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

作　　者：马博凯[1,2] 高峡[2] 刘伟丽[2] 林雨青[1] MA Bo-Kai Gao Xia LIU Wei-Li LIN Yu-Qing(Department of Chemistry, Capital Normal University, Beifing 100048, China Beijing Key Laboratory of Detection Technology and Quality Evaluation of Organic Materials, Beijing Center for Physical and Chemical Analysis, Belting 100089, China)

机构地区：[1]首都师范大学化学系,北京100048 [2]北京市理化分析测试中心,有机材料检测技术与质量评价北京市重点实验室,北京100089

出　　处：《分析化学》2016年第10期1528-1532,共5页Chinese Journal of Analytical Chemistry

摘　　要：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.

关 键 词：顶空气相色谱法 托比司他 残留溶剂 同时测定 

分 类 号：O657.71[理学—分析化学]