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目的:建立测定盐酸溴己新原料药中4种有机溶剂(丙酮、乙醇、甲苯和乙酸)残留量的方法。方法:采用顶空气相色谱法分别测定。色谱柱均为HP-FFAP柱,检测器均为氢火焰离子化检测器,温度均为250℃;丙酮、乙醇、甲苯检测进样口温度为200℃,程序升温,顶空瓶平衡温度80℃,时间30 min,以二甲基亚砜为溶解介质;乙酸检测进样口温度为150℃,柱温60℃,顶空瓶平衡温度60℃,时间20 min,以甲醇为溶解介质,衍生化法检测。结果:在2种色谱条件下,各被测溶剂峰均分离良好,线性相关系数均大于0.999;丙酮、乙醇、甲苯和乙酸的平均回收率分别为104.4%、98.7%、105.7%、100.8%,RSD分别为2.3%、2.6%、2.7%、2.1%(n=3);检测限分别为0.25、1.21、0.18、0.32μg/ml。样品中只检出乙醇。结论:建立的方法准确、迅速,可用于检测盐酸溴己新原料药中残留的丙酮、乙醇、甲苯和乙酸。
Objective: To establish a method for the determination of four organic solvents (acetone, ethanol, toluene and acetic acid) in bromhexixin hydrochloride. Methods: Determination by headspace gas chromatography. The column was HP-FFAP column, the detectors were hydrogen flame ionization detector, the temperature was 250 ℃; acetone, ethanol, toluene detection inlet temperature was 200 ℃, the program temperature, the balance of headspace bottle temperature 80 ℃ , 30 min with dimethylsulfoxide (DMSO) as the dissolution medium. The inlet temperature of acetic acid detection was 150 ℃, the column temperature was 60 ℃, the equilibrium temperature of headspace bottle was 60 ℃, and the time was 20 min. Methanol was used as the dissolution medium to derivatize France test. Results: Under the two chromatographic conditions, the peak of each solvent was well separated and the linear correlation coefficients were all greater than 0.999. The average recoveries of acetone, ethanol, toluene and acetic acid were 104.4%, 98.7%, 105.7% and 100.8%, respectively. RSD were 2.3%, 2.6%, 2.7% and 2.1% respectively (n = 3). The detection limits were 0.25,1.21,0.18 and 0.32μg / ml, respectively. Only ethanol is detected in the sample. Conclusion: The established method is accurate and rapid and can be used for the determination of acetone, ethanol, toluene and acetic acid in the bromhexine hydrochloride.