摘要
目的：建立正清风痛宁的制剂原料盐酸青藤碱中三氯甲烷残留量的测定方法。方法：采用顶空进样气相色谱法进行测定,使用Agilent DB-5MS毛细管色谱柱（30.0 m×250μm,涂层0.25μm）,载气为高纯氮气,流量2 m L·min^-1,进样量为1m L,分流比10∶1,进样口温度为200℃,柱温为60℃,采用电子捕获检测器,检测器温度为200℃;顶空进样法,水为溶剂,平衡温度为60℃,平衡时间30 min。结果：三氯甲烷在0.242 7~97.06 ng·m L^-1范围内呈良好的线性关系（r2=0.998 4）;平均回收率为98.48%,RSD为1.69%（n=6）;最低定量限为4.854 ng·g^-1。所检测6个批次的正清风痛宁制剂原料中三氯甲烷残留量介于0至237.6 ng·g^-1之间。结论：顶空气相色谱（HS-GC）-电子捕获检测器（ECD）法灵敏、准确,优于现有其他检测方法,可作为盐酸青藤碱中三氯甲烷残留的检测方法,有利于提高制剂的安全性。
Objective： To establish a method to determine the residual chloroform in the raw material of sinomenine hydrochloride in Zhengqing Fengtongning. Methods： A headspace gas chromatography（ HS-GC） method was established for the determination by using Agilent DB-5MS capillary column with the length of 30 meters,the internal diameter of 250 μm and the film thickness of 0. 25 μm. The high purity nitrogen was used as the carrier gas with the flow of 2 m L·min^-1. The injection volume was 1 m L with the split ratio of 10∶ 1. The injector temperature was 200℃,the column temperature was 60 ℃,and the detector temperature of electron capture detector（ ECD） was 200℃. Water was used as the solvent,and the sample was equilibrated at 60℃ for 30 min before detection. Results：The calibration curve showed a good linearity within the range of 0. 242 7-97. 06 ng·m L^-1（ r2= 0. 998 4）. The lower limit of quantification was 4. 854 ng ·g^-1. The repeatability of method was acceptable with the RSD of0. 72%. The average recovery of chloroform was 98. 48%（ RSD = 1. 69%,n = 6）. The contents of chloroform in different batches of sinomenine hydrochloride were detected to be in the range of 0 to 237. 6 ng·g^-1. Conclusion：The method is sensitive,accurate,precise and reliable to determine residual chloroform in sinomenine hydrochloride,which is superior to other detection methods and good for improving the safety of pharmaceutical preparations.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2015年第9期1645-1648,共4页
Chinese Journal of Pharmaceutical Analysis
