乌芪舒筋通络片中乌头碱限量检测方法研究

摘要

目的:建立测定乌芪舒筋通络片中乌头碱限量的方法.方法:采用薄层色谱(TLC)法对制剂中的乌头碱进行鉴定.薄层板为硅胶G薄层板,展开剂为甲苯-乙酸乙酯-三氯甲烷-丙酮-氨水(20:18:3:6:1,V/V/V/V/V),显色剂为稀碘化铋钾试液和亚硝酸钠乙醇试液.经耐用性和检测限考察,并优选薄层板、温度和湿度.结果:乌头碱的TLC图斑点清晰且阴性对照无干扰.本试验耐用性良好;检测限为0.9 μg;可用薄层板为Merck HPTLC预制板、硅胶G薄层板和自制的以羧甲基纤维素钠为黏合剂的硅胶G薄层板;温度为5~16℃,湿度为32%~72%.结论:本方法操作简便、重复性良好,可用于乌芪舒筋通络片中乌头碱限量的测定.%OBJECTIVE:To establish a method for the limit detection of aconitine in Wuqi shujin tongluo tablet. METHODS:TLC was conducted to identify the aconitine;TLC plate was silica gel G plate,developing solvent was toluene-ethyl acetate-chloro-form-acetone-ammonia(20:18:3:6:1,V/V/V/V/V),chromogenic agent was bismuth potassium iodide test solution and sodium ni-trite ethanol test solution;and durability investigation and detection limit detection were used to optimize the TLC plate,tempera-ture and humidity. RESULTS:TLC showed the aconitine had clear spots and negative control without interference. The durability was good;detection limit was 0.9 μg;available TLC plate was Merck HPTLC prefabricated plate, silica gel G TLC plate setf-made silica gel G TLC plate with adhesive of sodium carboxymethycellulose;temperature was 5-16 ℃ and humidity was 32%-72%. CONCLUSIONS:The method is simple and reproducibility,and can be used for the limit detection of aconitine in Wuqi shujin tongluo tablet.