柱前衍生-气相色谱法测定非布司他残留溶剂甲酸的含量

Determination of Residual Solvent Formic Acid Content in Febuxostat by Gas Chromatography with Pre-column Derivatization

目的:建立了柱前衍生-气相色谱法测定非布司他残留溶剂甲酸含量的方法研究。方法:采用DB-WAX UI(30 m×0.25 mm×0.5μm)色谱柱,氢火焰离子检测器(FID),检测器温度为230℃。结果:甲酸分离度良好,在2.5~500.0μg/mL浓度范围内线性关系良好(r=0.9999),定量限为2.5μg/mL,检测限为0.7μg/mL,平均回收率为97.8%,RSD为1.9%,供试品溶液稳定。非布司他原料药3批样品中均检测到有机溶剂甲酸,检测结果均符合甲酸的限度(不得过0.5%)要求。结论:本法操作简便、准确可靠、灵敏度高,适用于非布司他原料药中甲酸残留溶剂的分析检测。

Objective:A method for determining formic acid content of febuxostat residual solvent by pre-column derivatization-gas chromatography was established.Methods:DB-WAX UI(30 m×0.25 mm×0.5μm)column was used with hydrogen flame ion detector(FID).The detector temperature was 230℃.Results:The formic acid resolution was good,the linear relationship was good in the concentration range of 2.5~500.0μg/mL(r=0.9999),the limit of quantification was 2.5μg/mL,the detection limit was 0.7μg/mL,the average recovery rate was 97.8%,the RSD was 1.9%,and the test solution was stable.Organic solvent formic acid was detected in 3 batches of samples of febuxostat API,and the test results all met the limit of formic acid(not exceeding 0.5%).Conclusion:This method is simple to operate,accurate and reliable,and has high sensitivity,which is suitable for the analysis and detection of formic acid residual solvent in febuxostat APIs.