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采用微型基质固相分散微萃取结合 UHPLC 定量分析生首乌和制首乌中的八种活性成分。

Quantification of eight active ingredients in crude and processed radix polygoni multiflori applying miniaturized matrix solid-phase dispersion microextraction followed by UHPLC.

机构信息

Tianjin State Key Laboratory of Modern Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Tianjin, China.

Key Laboratory of Formula of Traditional Chinese Medicine, Tianjin University of Traditional Chinese Medicine, Ministry of Education, Tianjin, China.

出版信息

J Sep Sci. 2018 Sep;41(17):3486-3495. doi: 10.1002/jssc.201800342. Epub 2018 Aug 2.

DOI:10.1002/jssc.201800342
PMID:30028075
Abstract

A rapid, efficient, and green sample preparation method has been developed to extract eight active ingredients (gallic acid, catechins, epicatechin, polydatin, 2,3,5,4'-tetrahydroxystilbene-2-O-β-d-glucoside, resveratrol, emodin, and physcion) in radix polygoni multiflori by miniaturized matrix solid-phase dispersion microextraction. Simple and sensitive ultra high performance liquid chromatography combined with ultraviolet detection has been applied to analyze the multiple compounds. The best results were obtained by adding 25 mg sample into 25 mg adsorbent and grinding for 2 min with disorganized silica as adsorbent and 1 mL 150 mM 1-dodecyl-3-methylimidazolium bromide as a green eluting solvent. Good linearity (r > 0.998) for each analyte was obtained by this method. The intra-day and inter-day precision (RSD) were both below 5.31%, and the recoveries of the analytes ranged from 93.3 to 100.0%. This simple miniaturized matrix solid-phase dispersion microextraction method for analyzing the compounds in radix polygoni multiflori needs a short time and requires little sample and reagent. Thus, this method is far more eco-friendly and efficient than traditional extraction methods (reflux and ultrasound-assisted extraction). The present investigation provided a promising method for the fast preparation and discrimination of chemical differences in crude and processed radix polygoni multiflori.

摘要

一种快速、高效、绿色的样品制备方法已经被开发出来,用于通过微型化基质固相分散微萃取法从何首乌中提取八种活性成分(没食子酸、儿茶素、表儿茶素、白藜芦醇苷、2,3,5,4'-四羟基二苯乙烯-2-O-β-D-葡萄糖苷、白藜芦醇、大黄素和大黄素甲醚)。简单灵敏的超高效液相色谱法结合紫外检测法被用于分析多种化合物。最佳结果是通过将 25mg 样品加入 25mg 吸附剂并以无序二氧化硅作为吸附剂,以 1ml 150mM 1-十二烷基-3-甲基溴化咪唑作为绿色洗脱溶剂进行研磨 2 分钟得到的。该方法对每种分析物均具有良好的线性(r>0.998)。日内和日间精密度(RSD)均低于 5.31%,分析物的回收率范围为 93.3%至 100.0%。这种简单的微型化基质固相分散微萃取方法用于分析何首乌中的化合物,所需时间短,所需样品和试剂少。因此,与传统的提取方法(回流和超声辅助提取)相比,这种方法更加环保和高效。本研究为快速制备和鉴别生何首乌和制何首乌的化学成分差异提供了一种有前途的方法。

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