回春育子颗粒质量标准研究

目的 提高回春育子颗粒的质量标准.方法 采用薄层色谱(TLC)法对制剂中的当归、熟地黄、川续断和甘草进行定性鉴别;采用高效液相色谱(HPLC)法测定制剂中原儿茶酸、阿魏酸、柚皮苷、淫羊藿苷和五味子醇甲的含量,色谱柱为Waters Symmetry C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.4％磷...

Quality Standard of Huichunyuzi Granules

Objective To improve the quality standard of Huichunyuzi Granules.Methods Thin-layer chromatography(TLC)method was used for the qualitative identification of Angelicae Sinensis Radix,Rehmanniae Radix Praeparata,Dipsaci Radix,Glycyrrhizae Radix et Rhizoma.High-performance liquid chromatography(HPLC)method was used for the content determination of protocatechuic acid,ferulic acid,naringin,icariin and schisandrin.The chromatographic column was Waters Symmetry C₁₈ column(250 mm×4.6 mm,5μm),the mobile phase was methanol-0.4%phosphoric acid solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelengths were 260 nm(protocatechuic acid),320 nm(ferulic acid),283 nm(naringin),270 nm(icariin)and 250 nm(schisandrin),the column temperature was 35℃,and the injection volume was 10μL.Results The TLC spots of Angelicae Sinensis Radix,Rehmanniae Radix Praeparata,Dipsaci Radix,Glycyrrhizae Radix et Rhizoma were clear with good resolution,and the negative samples had no interference.The linear ranges of protocatechuic acid,ferulic acid,naringin,icariin and schisandrin were 1.10-55.09μg/mL(r=0.9996),0.96-48.36μg/mL(r=0.9981),0.14-7.11μg/mL(r=0.9979),2.83-141.46μg/mL(r=0.9993)and 1.00-49.97μg/mL(r=0.9986),respectively.The limits of detection(LOD)were 5.56,9.77,4.95,5.09 and 5.02 ng/mL,respectively.The limits of quantitation(LOQ)were 18.53,32.57,16.50,16.97 and 16.73 ng/mL,respectively.The RSDs of precision,stability and reproducibility tests were lower than 2.0%(n=6).The average recoveries of protocatechuic acid,ferulic acid,naringin,icariin and schisandrin were 94.50%,92.28%,99.77%,98.54%and 99.14%with RSDs of 1.61%,0.75%,1.34%,0.90%and 1.01%(n=6),respectively.Conclusion The method is simple,accurate,reliable,reproducible and stable,which can be used for the quality control of Huichunyuzi Granules.