顶空GC法测定奥替溴铵中有机溶剂残留量

Determination of Residual Solvents in Otilonium Bromide by Headspace GC

目的:建立奥替溴铵中甲醇、三氯甲烷、环己烷、丙酮、乙酸乙酯5种有机溶剂残留量检测方法。方法:采用顶空气相色谱法,载气为氮气,FID检测器,色谱柱为DB-624毛细管柱,程序升温,外标法测定了奥替溴铵中5种有机溶剂的残留量。结果:5种有机溶剂完全分离,分别在考察浓度3.04～48.64,0.51～8.10,0.40～6.48,4.12～65.92,4.26～68.16μg·ml^(-1)范围内具有良好的线性关系,r分别为0.999 3,0.999 9,0.999 4,0.999 6,0.999 7,平均回收率依次为95.4%,85.2%,83.5%,90.3%,87.3%,RSD分别为2.4%,2.9%,3.5%,2.7%,3.1%(n=9),最低检测限分别为0.12,0.09,0.23,0.04,0.05μg·ml^(-1)。结论:该方法简便、准确,可用于奥替溴铵中几种残留溶剂的同时检测。

Objective： To establish a determination method for the residual solvents including methanol, chloroform, cyclobexane, acetone and ethyl acetate in otilonium bromide. Method： The residual solvents were determined by headspace GC on a DB-624 column with FID detector, and nitrogen was selected as the carrier gas. The amounts of the residual solvents were calculated according to the external standard method. Result： The five residual solvents were well separated, the linear range was 3.04-48.64 （r = 0.999 3 ）, 0.51-8.10（r =0.999 9） ,0.40-6.48（r =0. 999 4） ,4.12-65.92（r =0.999 6） and 4.26-68.16μg ~ ml-1 （r =0.999 7） with the re- covery of 95.4% ,85.2% , 83.5%, 90.3% and 87.3% , and RSD of 2.4% ,2.9% , 3.5% ,2.7% and 3.1% , respectively（n =9）. The minimum detective limit was 0.12,0. 09,0. 23 ,0. 04 and 0.05 μg ml -1, respectively. Conclusion： The method is simple and ac- curate, and can be used in the determination of several solvents in otilonium bromide.