Yıldız Technical University, Department of Chemistry, 34349 İstanbul, Turkey.
Bülent Ecevit University, Institute of Science, Environmental Engineer Department, 67100 Zonguldak, Turkey.
J Hazard Mater. 2022 Mar 15;426:127819. doi: 10.1016/j.jhazmat.2021.127819. Epub 2021 Nov 22.
This study reports an efficient, green, sensitive and simple analytical protocol for trace determination of methyl paraben, ethyl paraben, propyl paraben, butylparaben and benzyl paraben by high-performance liquid chromatography-ultraviolet detection (HPLC-UV). The analytes were preconcentrated using an ultrasonication supported (US) dispersive solid phase extraction (DSPE) method based on reduced graphene oxide (rGO) modified iron nanoparticles (US-FeO@rGO-DSPE). A reversed-phase C18 column and an isocratic elution program comprising of 20 mM phosphate buffer (pH 4.50) and acetonitrile(58:42, v/v) were used to elute and separate the analytes for detection. The limits of detection determined for the analytes were very low and were in the range of 0.02 - 0.16 ng mL. The coefficients of determination obtained for the analytes ranged from 0.9973 to 0.9998, and this validated good linearity of the method.Percent relative standard deviations obtained in the range of 2.5 - 10.6% verified the method's high intraday repeatability. Accuracy of the proposed method was assessed with spiking experiments performed on complex sample matrices. Percent recoveries calculated for spiked soil, artificial seawater and seaweed samples were in acceptable ranges of 95 - 121%, 87 - 117% and 85 - 111%, respectively. These figures of merit suggest that HPLC-UV coupled with the US-FeO@rGO-DSPEmethod is suitable for the determination of parabens in Antarctic samples.
本研究报告了一种高效、绿色、灵敏、简单的分析方案，用于通过高效液相色谱-紫外检测（HPLC-UV）法对痕量的甲基对羟基苯甲酸酯、乙基对羟基苯甲酸酯、丙基对羟基苯甲酸酯、丁基对羟基苯甲酸酯和苄基对羟基苯甲酸酯进行测定。采用超声辅助（US）分散固相萃取（DSPE）法，基于还原氧化石墨烯（rGO）修饰的铁纳米粒子（US-FeO@rGO-DSPE）对分析物进行预浓缩。采用反相 C18 柱和等度洗脱程序，洗脱和分离分析物进行检测，洗脱程序由 20 mM 磷酸盐缓冲液（pH 4.50）和乙腈（58:42，v/v）组成。所测定的分析物的检出限非常低，范围在 0.02-0.16 ng mL。分析物的相关系数在 0.9973-0.9998 之间，表明该方法具有良好的线性度。在 2.5-10.6%的范围内获得的相对标准偏差（RSD）验证了该方法具有较高的日内重复性。通过在复杂的样品基质上进行加标实验来评估该方法的准确性。加标土壤、人工海水和海藻样品的回收率分别在 95-121%、87-117%和 85-111%的可接受范围内。这些优良的技术指标表明，HPLC-UV 与 US-FeO@rGO-DSPE 法相结合，适用于南极样品中对羟基苯甲酸酯的测定。
