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Graphene-magnetite as adsorbent for magnetic solid phase extraction of 4- hydroxybenzoic acid and 3,4-dihydroxybenzoic acid in stingless bee honey

机译:石墨烯-磁铁矿为吸附剂,用于磁性固相萃取无刺蜂蜂蜜中的4-羟基苯甲酸和3,4-二羟基苯甲酸

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摘要

Graphene-magnetite composite (G-Fe3O4) was successfully synthesized and applied as adsorbent for magnetic solid phase extraction (MSPE) of two phenolic acids namely 4-hydroxybenzoic acid (4-HB) and 3,4-dihydroxybenzoic acid (3,4-DHB) from stingless bee honey prior to analysis using high performance liquid chromatography with ultraviolet-visible detection (HPLC-UV/Vis). Several MSPE parameters affecting extraction of these two acids were optimized. Optimum MSPE conditions were 50 mg of G-Fe3O4 adsorbent, 5 min extraction time at 1600 rpm, 30 mL sample volume, sample solution pH 0.5, 200 mu L methanol as desorption solvent (5 min sonication assisted) and 5% w/v NaCl. The LODs (3 S/N) calculated for 4-HB and 3,4-DHB were 0.08 and 0.14 mu g/g, respectively. Good relative recoveries (72.6-110.6%) and reproducibility values (RSD 8.5%, n= 9) were obtained. The developed G-Fe3O4 MSPE method offered is simple, easy, environmental friendly and efficient for extraction of the two phenolic acids from stingless bee honey samples.
机译:成功合成了石墨烯-磁铁矿复合物(G-Fe3O4),并用作吸附剂用于磁性固相萃取(MSPE)两种酚酸,分别是4-羟基苯甲酸(4-HB)和3,4-二羟基苯甲酸(3,4-使用高效液相色谱和紫外可见检测(HPLC-UV / Vis)分析之前,从无刺蜂蜂蜜中提取DHB)。优化了影响这两种酸提取的几个MSPE参数。 MSPE的最佳条件是50 mg G-Fe3O4吸附剂,1600 rpm的萃取时间5分钟,样品体积30 mL,样品溶液pH 0.5、200μL的甲醇作为解吸溶剂(超声处理5分钟)和5%w / v NaCl 。计算出的4-HB和3,4-DHB的LOD(3 S / N)分别为0.08和0.14μg / g。获得了良好的相对回收率(72.6-110.6%)和重现性值(RSD <8.5%,n = 9)。提供的已开发的G-Fe3O4 MSPE方法简单,容易,环保且高效,可从无刺蜂蜂蜜样品中提取两种酚酸。

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