顶空气相色谱法测定布美他尼原料药中残留有机溶剂

Determination of Residual Organic Solvents in Bumetanide by Headspace Gas Chromatography

摘要: 建立测定布美他尼原料药中残留有机溶剂乙醇和甲苯的顶空气相色谱法方法。采用氢火焰离子化检测器，以二甲亚砜为样品溶剂，通过优化条件，建立了以DB-624为分析柱，90℃为平衡温度，30 min为平衡时间的残留溶剂测定方法。以外标法进行定量，乙醇及甲苯最低检测限分别是0.306 µg∙mL⁻¹和0.082 µg∙mL⁻¹，2种溶剂的线性系数均为1.0，回收率分别为103.5%和96.0%，RSD分别为4.0%和2.2%。结果表明，该方法简单、准确、灵敏度高、重现性好，能够满足对布美他尼质量的控制要求。将该方法应用于布美他尼原料药3批样品的检测，均未检出乙醇与甲苯。

Abstract: In order to develop quality control system of Bumetanide active substances, a headspace gas chromatographic method was established and validated for the determination of residual solvents of ethanol and toluene in Bumetanide by using FID as the detector and dimethylsulfoxide as sample solvent. The detection of four residual solvents was performed on a DB-624 capillary column with vial equilibration temperature of 90˚C and equilibration time of 30 min. The limits of detection (LOD) for ethanol and toluene were 0.306 µg∙mL⁻¹ and 0.082 µg∙mL⁻¹, respectively. The relative standard deviations (RSDs) of peak areas were 4.0% and 2.2%, the average recoveries were 103.5% and 96.0%, and the correlation coefficients were 1.0, respectively. The results indicated that the method showed the advantages of high sensitivity, good accuracy and linearity. The established method was applied in the quality control of three batches of Bumetanide, and no solvents were checked out.