Studies On Chemical Constituents Analysis And Preparative Technologies From Cinnamomi Ramulus

Clear chemical constituents and exact pharmacological activities were two important parts for traditional Chinese medicine modernization. Preparative chromatography as a crucial technology for separation was not systematical and repeatable. This study using Cinnamomi ramulus as the subject centered on preparative chromatography discussed chromatography pre-treatment technologies and methods of condition screening and process parameters prediction and the separateness for chromatography separation which wished to build a repeatable large-scale and high purity separation method.Pre-treatments including extract, precipitation and the adjustment of pH in Cinnamomi ramulus were studied detected by TLC and HPLC. The results showed that extracted by n-hexane and ethyl acetate distributed all components into three different parts which simplified the complexity of samples and reduced the difficulty of separation. Precipitations containing ethanol precipitation and salting-out did not work out obviously. The adjustment of pH value resulted in changes of chemical constructure of some composition which were bad for the systematic separations.Based on the same theory of separation between TLC and column chromatography, rules for selection of chromatographic conditions involved separation mode and elution systems were investigated directed by thin layer ohromatography.The results showed that the best separation mode was normal phase chromatography and the packing was silica gel and the best elution systems were n-hexane/ethyl acetate and n-hexane/acetone for which separation results were similar.Comparisons with the same solvent strength for two elution systems indicated that ethyl acetate would minish the width of spots and was more suitable. Function between capacity factor(k) of analysts and the volume fraction of solar solvents in binary mixture was lnk=a+blnC+cC. Preparative chromatogram parameters including elution volumes of each solvents and the retention volume of each analyte were estimated from thin-layer chromatography data.8pure fractions with one single spot in TLC were isolated and the purity of5component were great than95%detected by HPLC. Four continuous TLC were developed as a pilot technique for the optimization of gradient liquid chromatography. Linear relationship were found between the Rf value of analytes and the times of development and the slope differed from solvent strength and analytes structure.Finally the separableness between adjacent spots were discussed in TLC and preparative chromatography which shows that analytes were separated completely when△Rf was greater than0.06and the Rf values of material series range from0.1to0.3.For a preparative chromatography column size of4cm×30cm, the suitable load mass was1.2g which would be calculated by the function of Sg=151.2SSsio2+0.5.