顶空气相色谱法测定阿尼芬净关键原料对戊氧基三联苯甲酸中的残留溶剂

Determination of Residual Solvents in p-Pentyloxytribenzoic Acid as Key Raw Material of Anidulafungin by Headspace Gas Chromatography

建立了同时测定阿尼芬净关键原料对戊氧基三联苯甲酸中7种残留溶剂(正己烷、乙酸乙酯、四氢呋喃、乙基苯、对二甲苯、邻二甲苯、二甲基亚砜)的顶空气相色谱法.色谱条件为:色谱柱采用以6%氰丙基苯基-94%二甲基聚硅氧烷(DB-624)为固定液的毛细管柱,程序升温,进样口温度240℃,氢火焰离子化检测器(FID)温度250℃,顶空平衡温度130℃,平衡时间40min.结果表明,7种残留溶剂的浓度与峰面积线性关系良好,相关系数均在0.999以上;7种残留溶剂的平均加标回收率分别为89.23%、95.80%、94.74%、95.82%、92.45%、92.80%、104.47%,RSD值分别为4.1%、3.7%、3.2%、5.2%、4.4%、4.3%、3.4%.该方法操作简单、灵敏度高、准确性高、专属性强,可用于对戊氧基三联苯甲酸中残留溶剂的测定.

We established a headspace gas chromatography method for the simultaneous determination of seven residual solvents(n-hexane,ethyl acetate,tetrahydrofuran,ethyl benzene,p-xylene,o-xylene,and dimethyl sulfoxide)in p-pentyloxytribenzoic acid as the key raw material of Anidulafungin.The chromatographic conditions are determined as follows:the analysis is performed on capillary column with 6%cyanopropyl phenyl-94%dimethyl polysiloxane(DB-624)as the stationary liquid,temperature programming is adopted,the inlet temperature is set to be 240℃,the temperature of hydrogen flame ionization detector is set to be 250℃,the headspace equilibrium temperature is set to be 130℃,and the equilibrium time is set to be 40 min.The results show that the concentrations of the seven residual solvents bear good linear relationships with the peak areas,and the correlation coefficients are all above 0.999.The recoveries of the seven residual solvents are 89.23%,95.80%,94.74%,95.82%,92.45%,92.80%,and 104.47%,with RSD values of 4.1%,3.7%,3.2%,5.2%,4.4%,4.3%,and 3.4%,respectively.The method is simple,sensitive,accurate,and specific,which can be used for the determination of residual solvents in p-pentyloxytribenzoic acid as the key raw material of Anidulafungin.