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A new and improved strategy combining a dispersive-solid phase extraction-based multiclass method with ultra high pressure liquid chromatography for analysis of low molecular weight polyphenols in vegetables

机译：一种新的改进策略，结合了基于分散固相萃取的多类方法与超高压液相色谱法，用于分析蔬菜中的低分子量多酚

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This paper reports on the development and optimization of a modified Quick, Easy, Cheap Effective, Rugged and Safe (QuEChERS) based extraction technique coupled with a clean-up dispersive-solid phase extraction (dSPE) as a new, reliable and powerful strategy to enhance the extraction efficiency of free low molecular-weight polyphenols in selected species of dietary vegetables. The process involves two simple steps. First, the homogenized samples are extracted and partitioned using an organic solvent and salt solution. Then, the supernatant is further extracted and cleaned using a dSPE technique. Final clear extracts of vegetables were concentrated under vacuum to near dryness and taken up into initial mobile phase (0.1% formic acid and 20% methanol). The separation and quantification of free low molecular weight polyphenols from the vegetable extracts was achieved by ultrahigh pressure liquid chromatography (UHPLC) equipped with a phodiode array (PDA) detection system and a Trifunctional High Strength Silica capillary analytical column (HSS T3), specially designed for polar compounds.The performance of the method was assessed by studying the selectivity, linear dynamic range, the limit of detection (LOD) and limit of quantification (LOQ), precision, trueness, and matrix effects. The validation parameters of the method showed satisfactory figures of merit. Good linearity (View the MathML sourceRvalues2>0.954; (+)-catechin in carrot samples) was achieved at the studied concentration range. Reproducibility was better than 3%. Consistent recoveries of polyphenols ranging from 78.4 to 99.9% were observed when all target vegetable samples were spiked at two concentration levels, with relative standard deviations (RSDs, n = 5) lower than 2.9%. The LODs and the LOQs ranged from 0.005 μg mL−1 (trans-resveratrol, carrot) to 0.62 μg mL−1 (syringic acid, garlic) and from 0.016 μg mL−1 (trans-resveratrol, carrot) to 0.87 μg mL−1 ((+)-catechin, carrot) depending on the compound. The method was applied for studying the occurrence of free low molecular weight polyphenols in eight selected dietary vegetables (broccoli, tomato, carrot, garlic, onion, red pepper, green pepper and beetroot), providing a valuable and promising tool for food quality evaluation.
机译：本文报告了改进的基于快速，简单，廉价有效，坚固耐用且安全（QuEChERS）的提取技术与净化分散固相提取（dSPE）的开发和优化，作为一种新的，可靠且功能强大的策略，提高某些饮食蔬菜中游离低分子量多酚的提取效率。该过程涉及两个简单步骤。首先，提取均质化的样品，并使用有机溶剂和盐溶液分配。然后，使用dSPE技术进一步提取和清洗上清液。将蔬菜的最终澄清提取物在真空下浓缩至接近干燥，并吸收至初始流动相（0.1％甲酸和20％甲醇）中。通过配备了光电二极管阵列（PDA）检测系统和三功能高强度硅胶毛细管分析柱（HSS T3）的超高压液相色谱（UHPLC）实现了从植物提取物中分离和定量游离低分子量多酚的研究通过研究选择性，线性动态范围，检测限（LOD）和定量限（LOQ），精密度，真实度和基质效应来评估该方法的性能。该方法的验证参数显示令人满意的品质因数。在研究的浓度范围内，获得了良好的线性度（查看胡萝卜样品中的（+）-儿茶素）。重现性优于3％。当所有目标蔬菜样品在两个浓度水平上加标时，多酚的回收率一致保持在78.4％至99.9％之间，相对标准偏差（RSDs，n = 5）低于2.9％。 LOD和LOQ范围为0.005μgmL-1（反式白藜芦醇，胡萝卜）至0.62μgmL-1（丁香酸，大蒜）和0.016μgmL-1（反式白藜芦醇，胡萝卜）至0.87μgmL− 1（（+）-儿茶素，胡萝卜）取决于化合物。该方法用于研究八种精选饮食蔬菜（西兰花，番茄，胡萝卜，大蒜，洋葱，红辣椒，青椒和甜菜根）中游离低分子量多酚的存在，为食品质量评估提供了有价值和有希望的工具。

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