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Study on the Analysis Method, Process of Extraction and Purification of Camptothecin

Author: MaYunChao
Tutor: XieWenMing
School: Jilin Agricultural University
Course: Pesticides
Keywords: Camptothecin Extract Purification Reflux Macroporous resin
CLC: TQ450
Type: Master's thesis
Year: 2007
Downloads: 531
Quote: 1
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Abstract


This thesis hi leaves as raw material extraction and purification process of camptothecin, explore a high extraction rate of purification effect good process route study to establish the applicability of camptothecin analysis, stability good camptothecin HPLC analysis method. Identified camptothecin Soxhlet extraction - HPLC method: using methanol as the extraction solvent, extraction temperature of 80 ° C, extraction time 6h as a pre-processing methods of sample analysis, SinoChrom ODS-BP column, detector wavelength 254nm, acetonitrile / water (40:60, V / V) as mobile phase HPLC analysis method. The method in 3.55 ~ 71μg mL -1 of a good linear relationship in the concentration range, the average recoveries of 95.4%, the relative standard deviation (RSD) was 2.52%. The impregnation method reflux method, and soda extraction process hi leaves camptothecin analysis by single factor and orthogonal experiment to optimize the extraction process, the impregnation method optimum extraction conditions were as follows: 65% methanol solid to liquid ratio of 1:8, and extracted for 48 hours, proven this condition, the average extraction rate of 0.318 ‰ camptothecin; the reflux method optimum extraction conditions were as follows: 65% methanol, solid-liquid ratio 1:10, extraction 1h, extraction temperature 70 ℃, extraction time, under the conditions of the proven camptothecin average extraction rate of 0.490 ‰; verification Wang Yang proposed soda extraction process, the average extraction process camptothecin rate of 0.0746 ‰. The three extraction methods can be seen: Extraction was refluxed for a short time, high extraction efficiency, extract treatment is simple, the process is stable and reliable, so experiments using reflux extraction process. By static adsorption - desorption experiments, from five commonly macroporous adsorption resin filter out with a larger amount of adsorption and desorption rate of AB-8 resin as a column filler, AB-8 resin camptothecin static adsorption amount 16.68mg g -1 , 95% ethanol static desorption rate was 92.4%; the camptothecin crude extract purification process to determine the optimum adsorption conditions: the sample concentration was 0.175 the mg mL -1 , on the kind of solution does not adjust the pH value, adsorption flow rate of 2BV h -1 , equilibrium adsorption 5h; optimal elution conditions: eluent 95% ethanol, the elution rate as 1BV H -1 , the eluted amount 8BV eluate camptothecin purity of 7.43%, under the process conditions, the elution rate reached 83.1% .

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