摘要
目的:建立碘佛醇原料药中甲醇、正丁醇和2-甲氧基乙醇残留量的测定方法。方法:采用顶空进样法,N,N-二甲基乙酰胺为溶剂,甲苯为内标,平衡温度80℃,平衡时间为45min。气相色谱条件:采用PEG20M毛细管柱为色谱柱(30m×0.53mm),柱温50℃维持2min,以5℃·min^(-1)的速率升温至200℃,维持10min。进样口温度为220℃,FID检测器,检测器温度为250℃。载气为氮气,流速为1mL·min^(-1)。结果:甲醇、正丁醇和2-甲氧基乙醇分别在61.5～418.9,59.3～419.5,20～140μg·mL^(-1)的浓度范围内呈良好的线性关系;加样回收率分别为97.7%,99.5%,98.6%;精密度良好。结论:该方法灵敏,准确,可靠,适用于本品有机溶剂残留量的测定。
Objective: To establish a method for quantification of residual methanol, n-butanol and 2-methoxyethanol in drug substance ioversol. Methods: Samples dissolved in N, N-dimethylacetamide were loaded onto the head space-GC and then was equilibrated at 80℃ for 45min. Toluene was used as internal standard. The optimal gas chromatography was run in a PEG20M capillary column (30m×0.53mm). The initial column temperature was kept at 50℃ for 2min. The column temperature was then escalated to 200℃ at the rate of 5℃·min^(-1) and subsequently sustained for 10min. The temperature at the injection port and the FID detector were 220℃ and 250℃, respectively. N_2 was used as carrier gas at a flow rate of 1mL·min^(-1). Results: Methanol, n-butanol and 2-methoxyethanol showed a linear plot within 61.5～418.9μg·mL^(-1), 59.3～419.5μg·mL^(-1) and 20～140μg·mL^(-1), respectively, with a mean recovery of 97.7%, 99.5% and 98.6%, respectively. Conclusion: The sensitive and accurate method was reliable in the quantification of residual solvents.
出处
《中国新药杂志》
CAS
CSCD
北大核心
2005年第2期187-189,共3页
Chinese Journal of New Drugs
