土家药红黑二丸质量标准研究

Study on the Quality Standard of Tujia Herbal Hong Hei Er Pill

目的:建立土家药红黑二丸药材的质量标准。方法:研究红黑二丸药材的性状、显微特征;采用TLC法,以β-谷甾醇为指标成分,环已烷-三氯甲烷-乙酸乙酯-冰醋酸(20∶5∶8∶0.1)为展开剂,进行红黑二丸薄层鉴别研究;采用HPLC法,色谱柱为Agilent 5 TC C18(2)柱(250 mm×4.6 mm,5μm),流动相为乙腈-异丙醇(70∶30),流速0.8 mL/min,检测波长210 nm,柱温30℃,测定红黑二丸中β-谷甾醇含量。结果:显微鉴别中根茎横切面显微特征明显,粉末组织特征明显;薄层色谱中特征性斑点清晰可见;HPLC中β-谷甾醇进样量在0.1978~3.9560μg范围内线性良好(r=0.9999),平均回收率为97.3%,RSD为2.9%。结论:红黑二丸的显微、TLC鉴别方法可行,HPLC含量测定方法简单、快速、准确,建立的土家药红黑二丸标准可用于其质量控制。

Objective:To establish the quality standard of Tujia Herbal Hong hei er pill.Methods:Study on the characters and microscopic characteristics of Tujia Herbal Hong hei er pill;the TLC method was used to identify Hong hei er pill withβ-sitosterol as index component and cyclohexane-trichloromethane-ethyl acetate-glacial acetic acid(20∶5∶8∶0.1)as developing agent;the content ofβ-sitosterol in Hong hei er pill was determined by HPLC with Agilent 5 TC C18(2)column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-isopropanol(70∶30),the flow rate was 0.8 mL/min,the detection wavelength was 210 nm,and the column temperature was 30℃.Results:In the microscopic identification,the transverse section of rhizome has obvious microscopic characteristics,and the powder structure characteristics are obvious;the characteristic spots were clearly visible in TLC;in HPLC,the linear range ofβ-sitosterol was 0.1978-3.9560μg(r=0.9999),the average sample recovery was 97.3%,RSD was 2.9%.Conclusion:The results showed that the identification method of Hong hei er pill by microscope and TLC was feasible,and the HPLC content determination method was simple,fast and accurate.The established standard of Tujia Herbal Hong hei er pill can be used for its quality control.