毛细管气相色谱法同时测定盐酸普萘洛尔原料药中5种有机溶剂残留量

Simultaneous Determination of 5 Kinds of Residual Organic Solvents in Propranolol Hydrochloride by Capillary GC

目的：建立同时测定盐酸普萘洛尔原料药中乙醇、异丙胺、环氧氯丙烷、三乙胺和二甲苯残留量的方法。方法：采用毛细管气相色谱法。色谱柱为Wonda Cap-1毛细管柱,氢火焰离子化检测器,载气为氮气,流速为3 ml/min,进样口温度为180℃,检测器温度为250℃,程序升温,直接进样,进样量为1μl,以N,N-二甲基甲酰胺为溶剂,采用外标法计算溶剂残留量。结果：5种有机溶剂均能得到良好分离;各溶剂在所考察的质量浓度范围内与峰面积线性关系良好（r=0.993 8～0.999 8）;精密度试验的RSD≤4.07%;平均加样回收率为98.31%～103.75%（RSD=0.12%～3.66%,n=3）。结论：该方法简便、准确、可靠,可用于盐酸普萘洛尔原料药中多种有机溶剂残留量的同时测定。

OBJECTIVE： To establish a method for the determination of residual ethanol, isopropylamine, epichlorohydrin, tri- ethylamine and xylene in propranolol hydrochloride. METHODS： Capillary GC method was adopted. The determination was per- formed on WondaCap-1 capillary column with FID detector. Nitrogen was the carrier gas at the flow rate of 3 ml/min. The injector temperature was 180 ℃ and the detector temperature was 250℃ by temperature programming with direct sampling. The Sample size was 1 μl. The residual organic solvents were determined by external standard method using N,N-dimethylformamide as solvent. RESULTS： The five residual organic solvents were completely separated. Good linearity of the five organic solvents were obtained （r=0.993 8-0.999 8）. RSD of precision was lower than 4.07%. The average recoveries were ranged from 98.31% to 103.75% （RSD= 0.12 % -3.66 %, n = 3）. CONCLUSIONS ： The established method is simple, accurate and reliable which can be used for the determination of multiple residual organic solvents in propranolol pydrochloride simultaneously.