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利用超临界二氧化碳对秋水仙块根(经粉碎)中的秋水仙碱进行了萃取,采用高效液相色谱法对萃取出的秋水仙碱的质量分数进行了测定。实验选择40℃20~40MPa作为超临界苹取的操作条件,采用体积分数为95%的乙醇在索氏提取器中对样品进行了对比苹取实验。结果表明:不加浸泡剂进行浸泡处理的样品中的秋水仙碱很难被超临界二氧化碳萃取,在40℃,35MPa条件下,消耗1.28mol的二氧化碳只得到3%的萃取率。加入极少量的有机溶剂浸泡处理样品15min后再进行超临界萃取,可以极大程度地提高秋水仙碱的萃取率。在所选的浸泡剂乙醚、丙酮、乙腈、甲醇、乙醇中,乙醇浸泡效果最佳,经浸泡后,在40℃,35MPa条件下进行超临界二氧化碳萃取,仅消耗0.21mol的二氧化碳,一次苹取的秋水仙碱萃取率就达80%。秋水仙碱的质量分数从原植物样品中的0.18%提高到萃取物中的6.92%,提高了近38倍,而有机溶剂乙醇提取只能达到0.98%,仅提高了5倍。超临界苹取后的样品经简单的过滤即可进样进行HPLC分析,有机溶剂乙醇提取则需要氯仿苹取、溶剂回收等样品制备过程。HPLC分离测定秋水仙碱采用苯基柱,甲醇-水梯度洗脱,流速0.5mL/min,UV检测λ=353um,经选择,其最佳条件为:从V(甲醇):V(水)=50:50开始,15min内到V
The colchicine was extracted from the roots (crushed) of daffodils by supercritical carbon dioxide, and the mass fraction of extracted colchicine was determined by high performance liquid chromatography (HPLC). The experiment selected 40 ~ 40 ℃ 20 ~ 40MPa as the operating conditions of supercritical extraction, using 95% volume fraction of ethanol in the Soxhlet extractor samples were compared to take the test. The results showed that colchicine in samples soaked with no soaking agent was hard to be extracted by supercritical carbon dioxide. At 35 ℃ and 40 ℃, 1.28mol of carbon dioxide consumed only 3% of the extraction rate. Adding a very small amount of organic solvent immersion treatment samples 15min and then supercritical extraction, can greatly improve the colchicine extraction rate. In the selected soaking agent ether, acetone, acetonitrile, methanol, ethanol, the best ethanol soaking, after soaking, at 40 ℃, 35MPa under the conditions of supercritical carbon dioxide extraction, only consumes 0.21mol of carbon dioxide, an apple Take colchicine extraction rate of up to 80%. The mass fraction of colchicine increased from 0.18% in the original plant sample to 6.92% in the extract, nearly 38 times higher, while the organic solvent ethanol extract only reached 0.98%, only 5 Times After supercritical extraction of the sample by simple filtration can be injected for HPLC analysis, organic solvent ethanol extraction is required chloroform extraction, solvent recovery and other sample preparation process. The optimal conditions for the determination of colchicine were as follows: V (methanol): V (water) at pH = 353um with UV detection at a flow rate of 0.5mL / min. = 50:50 start, within 15min to V