摘要
建立瑞替加滨原料药中甲醇、异丙醇、乙酸乙酯残留溶剂的测定方法。以二甲基亚砜(DMSO)为溶剂,DB–WAX123–7032石英毛细管柱为色谱分离柱,FID检测器,程序升温,氮气为载气。甲醇、异丙醇、乙酸乙酯能得到良好分离,甲醇在29.23~292.30μg/m L范围内有良好的线性,线性相关系数为0.996,平均回收率为103.83%;异丙醇在49.96~499.60μg/m L范围内有良好的线性,线性相关系数r=0.996,平均回收率为105.16%;乙酸乙酯在51.59~515.90μg/m L范围内有良好的线性,线性相关系数为0.996,平均回收率为101.36%。甲醇、异丙醇、乙酸乙酯的检出限分别为0.036,0.213,0.062μg/m L,测定结果的相对标准偏差分别为4.96%,4.52%,4.34%(n=6)。该方法灵敏度高,可用于瑞替加滨原料药中有机溶剂的检测。
A method for determining methanol,isopropanol and ethyl acetate in retigabine material by headspace gaschromatography was established.The solvent media was dimethyl sulfoxide(DMSO),the seperation was carried on DB–WAX123–7032capillary column with the FID detector at temperature programming,the carrier gas was nitrogen.The resultshowed that the three solvents were completely separated.The standard curve of methanol was linear in the range of29.23–292.30μg/mL,r=0.996,the average recovery was103.83%.The standard curve of isopropanol was linear in the range of49.96–499.60μg/mL,r=0.996,the average recovery was105.16%.The standard curve of ethyl acetate was linear in therange of51.59–515.90μg/mL,r=0.996,the average recovery was101.36%.The detector limit of methanol,isopropanoland ethyl acetate were0.036,0.213and0.062μg/mL,and the relative standard deviations of detection results were4.96%,4.52%,4.34%(n=6),repectively.The method is sensitive and it can be used for the detection of three residual solvents inretigabine.
作者
高海鹰
孟黎明
王海玲
关悦
Gao haiying;Meng Liming;Wang Hailing;Guan Yue(Jilin Institute of Pharmaceutical Research, Changchun 130061, China)
出处
《化学分析计量》
CAS
2017年第1期12-15,共4页
Chemical Analysis And Meterage
基金
吉林省科技发展计划项目(20130206017SF)
