气相色谱法测定恩曲他滨中5种有机溶剂残留量

Determination of 5 residual organic solvents in entrutabine by gas chromatography

建立恩曲他滨原料药中5种有机溶剂残留量的气相色谱测定方法。以10%N,N-二甲基甲酰胺(DMF)为溶解介质,采用气相色谱顶空进样法测定恩曲他滨中的甲醇、乙醇、四氢呋喃、苯;采用气相色谱直接进样法,测定恩曲他滨中的正己烷。在选定的仪器工作条件下,甲醇、乙醇、四氢呋喃、苯、正己烷5种残留溶剂完全分离,在所考察的浓度范围内4种有机溶剂的质量浓度与色谱峰面积具有良好的线性,线性相关系数为0.9994~0.9999,检出限为0.4~1.4 ng/mL,平均回收率为98.4%~99.0%,测定值的相对标准偏差均小于1.0%(n=9)。正己烷的质量浓度在0.01159~0.1159 mg/mL范围内与色谱峰面积具有良好的线性,线性相关系数为0.9999,样品加标回收率为97.9%,测定值的相对标准偏差小于1.0%(n=9),检出限为8.7 ng/mL。这两种方法灵敏度、准确度均达到溶剂残留量的检测要求,可用于恩曲他滨原料药中5种残留溶剂的检测与分析。

A gas chromatography(GC)was established to determine five residual organic solvents including methanol,ethanol,tetrahydrofuran,benzene and hexane in emtricitabine.Methanol,ethanol,tetrahydrofuran and benzene in emtricitabine were determined by gas chromatography headspace sampling with 10%N,N-dimethylformamide(DMF)as dissolution medium,the direct injection method of gas chromatography was used to determine n-hexane in emtricitabine.Under the working conditions of the selected instrument,the 5 residual solvents of methanol,ethanol,tetrahydrofuran and benzene and n-hexane were completely separated.Within the investigated concentration range,the mass concentration of the four organic solvents had a good linearity with the chromatographic peak area.The linear correlation coefficiesnt were 0.9994–0.9999,the detection limits were 0.4–1.4 ng/mL,the average recoveries were 98.4%–99.0%,and the relative standard deviations of the measured values were all less than 1.0%.The mass concentration of n-hexane had good linearity with the chromatographic peak area in the range of 0.01159–0.1159 mg/mL,the linear correlation coefficient was 0.9999,the recovery was 97.9%,the relative standard deviations of the measured value were less than 1.0%(n=9),and the detection limit was 8.7 ng/mL.The sensitivity and accuracy of the two methods meet the requirements for the detection of solvent residues,and it can be used for the detection and analysis of five residual solvents in enrotabine.