Hashemi Beshare, Shamsipur Mojtaba, Fattahi Nazir
Department Chemistry, Razi University, Kermanshah, Iran.
Research Center for Environmental Determinants of Health (RCEDH), Kermanshah University of Medical Sciences, Kermanshah, Iran
J Chromatogr Sci. 2015 Sep;53(8):1414-9. doi: 10.1093/chromsci/bmv011. Epub 2015 Feb 25.
A dispersive liquid-liquid microextraction based on solidification of floating organic drop method combined with solid-phase extraction (500-mg C18 sorbent) was developed for preconcentration and determination of some parabens. The experimental parameters influencing the extraction efficiency such as the type of extraction and disperser solvents, as well as their volumes, breakthrough volume, flow rate and salt addition were studied and optimized. The optimum experimental conditions found included: sample volume, 100 mL; KCl concentration, 1% (w/v); extraction solvent (1-undecanol) volume, 20 µL and disperser solvent (acetone) volume, 250 µL. Under the optimum experimental conditions, calibration graphs were linear in the range of 1-200 µg L(-1) with limits of detection ranged from 0.3 to 1.7 µg L(-1). The relative standard deviations were in the range of 1.2-3.1% (n = 5). The enrichment factors and absolute recoveries of parabens in different matrices were 245-1886 and 9.0-69.8%, respectively. The method was applied to the simultaneous determination of parabens in different matrices. The relative recoveries from water, shampoo and mouth rinse samples, which have been spiked at different levels of parabens, were 87.83-112.25%, 82.80-108.40% and 90.10-97.60%, respectively.
建立了一种基于浮上有机液滴固化法结合固相萃取(500mg C18吸附剂)的分散液液微萃取方法,用于对某些对羟基苯甲酸酯进行预富集和测定。研究并优化了影响萃取效率的实验参数,如萃取溶剂和分散剂溶剂的类型及其体积、穿透体积、流速和盐的添加量。所确定的最佳实验条件包括:样品体积100mL;KCl浓度1%(w/v);萃取溶剂(1-十一醇)体积20μL,分散剂溶剂(丙酮)体积250μL。在最佳实验条件下,校准曲线在1 - 200μg L⁻¹范围内呈线性,检测限为0.3 - 1.7μg L⁻¹。相对标准偏差在1.2 - 3.1%范围内(n = 5)。不同基质中对羟基苯甲酸酯的富集因子和绝对回收率分别为245 - 1886和9.0 - 69.8%。该方法应用于同时测定不同基质中的对羟基苯甲酸酯。在不同水平添加对羟基苯甲酸酯的水、洗发水和漱口水样品中的相对回收率分别为87.83 - 112.25%、82.80 - 108.40%和90.10 - 97.60%。