蒙药砂蓝刺头定性与定量质量控制方法研究

目的建立砂蓝刺头Echinops gmelini的质量控制方法。方法采用薄层色谱法,以三氯甲烷-醋酸乙酯-甲醇-甲酸(6∶1∶1∶0.8)为展开剂对砂蓝刺头花中1-甲基-4-甲氧基-8-(β-D-葡萄吡喃型糖苷)-2(1H)-喹啉酮(MMQ)进行定性鉴别;建立砂蓝刺头HPLC指纹图谱,并对MMQ的含量测定方法进行研究。结果建立的TLC方法对照品斑点清晰,分离度好;建立的指纹图谱分析方法能够区分砂蓝刺头与近源植物,标定了8个特征峰,并指认出其中4个成分。定量方法测定结果显示MMQ在2.024~151.800μg/mL呈良好线性关系,平均加样回收率为101.54%,RSD为1.46%。7批样品中MMQ的质量分数为0.13%~0.53%。结论建立的质量控制方法科学、可靠,可为砂蓝刺头质量标准的建立提供实验依据。

Study on qualitative and quantitative control method for Echinops gmelini

Objective To establish the quality control method for of Echinops gmelini. Methods Thin layer chromatography(TLC) method was used for quanlitative analysis of the 1-methyl-4-methoxy-8-(β-D-glucopyranoside)-2(1H)-quinolinone(MMQ) with a mixture of trichloromethane-ethyl acetate-methanol-formic acid(6∶1∶1∶0.8) as the developing solvent. The HPLC fingerprint of the capitulum of E. gmelini and the determination of MMQ were conducted by HPLC. Results The spots on TLC plate were clear, well-separated and specific without any interference. The linear range of calibration curve was 2.024—151.800 μg/mL, and the average recovery was 101.5% with RSD of 1.46%, which can be used for the quality control of E. gmelini. The contents of MMQ in seven batches of E. gmelini were 0.13%—0.53%. Conclusion The qualitative and quantitative determination method is scientific and reliable, which can provide an experimental basis for the establishment of the quality standard of E. gmelini.