| 引用本文: | 张玲,杨华良,王家明.GC测定安立生坦原料药中6种有机溶剂残留[J].中国现代应用药学,2014,31(10):1238-1241. |
| ZHANG Ling,YANG Hualiang,WANG Jiaming.Determination of the Six Residual Organic Solvents in Ambrisentan by GC[J].Chin J Mod Appl Pharm(中国现代应用药学),2014,31(10):1238-1241. |
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| 摘要: |
| 目的 建立测定安立生坦原料药中可能残留的6种有机溶剂(甲醇、乙醚、二氯甲烷、乙酸乙酯、1,4-二氧六环、N,N-二甲基甲酰胺)含量的检测方法。方法 采用顶空气相色谱法，色谱柱为DB-624 毛细管柱(30.0 m×0.53 mm，3.00 μm)，氢火焰离子化检测器(FID)，进样口温度250 ℃，检测器温度300 ℃；载气为高纯氮气，恒压模式，压力2 psi；柱温为升温程序，50 ℃保持10 min，以20 ℃·min-1升温升至200 ℃，保持4 min；顶空瓶平衡温度100 ℃，平衡时间30 min。结果 6种残留溶剂色谱峰的理论板数均>10 000，相邻峰的分离度均>2.0，甲醇、乙醚、二氯甲烷、乙酸乙酯、1,4-二氧六环、N,N-二甲基甲酰胺的线性关系良好(r分别为0.999 6，0.999 2，0.999 5，0.999 3，0.999 3，0.999 6)；精密度与重复性RSD均<5.0%；最低检出浓度分别为0.36，0.034，0.51，0.43，0.45，5.27 μg·mL-1；平均回收率均在90%以上；供试品溶液24 h内稳定。结论 该气相色谱法操作简便，准确，灵敏度高，可用于检测安立生坦原料药中有机溶剂的残留量。 |
| 关键词: 安立生坦 顶空进样法 毛细管气相色谱法 有机溶剂残留 |
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| Determination of the Six Residual Organic Solvents in Ambrisentan by GC |
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ZHANG Ling1, YANG Hualiang1, WANG Jiaming2
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1.Department of Pharmacy, Tianjin Central Obstetrics and Gynecology Hospital, Tianjin 300100, China;2.Key Laboratory of Industrial Microbial Fermentation of Ministry of Education, Tianjin University of Science and Technology Biological Engineering Institute, Tianjin 300457, China
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| Abstract: |
| OBJECTIVE To establish a method for determination of the six residual organic solvents(methanol, ether, dichloromethane, ethyl acetate, 1,4-dioxane and N,N-dimethylformamide) in ambrisentan. METHODS Gas chromatography with headspace sampling was applied in the study. Agilent DB-624 silica capillary column(30.0 m×0.53 mm, 3.00 μm) was used. The inlet temperature was 250 ℃ and the FID detector temperature was 250 ℃. N2 was carrier gas at a column pressure of 2 psi. The initial temperature was kept at 50 ℃ for 10 min, then the temperature was raised to 200 ℃ at the rate of 20 ℃·min-1 and subsequently sustained for 4 min. FID detector temperature was 300 ℃. The vial temperature was 100 ℃, and the vial time was 30 min. RESULTS The linear correlation coefficients of this method for methanol, ether, dichloromethane, ethyl acetate, 1,4-dioxane and N,N-dimethylformamide were 0.999 6, 0.999 2, 0.999 5, 0.999 3, 0.999 3 and 0.999 6, respectively. The RSDs of precision and repeatability were all <5.0%. The limits of detection were 0.36, 0.034, 0.51, 0.43, 0.45 and 5.27 μg·mL-1, respectively. The average recovery were >90%. The sample solution was stable in 24 h. CONCLUSION The analytical method is simple, accurate and sensitive, and is suitable for the determination of residual solvents in ambrisentan. |
| Key words: ambrisentan headspace sampling GC residual organic solvents |
