Department of Chemistry, University of Ioannina, Ioannina, Greece.
J Sep Sci. 2012 Jul;35(13):1659-66. doi: 10.1002/jssc.201200106.
A simple and green method based on dispersive liquid-liquid microextraction, mated to chemometrics and followed by mass spectrometric detection for the determination of suspected fragrance allergens in water samples is developed and assessed in this work. Volume of extraction and disperser solvent, pH, ionic strength, extraction time, sample volume, as well as centrifugation time were initially optimized in a fractional factorial design. The obtained significant factors were optimized by using a central composite design and the quadratic model between the dependent and the independent variables was built. The obtained optimal conditions were: aqueous sample of 3.8 mL, 100 μL chloroform, 1.40 mL acetone, 4 min centrifugation time, natural pH containing 5% (w/v) NaCl, and centrifugation speed 4000 rpm. Method proved to be linear over a wide range of concentration for all analytes with R(2) between 0.9807 and 0.9959. The repeatability and reproducibility of the proposed method, expressed as relative standard deviation, varied between 3-13% and 4-16%, respectively. The limits of detection ranged from 0.007 to 1.0 μg L(-1) . The recommended method was applied to water samples including baby bath as well as swimming pool water samples and was compared with a previously reported method.
本工作开发并评估了一种基于分散液液微萃取、与化学计量学相结合、并结合质谱检测的简单绿色方法，用于测定水样中的可疑香料过敏原。在部分因子设计中，首先对萃取和分散溶剂体积、pH 值、离子强度、萃取时间、样品体积以及离心时间进行了优化。在中心复合设计中对得到的显著因素进行了优化，并建立了因变量与自变量之间的二次模型。得到的最佳条件为：水样 3.8 mL，100 μL 氯仿，1.40 mL 丙酮，4 分钟离心时间，含 5%（w/v）NaCl 的自然 pH 值，离心速度 4000 rpm。该方法对所有分析物在很宽的浓度范围内均呈线性，相关系数（R(2)）在 0.9807 至 0.9959 之间。所提出方法的重复性和再现性，分别以相对标准偏差表示，在 3-13%和 4-16%之间变化。检测限范围为 0.007 至 1.0 μg L(-1)。该方法已应用于包括婴儿浴液和游泳池水样在内的水样，并与先前报道的方法进行了比较。
