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利用微波能量优化从欧洲红豆杉中提取紫杉醇的工艺。

Optimization of the extraction of paclitaxel from Taxus baccata L. by the use of microwave energy.

作者信息

Talebi Mohammad, Ghassempour Alireza, Talebpour Zahra, Rassouli Ali, Dolatyari Lila

机构信息

Department of Chemistry, Faculty of Science, Shahid Beheshti University, Tehran, Iran.

出版信息

J Sep Sci. 2004 Sep;27(13):1130-6. doi: 10.1002/jssc.200401754.

Abstract

A simple and rapid microwave-assisted extraction (MAE) procedure was developed and optimized for the extraction of paclitaxel (Taxol) from the needles of yew trees Taxus baccata L. grown in Iranian habitats. The samples, immersed in a methanol-water mixture, were irradiated with microwaves in a closed-vessel system. The method was evaluated using a factorial design approach based on parameters such as extraction time, temperature, methanol concentration in water (v/v), and the ratio of grams of sample to 10 mL of solvent. Statistical treatment of the results revealed that the selected parameters were all significant except the extraction time. Optimum conditions would be 1.5 g samples in 10 mL solvent (90% methanol), an extraction temperature of 95 degrees C, and an extraction time of 7 min. The extracts has been analyzed by reverse-phase high-performance liquid chromatography with UV detection (LC/UV) at 227 nm for quantification. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) was used for confirmation. The main advantage of the proposed MAE method versus conventional solvent extraction (CSE) are the considerable reductions in time (7 min versus 16 h) and in solvent consumption (20 mL versus 150 mL). The MAE procedure yielded extracts that could be analyzed directly without any preliminary clean-up or solvent exchange steps. Both extraction methods show RSDs lower than 10% and lead to comparable recoveries of paclitaxel (87-92%).

摘要

开发并优化了一种简单快速的微波辅助萃取(MAE)方法,用于从生长在伊朗栖息地的欧洲红豆杉针叶中提取紫杉醇(泰素)。将样品浸入甲醇 - 水混合物中,在密闭容器系统中用微波辐照。该方法采用析因设计方法进行评估,所依据的参数包括萃取时间、温度、水中甲醇浓度(v/v)以及样品克数与10 mL溶剂的比例。结果的统计处理表明,除萃取时间外,所选参数均具有显著性。最佳条件为1.5 g样品溶于10 mL溶剂(90%甲醇),萃取温度95℃,萃取时间7 min。提取物通过反相高效液相色谱在227 nm处进行紫外检测(LC/UV)定量分析。液相色谱 - 串联质谱(LC - MS/MS)用于确证。与传统溶剂萃取(CSE)相比,所提出的MAE方法的主要优点是时间大幅减少(7 min对16 h)和溶剂消耗大幅降低(20 mL对150 mL)。MAE方法得到的提取物无需任何初步净化或溶剂交换步骤即可直接分析。两种萃取方法的相对标准偏差均低于10%,紫杉醇回收率相当(87 - 92%)。

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