“和胃饮合剂”中橙皮苷、厚朴酚的定性定量分析方法研究

目的为“和胃饮合剂”建立完整的定性定量方法。方法采用薄层色谱（TLC）和高效液相色谱（HPLC）的方法。Hypersil C18柱（200mm×4．6mm，5μm）；流动相甲醇-1％醋酸溶液，梯度洗脱（0～30min，甲醇浓度由30％递升至70％；30～40min，甲醇浓度由70％递升至80％；40～50min，甲醇浓度由80％递减至30％）；流速1．0mL／min；柱温为室温；检测波长294nm。结果测得标准品的工作曲线分别为：橙皮苷Y=139．718X＋4．511，线性相关系数为0．99994，线形范围0．5～6mg／ml；厚朴酚Y=1456．342X＋106．506，线性相关系数0．99957，线形范围0．5—6mg／ml。在上述条件下，用本方法测橙皮苷：精密度试验RSD=1．87％（n=5），加标回收率106．2％（RSD=2．628％，／Z：6）；测厚朴酚：精密度试验RSD：0．34％（n=5），加标回收率98．62％（RSD=3．093％，n=6）。用此法测定6批不同批号的样品，结果良好。结论本法可以作为“和胃饮合剂”中生理有效成分橙皮苷、厚朴酚的定性鉴别和定量测定方法加以推广运用。

The Research of Qualitative and Quantitative Method for the Determination of Hesperidin,Magnolol from “He - Wei - Yin” Mixture

Objective To develop a method for the determination of Hesperidin, magnolol from “He - Wei - Yin” Mixture, and for its quality control, high - performance liquid chromatography （HPLC） is used. Method After plenty of study about the condition, the final result choosed was as following： an analytical column of HypersiCls （200mm μ 4.6mm,5μm ） maked by HP was utilized. The column number was 13164421196. The mobile phase was adapted gradient with methanol - 1% aeetum solution, according to the following profile： 0 - 30min, methanol concentration from 30% to 70% ;30 -40min,from 70% to 80% ;40 -50min, from 80% to 30%. The flow rate was 1.0ml/min with the column kept at ambient temperature. All the components had come out in 45 min with the detection wavelength at 294nm. It followed the order of Heperidin, Magnolol according to the retention times in the chromatography. Results In the result,the regression equations were as following： Hesperidin was Y = 139. 718X ＋ 4. 511 with a good linearity （ r = 0. 99994）. Magnolol was Y = 1456. 342X ＋ 106. 506 with a good linearity （ r = 0. 99957） between the peak area and the mass of the standard. The recoveries of the method were as following： in the “He -Wei - Yin” Mixture, for hesperidin,precision of the method RSD = 1.87% （n = 5 ） , recovery of the method 96.53% （ RSD = 3.36% ,n = 3） ;for Magnolol,precision of the method RSD = 0.34% （ n = 5） ; recovery of themethod 93.17% （ RSD =4.69% ,n = 3）. At the same condition as above, the determination of content was carried out for six different dose and batch No. Conclusion The method is simple and reliable, easy to operate, suitable for the quality control of Hesperidin and Magnolol in “He - Wei - Yin” Mixture.