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首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >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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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

机译:硅胶载离子液体基质固相分散萃取-高效液相色谱-二极管阵列检测法测定蜂胶中酚酸和类黄酮

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摘要

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×4.6 mm, 3.5 μm) 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-SILbased 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.
机译:通过浸渍制备二氧化硅负载的离子液体(S-SIL),并用作基质固相分散体(MSPD)的分散吸附剂,用于同时萃取8种酚酸和黄酮类化合物,包括咖啡酸,阿魏酸,香豆素,木犀草素蜂胶中的槲皮素,槲皮素,芹菜素,菊花素和山emp素。使用具有Zorbax SB-C18色谱柱的高效液相色谱仪(150 mm×4.6 mm,3.5μm)分离分析物。流动相由0.2%磷酸水溶液和乙腈组成,流动相的流速为0.5 mL / min。优化了二氧化硅负载离子液体基基质固相分散体(S-SIL基MSPD)的实验条件。将含有10%[C6MIM] Cl的S-SIL用作分散剂,将20 mL的正己烷用作洗涤溶剂,将15 mL的甲醇用作洗脱溶剂。 S-SIL与样品的比例选择为4:1。标准曲线显示出良好的线性关系(r> 0.9995)。检测限和定量限分别在5.8-22.2 ng mL〜(-1)和19.2-74.0 ng mL〜(-1)之间。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%。与基于超声的辅助萃取(UAE)和索氏萃取相比,本方法消耗的样品,有机溶剂和萃取时间更少,尽管基于S-SIL的MSPD获得的萃取率略低于由阿拉伯联合酋长国获得的萃取率。

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