Abstract A capillary electrophoresis method with large volume sample stacking (CE-LVSS) has been developed and validated for the simultaneous determination of seven phenolic compounds: naringin, rutin, carnosic acid, apigenin, quercetin, morin, and chichoric acid. Optimization was carried out by response surface methodology and a set of 20 experiments helped to optimize the parameters such as the concentration of buffer, buffer pH, and applied voltage. Analytes were separated using a 50 µm diameter capillary with 56 cm effective length and an extended light path using 20 mM borate buffer at pH 9.2. The LVSS method was optimized and a three- to fivefold improvement in detectability was achieved with injection at 100 mbar for 20 s followed by polarity switching at –20 kV for 6 s. The linearity values of all seven analytes were observed in the concentration ranges from 0.5 to 50 µg/mL for CE and 0.1 to 25 µg/mL for LVSS. The limits of detection were from 0.012 to 0.241 and 0.003 to 0.086 µg/mL for CE and LVSS. The obtained limits of quantitation were within 0.041 to 0.802 for CE and 0.012 to 0.286 µg/mL for LVSS. The recoveries were between 91.1 and 109.8% and 96.3 and 108.4% for CE and LVSS, respectively. The developed method has been successfully applied for the quantitative determination of analyzed components from food samples that are important sources of these compounds.

中文翻译：

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毛细管电泳 (CE) 中的大体积样品堆积 (LVSS) 和响应面法 (RSM) 用于测定食品样品中的酚类物质

摘要 开发并验证了大体积样品堆积毛细管电泳法 (CE-LVSS)，可同时测定七种酚类化合物：柚皮苷、芦丁、鼠尾草酸、芹菜素、槲皮素、桑黄素和菊苣酸。优化是通过响应面方法进行的，一组 20 个实验有助于优化参数，例如缓冲液浓度、缓冲液 pH 值和施加的电压。使用有效长度为 56 cm 的 50 µm 毛细管和延长的光程，使用 pH 9.2 的 20 mM 硼酸盐缓冲液分离分析物。LVSS 方法经过优化，在 100 mbar 下进样 20 秒，然后在 –20 kV 下进行极性切换 6 秒后，可检测性提高了三到五倍。在 0.5 至 50 µg/mL 的 CE 和 0.1 至 25 µg/mL 的 LVSS 浓度范围内观察到所有七种分析物的线性值。CE 和 LVSS 的检测限为 0.012 至 0.241 和 0.003 至 0.086 µg/mL。获得的定量限对于 CE 为 0.041 至 0.802，对于 LVSS 为 0.012 至 0.286 µg/mL。CE 和 LVSS 的回收率分别在 91.1% 和 109.8% 之间以及 96.3% 和 108.4% 之间。开发的方法已成功应用于食品样品中分析成分的定量测定，这些成分是这些化合物的重要来源。LVSS 为 286 µg/mL。CE 和 LVSS 的回收率分别在 91.1% 和 109.8% 之间以及 96.3% 和 108.4% 之间。开发的方法已成功应用于食品样品中分析成分的定量测定，这些成分是这些化合物的重要来源。LVSS 为 286 µg/mL。CE 和 LVSS 的回收率分别在 91.1% 和 109.8% 之间以及 96.3% 和 108.4% 之间。开发的方法已成功应用于食品样品中分析成分的定量测定，这些成分是这些化合物的重要来源。