摘要
目的:建立测定盐酸苯海拉明原料药中乙醇、甲苯残留量的方法。方法:采用顶空毛细管气相色谱法,以丁酮为内标。色谱柱为Agilent DB-624弹性石英毛细管柱,进样口温度为200℃,氢火焰离子化检测器温度为250℃,载气为高纯氮气,流速为3.0 ml/min,柱温为程序升温,进样方式为分流进样,分流比为20∶1,顶空平衡温度为80℃,平衡时间为30 min,进样时间为1 min。结果:在该色谱条件下,乙醇、甲苯与内标峰能得到良好分离;乙醇、甲苯的检测质量浓度线性范围均为0.02~0.8 mg/ml(r=0.9998、0.9994);精密度、稳定性、重复性试验的RSD<3%,乙醇、甲苯的加样回收率分别为95.50%~103.50%、96.91%~103.74%,RSD分别为2.6%、2.2%(n=9)。结论:该方法简单、灵敏、准确,可用于盐酸苯海拉明原料药中乙醇、甲苯残留量的测定。
OBJECTIVE:To establish a method for the determination of residual solvent of ethanol and toluene in diphenhydr-amine hydrochloride raw material. METHODS:Headspace capillary gas charmatography and butanone as internal standard were used. The column was Agilent DB-624 capillary column,inlet temperature was 200 ℃,hydrogen flame ionization detector was 250 ℃,the carried gas was high purity nitrogen,flow rate was 3.0 ml/min with temperature programmed,the splitting-ratio was 20∶1,the containers of headspace injector were in equilibrium at 80 ℃ for 30 min,and the injection time was 1 min. RESULTS:With this chromatographic condition,ethanol,toluene and internal standard peak were well separated;there was a good linear rela-tionship of ethanol and toluene in the range of 0.02-0.8 mg/ml (r=0.999 8 and r=0.999 4);RSDs of precision and stability test were lower than 3%;recoveries were 95.50%-103.50%(RSD=2.6%,n=9) and 96.91%-103.74%(RSD=2.2%,n=9). CON-CLUSIONS:The method is simple,sensitive and accurate,and can be used for the determination of residual solvent of ethanol and toluene in diphenhydramine hydrochloride raw material.
出处
《中国药房》
CAS
北大核心
2016年第18期2563-2565,共3页
China Pharmacy
关键词
顶空毛细管气相色谱法
盐酸苯海拉明原料药
残留溶剂
乙醇
甲苯
Headspace capillary gas charmatography
Diphenhydramine hydrochloride raw material
Residual solvent
Etha-nol
Toluene