气相色谱法对药品中残留溶剂的检测分析

蓝明玉

[摘要] 目的 探讨苯磺酸氨氯地平中残留溶剂采用顶空气相色谱法测定的应用价值。 方法 采用顶空气相色谱法对苯磺酸氨氯地平中的残留溶剂N，N-二甲基乙酰胺、乙酸乙酯、甲苯、异丙醇进行测定。 结果 N，N-二甲基乙酰胺、乙酸乙酯、甲苯、异丙醇在考察范围内线性良好，线性范围分别为124.76～396.55mg/L、500.36～1500.55mg/L、50.32～150.17mg/L和500.54～1500.88mg/L；r分别为0.9987、0.9996、0.9998、0.9999；平均回收率分别为101.5%、102.9%、103.3%和102.1%；RSD分别为5.8%、5.1%、5.9%、5.4%；检测限分别为12.9mg/L、10.6mg/L、6.41mg/L和19.8mg/L。 结论 采用顶空气相色谱法测定苯磺酸氨氯地平中残留溶剂含量具有准确度好、灵敏度高、操作简单、重现性好等优点，是苯磺酸氨氯地平实际生产中残留溶剂含量测定的有效方法。

[关键词] 顶空气相色谱法；苯磺酸氨氯地平；残留溶剂；含量测定

[中图分类号] R927 [文献标识码] A [文章编号] 2095-0616（2015）11-38-04

[Abstract] Objective To explore application value of headspace gas chromatography in determination of amlodipine besylate residual solvents. Methods Amlodipine besylate residual solvents N， N-dimethylacetamide，ethyl acetate，toluene，isopropanol were determinated by headspace gas chromatography. Results N，N-dimethylacetamide，ethyl acetate，toluene and isopropanol were all in good linearity in the scope of the study and the linear ranges were 124.76-396.55mg/L，500.36-1500.55mg/L，50.32-150.17mg/L and 500.54-1500.88mg/L respectively；r were 0.9987，0.9996，0.9998 and 0.9999 respectively.Average recoveries were 101.5%，102.9%，103.3% and 102.1% respectively.RSD were 5.8%，5.1%，5.9% and 5.4 % respectively.The detection limits were 12.9mg/L，10.6mg/L， 6.41mg/L and 19.8mg/L respectively. Conclusion Headspace gas chromatography in determination of amlodipine besylate residual solvents has some advantages including good accuracy，high sensitivity，simple operation and good reproducibility etc.And it is an effective method of the determination of amlodipine besylate residual solvents in actual production.

[Key words] Headspace gas chromatography；Amlodipine besylate；Residual solvent；Determination

苯磺酸氨氯地平是临床常用的高血压及心绞痛治疗药物，属第三代二氢吡啶类钙离子通道阻断剂，具有吸收好（吸收不受饮食影响），口服生物利用度高，清除半衰期长（一次给药可维持有效血药浓度24h），不良反应少等优点[1-2]。在苯磺酸氨氯地平合成过程中会使用到N，N-二甲基乙酰胺、乙酸乙酯、甲苯、异丙醇等二类和三类溶剂，如果这些溶剂残留超标将会对使用人员的身体造成一定的损害，因此，根据2010版《中华人民共和国药典》[3]，本研究旨在建立顶空气相色谱法测定苯磺酸氨氯地平中残留溶剂含量的方法，为苯磺酸氨氯地平实际生产中残留溶剂含量测定的提供借鉴和指导。

1 仪器与试剂

美国安捷伦7890A型气相色谱仪、安……