摘要
目的:建立毛细管色谱法测定盐酸青藤碱中三氯甲烷的残留量。方法:采用DB-624毛细管色谱柱(30 m×0.32 mm,涂层厚1.8μm),载气为氮气,进样口温度为200℃,柱温为65℃,检测器温度为230℃,FID为检测器,顶空进样法,水为溶剂,平衡温度70℃,平衡时间45min。结果:三氯甲烷在0.1845~18.45μg·mL-1范围内呈良好的线性关系(r=0.9995);平均回收率为98.2%,RSD为2.2%(n=6);最低检出限为36.9 ng·mL-1。结论:该方法灵敏、简单、准确,可用于测定盐酸青藤碱中三氯甲烷的残留量。
Objective:A headspace GC method was established for determination of residual chloroform in sinomenone hydrochloride.Method:Using a DB-624 column with 30 m long and 0.32 mm in internal diameter(diameter 1.8 μm),with nitrogen as carrier gas and FID as detector.The injector temperature was 200 ℃,the column temperature was 65 ℃ and the detector temperature was 230 ℃.Water was used as solvent,and samples had been equilibrated at 70 ℃ for 45 minutes.Results:The calibration curves of chloroform showed good linearity in the range of 0.1845-18.45 μg·mL-1(r=0.9995);The average recovery was 98.2% with RSD 2.2%(n=6);The detection limit was 36.9 ng·mL-1.Conclusion:The method is accurate sensitive,simple and reliable,it is suitable for measurement of residual chloroform in the sinomenone hydrochloride.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2011年第3期567-569,共3页
Chinese Journal of Pharmaceutical Analysis
基金
中国药典起草
正清风痛宁注射液品质风险控制关键技术研究课题
关键词
顶空气相色谱法
盐酸青藤碱
三氯甲烷残留量
headspace gas chromatography
sinomenone hydrochloride
residual chloroform.