十味益脾颗粒的质量标准提升研究

目的:为提升十味益脾颗粒的质量标准提供参考。方法:按2015年版《中国药典》(四部)通则相关方法,采用显微鉴别法鉴别六神曲和鸡内金药材,薄层色谱法(TLC)鉴别山楂和莱菔子药材,高效液相色谱法(HPLC)测定莱菔子中芥子碱硫氰酸盐的含量。结果:十味益脾颗粒中六神曲(种皮栅状细胞和种皮石细胞)和鸡内金(不规则碎块)的显微特征明显;山楂、莱菔子药材与熊果酸、芥子碱硫氰酸盐对照品和莱菔子对照药材在相应位置处显相同的荧光斑点。芥子碱硫氰酸检测进样量的线性范围为23.27～9 574.42 ng(r=1.000 0),检测限为0.50μg/m L、定量限为1.68μg/mL;精密度、重复性、中间精密度、稳定性(24 h)试验的RSD均小于1.5%,平均回收率为99.40%～100.89%(RSD为0.18%～0.49%,n=3)。3批十味益脾颗粒中芥子碱硫氰酸盐的含量为0.086 4～0.220 6 mg/g,平均值为0.168 4 mg/g。结论:成功建立十味益脾颗粒中六神曲、鸡内金、山楂、莱菔子药材的鉴别方法和莱菔子中芥子碱硫氰酸盐的含量测定方法;该品含莱菔子以芥子碱硫氰酸盐(C16H24N...

Study on Improvement of Quality Standards of Shiwei Yipi Granules

OBJECTIVE:To provide reference for the improvement of quality standards of Shiwei yipi granules.METHODS:According to the general rules of 2015 edition of Chinese Pharmacopeia(partⅣ),microscopic identification was used to identify Massa Medicata Fermentata and Galli Gigerii Endothelium Corneum;TLC method was used to qualitatively identify Crataegi Fructus and Semen Raphani;the content of sinapine thiocyanate in Semen Raphani was determined by HPLC.RESULTS:The microscopic characteristics were obvious for Massa Medicata Fermentata(palisade cells of testa and stone cells of testa)and Galli Gigerii Endothelium Corneum(irregular fragments).The same fluorescent spots of Crataegi Fructus and Semen Raphani were displayed at the same position of ursolic acid,sinapine thiocyanate control and Semen Raphani reference substance.The linear range of sinapine thiocyanate was 23.27-9574.42 ng(r=1.0000).The LOD and LOQ were of 0.50μg/mL and 1.68μg/mL,respectively.RSDs of precision,repeatability,intermediate precision and stability tests(24 h)were all less than 1.5%.The average recoveries were 99.40%-100.89%(RSDs were 0.18%-0.49%,n=3).The contents of sinapine thiocyanate in 3 batches of Shiwei yipi granules were 0.0864-0.2206 mg/g,the average was 0.1684 mg/g.CONCLUSIONS:The identification method of Massa Medicata Fermentata,Galli Gigerii Endothelium Corneum,Crataegi Fructus and Semen Raphani in Shiwei yipi granules as well as the method for content determination of sinapine thiocyanate in Semen Raphani are established successfully.The content of Semen Raphani in the Shiwei yipi granules is no less than 0.16 mg/g calculated by sinapine thiocyanate(C16H24NO5·SCN).