甲磺酸萘莫司他中有机溶剂残留的测定  

Determination of residual solvents in nafamostat mesilate by gas chromatography

作　　者：李博[1,2] 步芬[1] 徐光富[2,3] 

机构地区：[1]中国药科大学食品质量与安全教研室,江苏南京210009 [2]教育部药物质量与安全预警重点实验室,江苏南京210009 [3]中国药科大学分析化学教研室,江苏南京210009

出　　处：《中国医药科学》2011年第23期41-42,共2页China Medicine And Pharmacy

摘　　要：目的建立气相色谱法测定甲磺酸萘莫司他中有机溶剂残留量。方法在EC-1000(30m×0.54mm×1.2μm)毛细管柱上采用程序升温法,载气为氮气,汽化室温度200℃,检测器温度220℃,以二氧六环为内标,内标法测定甲磺酸萘莫司他中残留的甲醇、丙酮、吡啶、N,N-二甲基甲酰胺。结果在本研究色谱条件下,各溶剂及内标均能得到良好的分离度,空白无干扰;在所考察的浓度范围内线性良好,相关系数均在0.9996以上,回收率96.7%～102.0%,检测限0.15～2.8μg/mL。结论试验建立的色谱方法简便、准确,灵敏度高,适合甲磺酸萘莫司他机溶剂残留量的检测。Objective To establish a gas chromatography method for the determination of residual solvents in nafamostat mesilate. Methods The residual solvents in nafamostat mesilate were separated by EC-1000 capillary column （ 30 m × 0.54 mm×1.2 μm ）using programmed column temperature.N2 was used as carrier gas.and the temperature of injector and detector were 200℃ and 220℃ respectively.The residue of acetone,menthanol,pyridine and N,N-dimethylformamide in nafamostat mesilate were quantified with 1,4-dioxane as internal standard. Results The solvents and internal standard were seperated completely,and blank showed no interference.The calibration curve of each solvent showed a good linear relationship（r ≥ 0.999 6）.The average recovery was in the range of 97.6% - 102.0%.The detection limit of acetone,methanol, pyridine and N,N-dimethylformamide were 0.15 - 2.8 μg/mL. Conclusion The established method was simple, accurate and sensitive.It can be used for the determination of residual solvents in nafamostat mesilate.

关 键 词：甲磺酸萘莫司他 残留溶剂 气相色谱法 

分 类 号：R961[医药卫生—药理学]