文档介绍：5种大黄蒽醌类衍生物的同时测定及应用
【摘要】  目的建立同时测定大黄药材中5种蒽醌类衍生物(芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚)含量的方法,优化大黄蒽醌的超声提取工艺。方法采用反相高效液相法,色谱柱:Waters C18柱(250 mm× mm, 5 μm);流动相:甲醇-乙腈-%磷酸溶液(3∶5∶2);柱温:25 ℃;流速: ml/min;检测波长:225 nm。结果5种游离蒽醌均具有较宽的线性范围且呈良好的线性关系(R2= 7~ 7),%~%,%~%,%~%。结论该方法成功应用于大黄活性物质的提取工艺优化,根据所建立的方法测得的5种游离蒽醌含量,确定了大黄蒽醌的最佳超声提取工艺为:以70%乙醇为溶剂、料液比为1∶30 (g∶ml)、超声提取2次、每次提取20 min。
【关键词】  超声提取; 大黄; RP-HPLC; 蒽醌
Abstract:ObjectiveTo develop a method for the simultaneous determination of five anthraquinone derivatives (aloe-emodin, rhein, emodin, chrysophanol and physcion) in rhubarb, and to optimize the ultrasonic extraction -HPLC on a Waters C18 column (250 mm× mm, 5  μm) was used. The mobile phase was methanol-acetonitrile-% phosphoric acid solution (3:5:2), at a flow rate of ml/min, and the detection wavelength was 225 nm. ResultsThe linear ranges of the five free anthraquinones were wide, showing good linear correlations with correlation coefficients (R2) of to . The average recoveries were from % to %. While the intra-day and inter-day precision were %~% and %~%, the contents of five anthraquinone derivatives obtained by the developed RP-HPLC method, the optimum ultrasonic extraction conditions are determined as follows: using 70% EtOH as extracting solvent, the sample is extracted two times and each time for 20 min by a ultrasonic processor, when the solid to liquid ratio is 1:30 (g/ml).
Key words:Ultrasonic extraction;  Rhubarb;  RP-HPLC;  Anthraquinones
    
大黄Radix et Rhizoma Rhei为蓼科植物掌叶大黄Rheum Palmatum L.,唐古特大黄Rheum tanguticum Maxim. ex Balf 或药用大黄Rheum officinale Baill的干燥根和根茎,味苦、性寒。临床研究证实,大黄具有抗衰老、降血脂、抗肿瘤和抗炎、泻下作用及抗菌性、止血性等多种生物学活性[1]。其主要有效成分为蒽醌类衍生物,包括芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚以及与葡萄糖结合成苷。5种蒽醌是大黄以及衍生中药大黄属[2]质量控制的基础。 
    
大黄中蒽醌的分离和测定方法有薄层色谱法(TLC)[3],高速逆流色谱法()[4,5],胶束电动毛细管色谱法(MEKC)[6],毛细管区带电泳法(CZE)[7],高效液相色谱法(HPLC)[8],加压毛细管电色谱(pC