0.25mm, 1.4μm). The carrier gas was nitrogen and hydrogen flame ionization detector. The column temperature was programmed. Results: The five solvents methanol, isopropanol, methylene chloride, methyl formate and methyl acetate were effectively separated under these conditions, and the linear relationship was good. The linear ranges of methanol, methyl formate, isopropanol, methyl acetate and dichloromethane were 10.32 ~ 127.89μg · ml -1 (r = 0.999 8), 1.34 ~ 17.08μg · ml -1 (r = 0.999 9), 3.44-43.16 μg · ml -1 (r = 0.9999), 1.47-16.94 μg · ml -1 (r = 0.999 8), 0.79-8.61 μg · ml -1 (R = 0.999 4). The average recoveries were 97.7% (RSD = 1.8%, n = 6), 100.0% (RSD = 1.4%, n = 6), 99.7% (RSD = 4.6%, n = 6) .The detection limits were 5.16,0.67,1.72,0.74,0.40μg · ml ~ (- 1). Conclusion: The method is simple, accurate, sensitive and reproducible. It is suitable for the detection of residual solvents in azacitidine.