第1页参见附件。
[摘要] 目的 建立毛细管气相色谱法测定七氟烷的有关物质。 方法 本文采用毛细管气相色谱法，程序升温，FID检测器，色谱柱为DM-624毛细管柱(以6%氰丙苯基-94%二甲基聚硅氧烷为固定相；75 m×0.53 mm，3.0 μm)，对七氟烷合成工艺中存在的已知杂质戊氟异丙基氟甲醚和己氟异丙基甲基醚及未知杂质都进行了很好的分离和测定。 结果 七氟烷杂质含量测定的线性范围为0.14~0.72 μg/mL，回归方程：Y = 4.269X-0.041 3(r = 0.999 6)。最低检测限为6.272 ng，精密度RSD为1.88%。 结论 本法专属性强，灵敏度高，结果准确，可用于七氟烷的有关物质检查。
[关键词] 七氟烷；有关物质；气相色谱法
[中图分类号] O657.71 [文献标识码] A [文章编号] 1673-7210(2012)02(a)-0119-02
Determination of related substances of sevoflurane by capillary gas chromatography
WANG Yue1 LIU Shuyang2 LI Yinfeng2 JIN Chaodong2
1.Tianjin University of Traditional Chinese Medicine, Tianjin 300193, China; 2.The Center of Forecasting and Analysis, Tianjin Institute of Pharmaceutical Research, Tianjin 300193, China
[Abstract] Objective To establish a method for determination of related substances of sevoflurane by capillary gas chromatography. Methods The determination was performed on a DM-624 capillary column (coated with cross-linked 6% Polycyanopropylphenylsiloxane and 94% Polydimethylsiloxane, 75 m×0.53 mm, 3.0 μm), using temperature programming, with FID detector. The known impurities and unknown impurities in the synthesis process of sevoflurane were separated very well. Results There was a linear relationship in the concentration range of 0.14-0.72 μg/mL, the regression equation was Y = 4.269X-0.041 3 (r = 0.999 6) with the correlation coefficient of 0.999 6. The limit of detection was 6.272 ng and the relative standard deviation (RSD) value for precision was 1.88%. Conclusion This method is validated to be specific, accurate and suitable for the measurements of sevoflurane and its related substances.
[Key words] Sevoflurane; Related substances; GC
七氟烷是一种较新的吸入麻醉药，1968年由Regan合成，1971年Willin等最先报道并于1975年对其理化性质、药理作用及毒理学进行了评价，1992年使用于日本，1995年经美国FDA批准在美国上市。吸入型麻醉剂[1-3]能通过呼吸有效地调节血中麻醉药浓度，并能迅速被“洗出”，而七氟烷对心血管系统的影响比异氟烷小；不引起过敏反应，对眼黏膜刺激轻微，麻醉深度易调节等，是一种非常优良、具有较多理想特性的新型吸入型麻醉剂[4]。目前国内使用的七氟烷多为进口，为保证药品质量，针对国内厂家的生产工艺，建立了毛细管气相色谱法测定七氟烷的有关物质，并对测定条件进行了系统的考察。
1 仪器与试药
Agilent Technologies 6890N气相色谱仪，FID检测器，七氟烷对照品(批号：090228)，三批样品(天津市智康科技有限公司，批号：090301、090302、090303) ......
