药物中石油醚残留量的气相色谱检测方法学探讨

Investigation of quantitive control of residual petroleum ether in pharmaceuticals by gas capillary chromatography

目的:采用气相色谱法对药物中残留的石油醚进行定量检测方法学探讨。方法:以市售石油醚(60～90℃)为例,结合新药尼非韦罗中涉及的甲醇、乙醇、二氯甲烷、乙酸乙酯、四氢呋喃以及1,4-二氧六环的分离情况,建立气相色谱条什。在分析了石油醚(60～90℃)的组分分布基础上,对其定量测定办法分别探讨了了单一组分的峰面积计算方式和主成分(按信噪比大于10)峰面积加和方式。结果:发现石油醚(60～90℃)在药物中的残留量计算采用主成分峰面积加和方式较合理,而且石油醚(60～90℃)和上述6种有机溶剂在相应的检测范围内线性良好,回收率均令人满意。结论:石油醚(60～90℃)在药物中的残留定量计算方式采用主成分峰面积加和法可以减少由于不同厂家来源或者不同批号的石油醚组分比例差异导致的汁算偏差,从而可以较好地满足对相关药物的质量控制要求。

Objective：A quantitative determination of residual petroleum ether in pharmaceuticals by gas chroma- tography（ GC ）was explored. Method：Using several batches of petroleum ether（60-90℃）obtained from market as samples, the separation was optimized to analyze the peak distributions of petroleum ether （ 60 - 90℃） combined with other residual solvents such as methanol, ethanol, dichloromethane, ethyl acetate, tetrahydrofuran and 1,4 -dioxane contained in a new drug candidate named as nifeviroc. Both calibration methods of peak area response based on one - component or multi - component （ S/N 〉 10 ） for petroleum ether （ 60 - 90℃） control in pharmaceutical were investigated. Results： It was found the quantitative determination for petroleum ether （ 60 - 90℃） based on multi - component calibration method had a good linear relationship and showed better rational control purpose. Sat- isfactory recoveries for all investigated residual solvents including petroleum ether（60 -90℃）were obtained. Conclusion：The proposed quantitative determination of petroleum ether（60 -90℃）can reduce the differences among different manufactures or different batches, thus then has a good quality control for pharmaceuticals concerned.