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Switchable-hydrophilicity solvent liquid-liquid microextraction for sample cleanup prior to dispersive magnetic solid-phase microextraction for spectrophotometric determination of quercetin in food samples
Sustainable Chemistry and Pharmacy ( IF 6 ) Pub Date : 2021-06-26 , DOI: 10.1016/j.scp.2021.100480
Malek Hassan , Furkan Uzcan , Syed Nasrullah Shah , Usama Alshana , Mustafa Soylak

Switchable-hydrophilicity solvent-liquid-liquid microextraction (SHS-LLME), as an efficient sample cleanup method, was combined with dispersive solid-phase microextraction (DSPME) for preconcentration of quercetin prior to its spectrophotometric determination. Optimum SHS-LLME were found as 1000 μL of N,N-dimethylcyclohexylamine as the extraction solvent and 750 μL of 10.0 M sodium hydroxide as the phase separation trigger. Optimum DSPME were sample pH at 6.0, 1000 μL of acetone as the eluent, 30.0 mL of sample, 12.5 mg of Fe3O4@XAD-16 as the adsorbent, 4.0 and 1.5 min as the adsorption and elution times, respectively. Calibration graphs with coefficient of determination (R2) higher than 0.9956, limits of detection (LOD) of 9.0–11.9 ng mL−1 and limits of quantitation (LOQ) of 29.9–39.6 ng mL−1 were obtained. Repeatability, expressed as percentage relative standard deviation (%RSD), was better than 3.2 and 8.9% for intra- and inter-day precision, respectively. The proposed SHS-LLME-DSPME-UV/Vis method was applied for the determination of quercetin in four food samples (i.e., apple, pepper, red and white onion) with percentage recoveries in the range of 92.1–107.4%. The proposed method is superior to others in terms of greenness, rapidness, simplicity, good repeatability and low capital cost.



中文翻译:

用于食品样品中槲皮素分光光度法测定的分散磁性固相微萃取之前用于样品净化的可切换亲水性溶剂液-液微萃取

可切换亲水性溶剂-液-液微萃取 (SHS-LLME) 作为一种有效的样品净化方法,与分散固相微萃取 (DSPME) 相结合,在分光光度法测定之前预浓缩槲皮素。发现最佳 SHS-LLME 为 1000 μL N,N-二甲基环己胺作为萃取溶剂,750 μL 10.0 M 氢氧化钠作为相分离触发剂。最佳 DSPME 是样品 pH 为 6.0,1000 μL 丙酮作为洗脱液,30.0 mL 样品,12.5 mg Fe 3 O 4 @XAD-16 作为吸附剂,吸附和洗脱时间分别为 4.0 和 1.5 分钟。具有确定系数的校准图 (R 2)高于0.9956,的9.0-11.9检测(LOD)的限制纳克毫升-1和29.9-39.6每mL(LOQ)定量限-1得到。以相对标准偏差百分比 (%RSD) 表示的重复性分别优于 3.2% 和 8.9% 的日内和日间精密度。建议的 SHS-LLME-DSPME-UV/Vis 方法用于测定四种食品样品(即苹果、胡椒、红洋葱和白洋葱)中的槲皮素,回收率范围为 92.1-107.4%。所提出的方法在绿色、快速、简单、良好的可重复性和低资本成本方面优于其他方法。

更新日期:2021-06-28
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