顶空毛细管气相色谱法测定奥曲肽中有机溶剂残留量

目的建立气相色谱法测定奥曲肽中有机溶剂二氯甲烷、吡啶、N,N-二甲基甲酰胺残留量的方法。方法采用顶空毛细管气相色谱法,应用DB-624大口径毛细管柱(30 m×0.53 mm×3μm);氢火焰离子化检测器,以水为溶剂,初始柱温为60°C维持3 min,以10℃/min的速率升温至160℃,维持3 min,进样口温度:140℃;检测器温度:250℃;以高纯氮气为载气,流速3.0 ml/min;分流比为5∶1,实现各组分的基线分离。结果此法具有良好的线性,r在0.999 5~1之间,RSD小于5%(n=5)。结论经方法学验证,该方法灵敏度、准确度均达到有机溶剂残留量的检测要求,可用于原料药奥曲肽中残留溶剂的检测。

Determination of three residual organic solvents in octreotide by headspace capillary gas chromatography

PurposeTo determine the content of residual organic solvents: dichloromethane,pyridine,DMF in octreotide.MethodsUsing DB-624 capillary column(30 m×0.53 mm×3 μm),FID detector and programablly increased temperature,the samples were dissolved in water.The initial temperature was kept at 60 ℃ for 3 min.The temperature was raised to 160℃ at the rate of 10 ℃/min.ResultsThere was a good linearity(r=0.999 5～1).The RSD of precision and accuracy was less than 5%.ConclusionThe methods proved to be accurate and sensitive after validation.It is suitable to the determination of residual organic solvents in octreotide.