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基于疏水性深共晶溶剂的涡旋辅助分散液相微萃取分析自紫草酸成琪汤中的主要活性化合物。

Vortex-assisted dispersive liquid-phase microextraction for the analysis of main active compounds from Zi-Cao-Cheng-Qi decoction based on a hydrophobic deep eutectic solvent.

机构信息

School of Pharmacy, Shanxi Medical University, Taiyuan, P. R. China.

Cancer Institute, the Affiliated Hospital of Qingdao University, Qingdao University, Qingdao, P. R. China.

出版信息

J Sep Sci. 2021 Dec;44(24):4376-4383. doi: 10.1002/jssc.202100270. Epub 2021 Nov 5.

Abstract

In this study, a vortex-assisted hydrophobic deep eutectic solvent dispersive liquid-phase microextraction was developed and used for the extraction and preconcentration of six main active compounds in Zi-Cao-Cheng-Qi decoction. The deep eutectic solvent, prepared by mixing tetrabutylammonium chloride and hexanoic acid at a molar ratio of 1:1, was added to the sample solution containing the analytes. In the absence of disperser, the extractant was rapidly dispersed into fine droplets by the aid of vortex and adequately contacted with the analytes. Some key parameters affecting the approach including extraction solvent type and volume, sample phase pH, extraction time, centrifugation time, and salt concentration were investigated and optimized. Under the optimum conditions, enrichment factors of the target analytes were in the range of 3-330. The calibration graphs were linear with a correlation coefficient (r) ≥ 0.9929. The detection limits were 0.3-0.9 ng/mL, and the satisfactory precisions (relative standard deviations, 0.5-8.9%) and accuracies (relative recoveries, 91.1-102.2%) were also obtained. The developed method was rapid (only 2 min), eco-friendly, effective, and easy to operate. And it has been successfully applied to simultaneous extraction, enrichment, and determination of the main active compounds in a traditional Chinese medicinal formula coupled with high-performance liquid chromatography.

摘要

在这项研究中,开发了一种涡旋辅助疏水深共晶溶剂分散液相微萃取方法,并将其用于提取和预浓缩紫草承气汤中的六种主要活性化合物。深共晶溶剂由四丁基氯化铵和己酸以 1:1 的摩尔比混合制备,加入含有分析物的样品溶液中。在没有分散剂的情况下,萃取剂在涡旋的帮助下迅速分散成细小的液滴,并与分析物充分接触。研究并优化了一些关键参数,包括萃取溶剂的类型和体积、样品相 pH 值、萃取时间、离心时间和盐浓度。在最佳条件下,目标分析物的富集因子在 3-330 范围内。校准曲线的线性相关系数(r)≥0.9929。检测限为 0.3-0.9ng/mL,同时还获得了令人满意的精密度(相对标准偏差为 0.5-8.9%)和准确度(相对回收率为 91.1-102.2%)。该方法快速(仅 2 分钟)、环保、有效且易于操作。并已成功应用于高效液相色谱法与传统中药配方中主要活性化合物的同时提取、富集和测定。

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