顶空气相色谱法测定盐酸溴己新原料药中4种有机溶剂的残留量

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。

Residual Determination of 4 Kinds of Organic Solvents in Bromhexine Hydrochloride Raw Material by Headspace Gas Chromatography

OBJECTIVE： To establish a method for the determination of 4 residual organic solvents in bromhexine hydrochloride raw material, such as acetone, ethanol, methylbenzene and acetic acid. METHODS： Headspace gas chromatography was adopted. The determination was performed on HP-FFAP column. FID detector was adopted with temperature of 250 ℃. The inlet temperature was 200 ℃ for acetone, ethanol and methylbenzene, and column temperature was programmed temperature; vial equilibration temperature was 80 ℃ and maintained for 30 min; dimethyl sulfoxide was used as dissolution medium. The inlet temperature was 150 ℃ for acetic acid and column temperature was 60 ℃ ; vial equilibration temperature was 60 ℃ and maintained for 20 min; methanol was used as dissolution medium for derivatization detection. RESULTS： All peaks could be separated from each other in chromatogram. The linearity of four solvents were fairly good （r〉0.999）. The average recovery of acetone, ethanol, toluene and acetic acid were 104.4% （RSD=2.3%, n=3）, 98.7% （RSD=2.6%, n=3）, 105.7% （RSD=2.7%, n=3） and 100.8% （RSD=2.1%, n=3）, respectively. The limits of detection were 0.25, 1.21, 0.18, 0.32 ~g/ml, respectively. Only ethanol was found in samples. CONCLUSIONS： The method is accurate and rapid for the determination of residual acetone, ethanol, methylbenzene and acetic acid in bromhexine hydrochloride raw material.