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作 者:陈勇[1] 邓家刚[1] 王勤[1] 刘婧[1] 潘丽娜[1] 丁光华[1]
出 处:《中国实验方剂学杂志》2007年第6期11-13,共3页Chinese Journal of Experimental Traditional Medical Formulae
摘 要:目的:建立抗痛风颗粒中青风藤的TLC定性鉴别方法和青藤碱的高效液相色谱含量测定方法。方法:以青藤碱为对照品,采用甲苯-乙酸乙酯-甲醇-氨水(2∶4∶2∶1)为展开剂,改良碘化铋钾溶液为显色剂,对抗痛风颗粒中青风藤进行薄层色谱法定性鉴别。采用Agilent extend C18柱(4.6 mm×150 mm,5μm),甲醇-0.1%磷酸溶液(用三乙胺调pH至10)(38∶62)为流动相,262 nm为检测波长,测定了抗痛风颗粒中青藤碱的含量。结果:抗痛风颗粒薄层色谱中,青藤碱斑点清晰,阴性对照无干扰。HPLC定量分析中,青藤碱线性范围为0.414~2.484μg(r=0.999 8),平均回收率为97.6%,RSD=0.32%。结论:所建立的分析方法简便可行,可用于该制剂的质量控制。Objective: To develop a TLC method for Caulis Sinomenii indentification and a HPLC method for Sinomenine determination in the anti gout granules. Methods: Caulis Sinomenii was identified on a silicagel thin layer plate dev reference eloped with methylbenzene : acetidin: methanol : ammonia water (2 : 4 : 2 : 1 ) and with sinomenine as the chemical substance, improved. Dragendorff reagent was used for visualization. The separation of Sinomenium was carried out on column Extend C18 4.6 mm × 150 mm, 5 μm. The mobile phase was the combination of methanol and the solution of 0.1% phosphoric acid(38:62), and the detection wareleng the was set at 262 nm. Result: Sinomenine spots on TLC plates was separated detection warelength well. The linear range is between 0.414 and 2.484 μg ( r = 0.999 8) and the recovery is 97.6% (RSD = 0.32% ). Conclusions: The methods are sensitive, simple; accurate and can be used for the control of anti gout granules.
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