Determination of phenolic acids and flavonoids in raw propolis by silica-supported ionic liquid-based matrix solid phase dispersion extraction high performance liquid chromatography-diode array detection
Determination of phenolic acids and flavonoids in raw propolis by silica-supported ionic liquid-based matrix solid phase dispersion extraction high performance liquid chromatography-diode array detection
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DOI：
10.1016/j.jchromb.2014.08.022
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发表时间：
2014-10-15
影响因子：
3
通讯作者：
Zhang, Hanqi
中科院分区：
文献类型：
--
作者：
Wang, Zhibing;Sun, Rui;Zhang, Hanqi
采用浸渍法制备二氧化硅负载离子液体（S-SIL），作为基质固相分散体（MSPD）的分散吸附剂，用于同时提取原料中的咖啡酸、阿魏酸、桑色素、木犀草素、槲皮素、芹菜素、白杨素、山柰素等8种酚酸和黄酮类化合物。 蜂胶。采用 Zorbax SB-C18 柱（150 mm x 4.6 mm，3.5 μm）的高效液相色谱法分离分析物。流动相由0.2%磷酸水溶液和乙腈组成，流动相流速为0.5 mL/min。对二氧化硅负载的离子液体基质固相分散体（S-SIL-based MSPD）的实验条件进行了优化。使用含有 10% [C6MIM]Cl 的 S-SIL 作为分散剂，20 mL 正己烷作为洗涤溶剂，15 mL 甲醇作为洗脱溶剂。 S-SIL与样品的比例选择为4:1。标准曲线呈良好的线性关系(r>0.9995)。检测限和定量限分别为5.8～22.2 ng·mL(-1)和19.2～74.0 ng·mL(-1)。日内和日间测定的相对标准偏差(RSD)分别低于8.80%和11.19%。回收率在 65.51% 至 92.32% 之间，RSD 低于 8.95%。与超声辅助提取（UAE）和索氏提取相比，尽管基于S-SIL的MSPD获得的提取率略低于UAE获得的提取率，但本方法消耗的样品、有机溶剂和提取时间更少。 (C) 2014 Elsevier B.V. 保留所有权利。
The silica-supported ionic liquid (S-SIL) was prepared by impregnation and used as the dispersion adsorbent of matrix solid phase dispersion (MSPD) for the simultaneous extraction of eight phenolic acids and flavonoids, including caffeic acid, ferulic acid, morin, luteolin, quercetin, apigenin, chrysin, and kaempferide in raw propolis. High performance liquid chromatography with a Zorbax SB-C18 column (150 mm x 4.6 mm, 3.5 mu m) was used for separation of the analytes. The mobile phase consisted of 0.2% phosphoric acid aqueous solution and acetonitrile and the flow rate of the mobile phase was 0.5 mL/min. The experimental conditions for silica-supported ionic liquid-based matrix solid phase dispersion (S-SIL-based MSPD) were optimized. S-SIL containing 10% [C6MIM]Cl was used as dispersant, 20 mL of n-hexane as washing solvent and 15 mL of methanol as elution solvent. The ratio of S-SIL to sample was selected to be 4:1. The standard curves showed good linear relationship (r> 0.9995). The limits of detection and quantification were in the range of 5.8-22.2 ng mL(-1) and 19.2-74.0 ng mL(-1), respectively. The relative standard deviations (RSDs) of intra-day and inter-day determination were lower than 8.80% and 11.19%, respectively. The recoveries were between 65.51% and 92.32% with RSDs lower than 8.95%. Compared with ultrasound-assisted extraction (UAE) and soxhlet extraction, the present method consumed less sample, organic solvent, and extraction time, although the extraction yields obtained by S-SIL-based MSPD are slightly lower than those obtained by UAE. (C) 2014 Elsevier B.V. All rights reserved.