Department of Chemistry, National Central University, Chung-Li 320, Taiwan; Department of Chemical Engineering, Army Academy ROC, Chung-Li 320, Taiwan.
Department of Chemistry, National Central University, Chung-Li 320, Taiwan.
J Chromatogr A. 2019 Nov 8;1605:460367. doi: 10.1016/j.chroma.2019.460367. Epub 2019 Jul 19.
A reliable and straightforward method was developed for the rapid determination of nine parabens (methyl-, ethyl-, propyl-, butyl-, isopropyl-, isobutyl-, pentyl-, hexyl-, and benzyl-parabens) in indoor dust by a mortar/pestle-free and column-free dual-vortex-assisted matrix solid-phase dispersion (DVA-MSPD) technique. After that, they were determined by isotope-dilution ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UHPLC-qTOF-MS, or called UHPLC-HRMS) and operating in negative electrospray ionization mode. Optimization of the DVA-MSPD was done using Box-Behnken Design along with response surface methodology. Validation was done by measuring and calculating selectivity, limits of detection (LOD), limits of quantitation (LOQs), precision and trueness (accuracy) of intra- and inter-day analysis. The LOQs of the method ranged from 0.9 to 2.8 ng/g. High precisions for both intra- and inter-day analysis were obtained ranging from 1 to 8%. Excellent trueness (or mean extraction recovery) varied from 93 to 104%. The DVA-MSPD combined with isotope-dilution UHPLC-qTOF-MS was successfully applied to determine parabens in indoor dust samples from office rooms and private houses, and the total concentrations ranged from 55 to 686 ng/g.
建立了一种可靠且直接的方法，通过无研钵/无柱双涡旋辅助基质固相分散（DVA-MSPD）技术，快速测定室内灰尘中的 9 种（甲基、乙基、丙基、丁基、异丙基、异丁基、戊基、己基和苄基）对羟基苯甲酸酯。然后，采用同位素稀释超高效液相色谱-四极杆飞行时间质谱法（UHPLC-qTOF-MS，或称为 UHPLC-HRMS），在负离子电喷雾模式下进行检测。通过Box-Behnken 设计和响应面法对 DVA-MSPD 进行优化。通过测量和计算选择性、检测限（LOD）、定量限（LOQ）、日内和日间分析的精密度和准确度来进行验证。该方法的 LOQ 范围为 0.9 至 2.8 ng/g。日内和日间分析的精密度均较高，范围为 1 至 8%。良好的准确度（或平均提取回收率）范围为 93 至 104%。DVA-MSPD 与同位素稀释 UHPLC-qTOF-MS 相结合，成功地应用于测定来自办公室和私人住宅的室内灰尘样品中的对羟基苯甲酸酯，总浓度范围为 55 至 686 ng/g。
