顶空气相色谱法检测依诺肝素钠原料药中有机溶剂残留

Determination of Organic Solvent Residue in Enoxaparin Sodium by Headspace Gas Chromatography

目的建立依诺肝素钠原料药中甲醇、乙醇、二氯甲烷残留量的检测方法。方法采用顶空毛细管气相色谱方法,使用HP-5毛细管柱(30 m×0.32 mm,0.25μm)为分析柱,以外标法定量。结果在选择的色谱条件下,检测质量浓度线性范围甲醇为4～160μg/mL、乙醇为10～400μg/mL、二氯甲烷为1.25～50μg/mL。加样回收率分别为甲醇88.74%、乙醇94.48%、二氯甲烷95.33%,RSD分别为1.6%,1.9%,2.8%(n=3)。结论建立的方法能有效检测依诺肝素钠原料药中甲醇、乙醇和二氯甲烷的残留量。

Objective To develop a headspace gas chromatography method for determining residual organic solvents methanol,ethanol and dichloromethane in enoxaparin sodium.Methods The headspace gas chromatography was adopted by using the Angilent HP-5 capillary column（ 30 m × 0.32 mm,0.25 μm） as the analytic column with external standard method for quantitation.Results Under the selected chromatographic condition,methanol,ethanol and dichloromethane within the ranges of 4-160 μg / mL,10-400 μg / mL and 1.25-50 μg /mL had good linear relation.The average recovery rates of methanol,ethanol and dichloromethane were 88.74%,94.48%,95.33% respectively,with RSD of 1.6%,1.9% and 2.8%（ n = 3） accordingly.Conclusion The established method can effectively determine the residual amounts of methanol,ethanol and dichloromethane in enoxaparin e sodium.