大黄及其醇提液HPLC特征图谱相关性研究

Analysis on Correlation of HPLC Specific Chromatogram of Rhei Radix Et Rhizoma and its Ethanol Extract

目的:建立大黄HPLC特征图谱分析方法,研究大黄与其醇提液HPLC特征图谱的相关性,评价大黄醇提工艺。方法:采用Zorbax SB-Aq C18色谱柱;流动相为乙腈-0.1%的磷酸溶液(梯度洗脱);检测波长430,280 nm,柱温为40℃,流速1.0 mL.min-1。结果:大黄及其醇提液在430 nm波长条件下均标示出14个蒽醌类共有峰,其中鉴别了5个游离蒽醌类成分,10批大黄及其醇提液中有8批样品相似度分别>0.96及0.95,2批样品差异较大,相似度<0.90;在280 nm波长条件下标示出10个共有峰,其中鉴别了2个特征成分,10批大黄及其醇提液中有8批样品相似度>0.94及0.92,2批相似度低于0.90。同批次大黄及其醇提液在430,280 nm波长处的相似度分别为0.992～0.999,0.987～0.999,表明大黄的常规醇提工艺能保留大黄饮片的主要特征成分。结论:方法准确可靠,重复性好,为大黄饮片及其醇提液的质量控制提供方法依据,并为大黄复方制剂的工艺与质量控制提供了参考。

Objective： To establish the method of specific chromatogram analysis of Rhei Radix Et Rhizoma by HPLC, and to study the correlation between Rhei Radix Et Rhizoma and its ethanol extract and to estimate the alcohol extracting technology. Method： HPLC was used with the Zorbax SB-Aq Cls column, the acetonitrile-phosphoric acid solution （Ф = 0. 1% ） （gradient elution） was employed as a mobile phase, detection wavelength was at 430 nm and 280 nm, column temperature was set at 40 ℃ , and flow rate was 1.0 mL .min-1 Result： Fourteen common peaks were separated in the decoction pieces and its ethanol extract of Rhei Radix Et Rhizoma and 5 peaks were identified in 430 nm, the similarities of 8 batches of the decoction pieces and ethanol extract were over 0.96 and 0.95, the similarities of the other 2 batches were below 0.90. 10 common peaks were separated in the decoction pieces and its ethanol extract and 2 peaks were identified in 280 nm, the similarities of 8 batches of the decoction pieces and ethanol extract were over 0.94 and 0.92, the similarities of the other 2 batches were below 0.90. The similarities between the decoction pieces and its ethanol extract were 0. 992-0. 999 in 430 nm and 0. 987-0. 999 in 280 nm, which respectively indicates that the traditional alcohol extracting technology of Rhei Radix Et Rhizoma can reserve the main characteristic component. Conclusion： The method is reliable, accurate and reproducible, which can be used for the quality control of the decoction pieces and ethanol extract ofRhei Radix Et Rhizoma as well as for compound preparation containing Rhei Radix Et Rhizoma.