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机构地区:[1]苏州市食品药品检验所,江苏苏州215104 [2]苏州市中医医院,215006
出 处:《中国执业药师》2016年第7期7-11,共5页China Licensed Pharmacist
基 金:苏州市"科教兴卫"青年科技项目(KJXW2015028)
摘 要:目的:建立同时测定珠黄散中胆酸、猪去氧胆酸、去氧胆酸、鹅去氧胆酸含量的方法。方法:以甲醇为提取溶剂,制备供试品溶液应用于薄层色谱扫描法,使用硅胶G高效薄层板,以异辛烷-乙酸乙酯-冰醋酸(15∶7∶6)为展开剂,10%硫酸乙醇溶液为显色剂,460 nm为测定波长,进行薄层定量扫描。结果:胆酸、猪去氧胆酸、去氧胆酸、鹅去氧胆酸分别在0.20~2.00μg(r≥0.999)内含量与峰面积积分值呈良好的线性关系,平均回收率(n=6)分别为95.88%(RSD=1.86%),97.43%(RSD=2.23%),96.24%(RSD=2.78%),96.63%(RSD=1.87%)。测得12批珠黄散中4种胆汁酸平均含量分别为31.94,6.36,20.19,10.53 mg/g。结论:该方法专属性强,重复性好,适用于珠黄散中4种胆汁酸的含量测定及质量控制。Objective : To develop a method for simultaneous determination of contents of four bile acids,i.e.cholic acid,hyodeoxycholic acid,deoxycholic acid and chenodeoxycholic acid,in zhuhuang san.Methods : Test sample solution was prepared for TLCS using methanol as an extraction solvent.Silica gel prefabricate thin layer plate was used with isooctane- ethyl acetate- glacial acetic acid(15∶7∶6) as a developing solvent and 10% alcoholic solution of sulfuric acid as a color development reagent.TLCS was performed at a detection wave-length of460 nm.Results : There was a good linear relation between the integrated peak area and the contents of four bile acids at a range of 0.20 ~ 2.00 μg(r ≥ 0.999).The average recovery rates(n = 6) of cholic acid,hyodeoxycholic acid,deoxycholic acid and chenodeoxycholic acid were 95.88%(RSD = 1.86%),97.43%(RSD = 2.23%),96.24%(RSD = 2.78%) and 96.63%(RSD = 1.87%) respectively.The average contents of the above-mentioned four bile acids in 12 batches of zhuhuang san were 31.94,6.36,20.19 and 10.53 mg/g respectively.Conclusion : The method showed high specificity and reproducibility,which was suitable for the determination of contents of four bile acids in Zhuhuang San.
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