顶空气相色谱法同时测定托比司他中的6种残留溶剂

Simultaneous Determination of Six Residual Solvents in Topiroxostat by Headspace Gas Chromatography

采用顶空气相色谱技术,建立了同时测定托比司他中6种残留溶剂的方法。考察了不同固定相对分离效果的影响,优化了平衡加热时间影响以及制样溶剂。在优化的实验条件下,采用Rtx-200型聚三氟丙基甲基硅氧烷为固定相的色谱柱(30 m×0.25 mm×1μm)分离、氢火焰离子化检测器检测、外标法定量的分析方案,实现了甲醇、乙醇、二氯甲烷、乙酸乙酯、1,4-二氧六环和吡啶6种残留溶剂的同时分离与测定。6种溶剂在各自的线性范围内线性关系良好,线性相关系数(R^2)均大于0.998,定量限分别为甲醇0.006%、乙醇0.005%、二氯甲烷0.012%、乙酸乙酯0.0025%、1,4-二氧六环0.0076%、吡啶0.004%。在3个添加水平下,6种残留溶剂的加标回收率在92.3%~100.3%之间,相对标准偏差为0.3%~3.6%。实际样品分析结果表明,本方法简单、快速、分离效果好,可用于托比司他中6种残留溶剂的检测。

A simple and sensitive headspace gas chromatographic method was developed and validated for simultaneous determination of methanol,ethanol,dichloromethane,ethyl acetate,1,4-dioxane and pyridine in topiroxostat. Under the conditions of optimization of stationary phase,heating temperature and equilibration time,the separation was achieved on a Rtx-200 column（ 30 m × 0. 25 mm × 1 μm） filled with polytrifluoropropyl（ methyl） siloxane by a flame ionization detector. The developed gas chromatographic method offered symmetric peak shape,and good resolution for all the 6 solvents. The good linearity was obtained for all the analytes with the correlation coefficients（R^2） greater than 0.998. The limits of quantification were 0.006%for methanol,0.005% for ethanol,0.012% for dichloromethane,0.0025% for ethyl acetate,0.0076% for 1,4-dioxane and 0.004% for pyridine,respectively. The recoveries for 6 residual solvents at three spiked levels were in the range of 92. 3%- 100. 3% with relative standard deviations of 0.32%-3.6%. The real sample analyses showed that this method was simple,fast and feasible for the simultaneous determination of 6 residual solvents in topiroxostat.