在这项工作中,全面的二维液相色谱系统,由第一和第二维度的ZIC-HILIC和C18柱组成,分别,被调整并用于在七个商业浆果汁中获得多酚图案的高分辨率轮廓。所开发的HILIC×RP-LC方法在线性范围方面进行了验证,相关系数,检测限,定量极限,精度(日内和日间),和恢复。共有104种属于不同化学类别的多酚化合物(羟基苯甲酸和肉桂酸衍生物,黄酮苷,黄酮醇,黄酮醇苷,二氢黄酮醇,和花青素苷)已在研究的果汁中进行了表征和定量。尽管选民相似,观察到分析的浆果物种之间的显着定量变化。接骨木的多酚含量最高(918±1.10mg100mL-1),其次是苦莓(516±0.08毫克100毫升-1)。另一方面,覆盆子的含量最低(104±1.21mg100mL-1)。Further,总酚,类黄酮,用分光光度法测定花青素含量,产生一致的结果。自由基清除活性(DPPH试验)和果汁的还原能力,表示为IC50(μLmL-1)和mgASEmL-1,从2.79±0.03(蜜莓)到31.66±0.02(蓝莓)和从1.71±0.01(蓝莓)到8.89±0.12(苦莓),分别。这种基于聚焦调制的ZIC-HILIC×C18平台,到目前为止从未被用于浆果汁,显示出显着的分离能力,具有较高的校正峰容量值(高达1372)和正交性(Ao高达0.80),因此提供了有利地用于其它复杂食品样品的大的适用性。
In this work, a comprehensive two-dimensional liquid chromatography system, comprised of a ZIC-HILIC and C18 columns in the first and second dimensions, respectively, was tuned and employed for attaining high resolution profiles of the polyphenolic pattern in seven commercial berry juices. The developed HILIC × RP-LC method was validated in terms of linearity range, correlation coefficients, limit of detection, limit of quantification, precision (intra- and inter-day), and recovery. A total of 104 polyphenolic compounds belonging to different chemical classes (hydroxybenzoic and cinnamic acid derivatives, flavone glycosides, flavonols, flavonol glycosides, dihydroflavonols, and anthocyanin glycosides) have been characterized and quantified in the juices investigated. Despite the constituents being similar, a notable quantitative variation among the analyzed berry species was observed. Elderberry contained the highest amount of polyphenols (918 ± 1.10 mg 100 mL-1), followed by chokeberry (516 ± 0.08 mg 100 mL-1). On the other hand, raspberry contained the lowest amount (104 ± 1.21 mg 100 mL-1). Further, total phenolic, flavonoid, and anthocyanin contents were determined spectrophotometrically, yielding consistent results. The free-radical scavenging activity (DPPH test) and reducing power of the juices, expressed as IC50 (μL mL-1) and mg ASE mL-1, varied from 2.79 ± 0.03 (honeyberry) to 31.66 ± 0.02 (blueberry) and from 1.71 ± 0.01 (blueberry) to 8.89 ± 0.12 (chokeberry), respectively. Such a ZIC-HILIC × C18 platform based on focusing modulation, never employed so far for berry juices, showed a remarkable separation capability with high values of corrected peak capacity (up to 1372) and orthogonality (Ao up to 0.80), thus providing a great applicability to be advantageously employed for other complex food samples.