顶空毛细管GC法测定盐酸苯海拉明原料药中乙醇、甲苯的残留量-中国药房

顶空毛细管GC法测定盐酸苯海拉明原料药中乙醇、甲苯的残留量

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篇名：	顶空毛细管GC法测定盐酸苯海拉明原料药中乙醇、甲苯的残留量
TITLE：
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＝0.999 8、0.999 4）；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。
ABSTRACT：	OBJECTIVE： To establish a method for the determination of residual solvent of ethanol and toluene in diphenhydramine 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 relationship 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）. CONCLUSIONS： 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.
期刊：	2016年第27卷第18期
作者：	谈学惠，漆秋兰，刘国强，傅应华
AUTHORS：	TAN Xuehui，QI Qiulan，LIU Guoqiang，FU Yinghua
关键字：	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
KEYWORDS：	Headspace capillary gas charmatography； Diphenhydramine hydrochloride raw material； Residual solvent； Ethanol； Toluene
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