中药材雷公藤中有效成分的提取与分离
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摘要
雷公藤(Tripterygium wilfordii Hook.f.)是一种传统的中药材,研究发现具有抗炎、抗菌、免疫抑制、抗生育、抗肿瘤等药理作用。目前雷公藤中药制剂被广泛用于治疗类风湿性关节炎,治疗效果显著,其中雷公藤甲素被公认为最主要的活性成分,而雷公藤红素则被认为是具有较大毒副作用。目前又有研究报道,雷公藤红素具有抗肿瘤等药理作用。如何分离雷公藤红素与甲素,一直是雷公藤制剂研究中急待解决的问题。因此,本文对雷公藤红素和雷公藤甲素的提取与分离技术进行了探讨,该研究对增效减毒问题的解决和新药的开发均具有重要意义。
本文采用先进的超临界CO2萃取技术从雷公藤带皮根部中高效地提取出同时含有雷公藤红素、雷公藤甲素以及其它有效成分的粗提物,然后,结合酸沉-碱化-乙酸乙酯萃取分离纯化手段将雷公藤红素和雷公藤甲素进行了有效分离。考察了不同浓度的盐酸、醋酸、柠檬酸对雷公藤有效成分分离的效果。采用HPLC仪器检测的结果表明,在优化得到的适宜工艺条件下,雷公藤甲素产品中已检测不到的雷公藤红素;而雷公藤红素产品中也检测不到雷公藤甲素。超临界流体萃取技术与后续分离方法的合理集成使雷公藤红素和雷公藤甲素在各自产品中的含量分别提高了1.7倍和5.3倍;雷公藤红素提取率为0.155 %,雷公藤红素在产品中的含量为17.72 %;雷公藤甲素的提取率为1.15×10-3 %,雷公藤甲素在产品中的含量为0.42 %。
本文还以雷公藤根皮为原料,以雷公藤红素提取率及含量为指标,进行单因素实验,确定超临界CO2萃取雷公藤红素的最佳萃取条件,优化实验结果显示,雷公藤红素提取率为0.33 %,含量为12.84 %;雷公藤甲素提取率为4.16×10-3 %,含量为0.33 %。比较了超临界流体萃取与一些传统提取方法在提取雷公藤红素的效果,表明超临界流体萃取雷公藤红素的提取率为传统方法的1.25-2.5倍,萃取物中雷公藤红素含量为传统方法的1.28-2.15倍,并避免了大量有机溶剂的使用以及减少萃取所用时间,确定了超临界CO2萃取方法提取雷公藤红素的优势。
Tripterygium wilfordii Hook.f. is a traditional Chinese herb which has many pharmacological effects such as anti-inflammation, antibacterial effect, immunosuppression, antifertility, anti-tumor and so on. So far most of products from Tripterygium wilfordii are crude extracts, in which triptolide is considered to have great curative effect on rheumatoid arthritis, but tripterine has been considered to have toxicity and side effects. And recently tripterine was found to be a great anti-tumor in spite of its toxicity. It is a problem all long that how to separate tripterine and triptolide. In this paper, with the help of advanced extraction and separation technologies, triptolide and tripterine are isolated with content improvements in their products respectively. The work in this thesis makes some contribution to the exploitation of new drugs and the problem of adding effect and reducing toxin.
Supercritical carbon dioxide extraction is used in the extraction of tripterine and triptolide and gives a high yield from the root with bark of Tripterygium wilfordii. Then a valid purification process of acidification-alkalization-organic solvent extraction was further employed to separate tripterine and triptolide. The HPLC results show that the content of tripterine in the product of triptolide is zero and the content of triptolide in another product of tripterine is also zero under the optimazed conditions. Meanwhile, the content of tripterine and triptolide in their own products concentrate by 1.7 and 5.3 times respectively. The yield of tripterine is 0.155 % and the content of tripterine in its products is 17.72 %. The yield of triptolide is 1.15×10-3 % and the content of triptolide in its products is 0.42 %.
Supercritical carbon dioxide extraction is also used to extract tripterine from the root bark of Tripterygium wilfordii. Optimum experimental results show the yield of tripterine is 0.33 % and the content of tripterine in its products is 12.84 %. The yield of triptolide is 4.16×10-3 % and the content of triptolide in its products is 0.33 %. Compared supercritical fluid extraction (SFE) with some traditional extraction methods, the results show the yield of tripterine by means of SFE is 1.25-2.5 times of traditional methods while content of tripterine is 1.28-2.15 times. SFE avoid using large amount organic solvent and reduce extraction time needed during the process.
本文采用先进的超临界CO2萃取技术从雷公藤带皮根部中高效地提取出同时含有雷公藤红素、雷公藤甲素以及其它有效成分的粗提物,然后,结合酸沉-碱化-乙酸乙酯萃取分离纯化手段将雷公藤红素和雷公藤甲素进行了有效分离。考察了不同浓度的盐酸、醋酸、柠檬酸对雷公藤有效成分分离的效果。采用HPLC仪器检测的结果表明,在优化得到的适宜工艺条件下,雷公藤甲素产品中已检测不到的雷公藤红素;而雷公藤红素产品中也检测不到雷公藤甲素。超临界流体萃取技术与后续分离方法的合理集成使雷公藤红素和雷公藤甲素在各自产品中的含量分别提高了1.7倍和5.3倍;雷公藤红素提取率为0.155 %,雷公藤红素在产品中的含量为17.72 %;雷公藤甲素的提取率为1.15×10-3 %,雷公藤甲素在产品中的含量为0.42 %。
本文还以雷公藤根皮为原料,以雷公藤红素提取率及含量为指标,进行单因素实验,确定超临界CO2萃取雷公藤红素的最佳萃取条件,优化实验结果显示,雷公藤红素提取率为0.33 %,含量为12.84 %;雷公藤甲素提取率为4.16×10-3 %,含量为0.33 %。比较了超临界流体萃取与一些传统提取方法在提取雷公藤红素的效果,表明超临界流体萃取雷公藤红素的提取率为传统方法的1.25-2.5倍,萃取物中雷公藤红素含量为传统方法的1.28-2.15倍,并避免了大量有机溶剂的使用以及减少萃取所用时间,确定了超临界CO2萃取方法提取雷公藤红素的优势。
Tripterygium wilfordii Hook.f. is a traditional Chinese herb which has many pharmacological effects such as anti-inflammation, antibacterial effect, immunosuppression, antifertility, anti-tumor and so on. So far most of products from Tripterygium wilfordii are crude extracts, in which triptolide is considered to have great curative effect on rheumatoid arthritis, but tripterine has been considered to have toxicity and side effects. And recently tripterine was found to be a great anti-tumor in spite of its toxicity. It is a problem all long that how to separate tripterine and triptolide. In this paper, with the help of advanced extraction and separation technologies, triptolide and tripterine are isolated with content improvements in their products respectively. The work in this thesis makes some contribution to the exploitation of new drugs and the problem of adding effect and reducing toxin.
Supercritical carbon dioxide extraction is used in the extraction of tripterine and triptolide and gives a high yield from the root with bark of Tripterygium wilfordii. Then a valid purification process of acidification-alkalization-organic solvent extraction was further employed to separate tripterine and triptolide. The HPLC results show that the content of tripterine in the product of triptolide is zero and the content of triptolide in another product of tripterine is also zero under the optimazed conditions. Meanwhile, the content of tripterine and triptolide in their own products concentrate by 1.7 and 5.3 times respectively. The yield of tripterine is 0.155 % and the content of tripterine in its products is 17.72 %. The yield of triptolide is 1.15×10-3 % and the content of triptolide in its products is 0.42 %.
Supercritical carbon dioxide extraction is also used to extract tripterine from the root bark of Tripterygium wilfordii. Optimum experimental results show the yield of tripterine is 0.33 % and the content of tripterine in its products is 12.84 %. The yield of triptolide is 4.16×10-3 % and the content of triptolide in its products is 0.33 %. Compared supercritical fluid extraction (SFE) with some traditional extraction methods, the results show the yield of tripterine by means of SFE is 1.25-2.5 times of traditional methods while content of tripterine is 1.28-2.15 times. SFE avoid using large amount organic solvent and reduce extraction time needed during the process.
引文
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