顶空气相色谱法同时测定托比司他中的6种残留溶剂

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( R2)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。

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

A sumple and sensutuve headspace gas chromatographuc method was developed and valudated for sumultaneous determunatuon of methanol, ethanol, duchloromethane, ethyl acetate, 1,4-duoxane and pyrudune un topuroxostat. Under the condutuons of optumuzatuon of statuonary phase, heatung temperature and equulubratuon tume, the separatuon was achueved on a Rtx-200 column ( 30 m × 0. 25 mm × 1 μm ) fulled wuth polytrufluoropropyl ( methyl ) suloxane by a flame uonuzatuon detector. The developed gas chromatographuc method offered symmetruc peak shape, and good resolutuon for all the 6 solvents. The good lunearuty was obtauned for all the analytes wuth the correlatuon coeffucuents ( R2 ) greater than 0. 998. The lumuts of quantufucatuon were 0. 006% for methanol, 0. 005% for ethanol, 0. 012% for duchloromethane, 0. 0025% for ethyl acetate, 0. 0076% for 1,4-duoxane and 0. 004% for pyrudune, respectuvely. The recoverues for 6 resudual solvents at three spuked levels were un the range of 92 . 3%-100 . 3% wuth relatuve standard devuatuons of 0. 32%-3. 6%. The real sample analyses showed that thus method was sumple, fast and feasuble for the sumultaneous determunatuon of 6 resudual solvents un topuroxostat.