采用HPLC法测定葡糖醛酸筛选葡醛内酯片制备方法

Determination of Glucuronic Acid by HPLC to Screen the Preparation Method of Glucuronolactone Tablets

目的:制备葡醛内酯片,采用HPLC(高效液相色谱法)法测定葡醛内酯片中葡糖醛酸的含量,筛选制备方法,并为葡醛内酯片的质量控制提供参考。方法:以片芯收率为指标,采用正交分析确定基本处方,并运用不同的制粒方法制备葡醛内酯片(50mg规格);采用HPLC(高效液相色谱法)法分析测定不同制法的葡醛内酯片中葡糖醛酸含量,筛选出最优的制备方法。结果:采用HPLC法葡糖醛酸与碱降解峰之间分离度均大于1.5,呈良好线性关系,回收率为90%~108%,精密度,重复性、专属性良好,同时该方法需临用前制备,2~8℃冰箱保存下20min内稳定。以乳糖占比30%,低取代羟丙纤维素占比4%,葡醛内酯粒径为40目作为基本处方,按同一处方不同制备方法自制制剂,分析葡糖醛酸含量结果表明干法制粒与流化床制粒下葡醛内酯片的葡糖醛酸含量较低。结论:HPLC(高效液相色谱法)方法灵敏,专属性好,可用于葡醛内酯片中葡糖醛酸的测定;葡醛内酯片干法制粒与流化床制粒工艺更好。

Objective:The content of glucuronic acid in glucurolactone tablets was determined by HPLC(high performance liquid chromatography),and the reference was provided for the quality control of glucurolactone tablets.Methods:Taking the core yield as the index,the basic formula was determined by orthogonal analysis,and the glucurolactone tablets(50 mg)were prepared by different granulation methods;The content of glucuronic acid in different preparation methods of glucuronolactone tablets was determined by HPLC,and the best preparation method was selected.Results:The resolution between glucuronic acid and alkaline degradation peak by HPLC is greater than 1.5,showing a good linear relationship.The recovery rate is 90%~108%,and the precision,repeatability and specificity are good.At the same time,the method needs to be prepared before use,and it is stable within 20 minutes after being stored in a refrigerator at 2~8℃.With lactose accounting for 30%,low substituted hydroxypropyl cellulose accounting for 4%,and glucuronolactone particle size of 40 mesh as the basic prescription,self-made preparations were prepared according to different preparation methods of the same prescription.The analysis of glucuronic acid content showed that the glucuronic acid content of glucuronolactone tablets under dry granulation and fluidized bed granulation was low.Conclusion:HPLC(high performance liquid chromatography)method is sensitive and specific,and can be used for the determination of glucuronic acid in glucuronolactone tablets;The dry granulation and fluidized bed granulation of glucurolactone tablets are better.