顶空气相色谱法测定两性霉素B中的有机溶剂残留量

Content determination of residual solvent in amphotericin B by headspace gas chromatography

目的建立两性霉素B中乙醇、丙酮两种有机溶剂残留量的测定方法.方法采用顶空气相色谱法,氢火焰离子化检测器(FID),毛细管柱DB-5(3m×0.53mm,0.5μm);柱温:40℃保持1min,以20℃/min的速率升温至200℃保持2min;载气:N 2;线速度:35cm/s;分流比:30/1.结果3批样品中有机溶剂残留量均符合要求,平均回收率95.3%～102.0%.结论本方法简便灵敏,重复性好,能较好的进行两性霉素B中有机溶剂残留量的测定.

Objective To determine the content of residual solvent, ethanol and acetone in (amphotericin) B. Methods The sample was subjected to a headspace gas chromatography in a DB-5 capillary column (3m×0.53mm, 0.5μm); programmed with a starting temperature of 40℃ for 10min, by increasing of 20℃/min up to 200℃, and then further for 2 min; a FID detector, nitrogen as the carrier gas; 35cm/sec of (velocity); 30/1 of split ratio. Results The contents of two residual solvents in three batches of samples could be satisfactorily determined. The average recoveries were 95.3%～102.0%. Conclusion The proposed method was simple, sensitive, accurate and reliable. It is suitable for the determination of the residual content of organic solvents.