高速剪切辅助疏水低共熔溶剂萃取技术在HPLC检测枸杞红素类成分的应用研究

Determination of Carotenoids in Lycium Barbarum L.by High Speed Shear Dispersing Emulsifier Assisted Hydrophobic Deep Eutectic Solvent Extraction Combined with HPLC

研究合成了一系列疏水性低共熔溶剂(Deep eutectic solvents,DES),以其为萃取剂建立了高速剪切(High-speed shear dispersing emulsifier,HSDE)辅助疏水低共熔溶剂萃取,结合高效液相色谱法测定枸杞中的枸杞红素类成分的新方法。通过优化料液比、萃取次数、高速剪切转速等影响萃取效率的因素,确定最佳条件为:以薄荷醇和正辛醇(比例为1:2)合成的DES-4为萃取剂,料液比为1:20,高速剪切转速为10000 r/min,室温萃取5 min,离心后定容经高效液相色谱检测,外标法定量。结果显示:3种主要的枸杞红素类成分(玉米黄质、玉米黄质单棕榈酸酯和玉米黄质双棕榈酸酯)在各自质量浓度范围内呈良好的线性关系,相关系数R;均大于0.995,日间精密度、日内精密度和重复性均良好,加标回收率分别为83.7%~102.8%、89.1%~114.3%和85.4%~99.3%。该方法操作简单、高效便捷,适用于枸杞中枸杞红素类成分的检测需求,为以枸杞红素类成分为指标成分的标准构建和枸杞品质保障质控体系构建提供了新的途径。

A series of hydrophobic deep eutectic solvents (DES) were synthesized and used as extractant to establish a new method for the determination of carotenoids in Lycium barbarum L.by high speed shear dispersing emulsifier (HSDE) assisted hydrophobic DES extraction combined with HPLC.Material-liquid ratio,extraction times,high-speed shearing speeds and other conditions were optimized.The optimal conditions were determined as follows:DES-4 synthesized with menthol and n-octanol (ratio 1:2) was used as the extractant,the ratio of material to liquid was 1:20,the high-speed shearing speed was 10000 r/min,and the extraction at room temperature was 5 min.After centrifugation,the volume was determined by high-performance liquid chromatography and quantified by external standard method.The results showed that the three main components of carotenoids (zeaxanthin,zeaxanthin monopalmitate and zeaxanthin dipalmitate) showed a good linear relationship within their respective mass concentration ranges,and the correlation coefficient R;was all more than 0.995,the inter-day precision,intra-day precision and repeatability were all good,and the recovery rates of standard addition were 83.7%~102.8%,89.1%~114.3% and 85.4%~99.3%,respectively.This method was simple to operate,efficient and convenient,and is suitable for the detection requirements of zeaxanthin dipalmitate and its derivatives in Lycium barbarum L.This research provides a new way for the standard construction of zeaxanthin dipalmitate and its derivatives as indicator components and the construction of a quality control system for Lycium barbarum L.quality assurance.