Roscales Jose L, Vicente Alba, Ramos Lourdes, Jiménez Begoña
Department of Instrumental Analysis and Environmental Chemistry, Institute of Organic Chemistry, CSIC (IQOG-CSIC), Juan de la Cierva 3, 28006, Madrid, Spain.
Anal Bioanal Chem. 2017 Aug;409(20):4905-4913. doi: 10.1007/s00216-017-0432-5. Epub 2017 Jun 7.
A simplified, miniaturised matrix solid-phase dispersion (MSPD)-based method allowing the simultaneous extraction and purification of contaminants belonging to selected families of regulated persistent organic pollutants (POPs), i.e. polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs) and penta- to octa-polybrominated diphenyl ethers (PBDEs), and related contaminants of emerging concern, such as deca-BDE and Dechlorane Plus (DP), has been proposed. Wild bird eggs were used as biotic fat-containing model matrices. Once optimised, the procedure allowed sample preparation to be accomplished within 30 min, in a single step, and with minimal sample and reagent consumption and waste generation. These features contributed to speeding up and greening the analytical process as compared to the large-scale multistep procedures for these types of analyses. The method was combined with gas chromatography-quadrupole mass spectrometry (GC-qMS) for PCB and OCP analysis and with GC-negative ion chemical ionisation-quadrupole mass spectrometry (NCI-qMS) for PBDE and DP determination. The complete analytical method provided satisfactory recoveries of the target compounds (above 83% for all analytes, except for PBDE 209, 63%), although as small an amount of sample as 0.300 g was used. The repeatability of the complete procedure was less than 16% (with the only exception for PCB 153, which looked to be affected by an interference). The limits of detection were in all cases lower than 34 pg g dry weight (as calculated for real samples), demonstrating the feasibility of the proposed procedure for accurate determination of the target compounds in biological samples. The proposed procedure was applied to the analysis of the target POPs in unhatched eggs of wild bird species. Graphical abstract Scheme of the miniaturised methodology proposed for environmental monitoring of POPs and related compounds in wild bird eggs.
本文提出了一种基于简化、小型化基质固相分散（MSPD）的方法，可同时萃取和纯化属于特定类别受管制持久性有机污染物（POPs）的污染物，即多氯联苯（PCBs）、有机氯农药（OCPs）和五至八溴二苯醚（PBDEs），以及新兴关注的相关污染物，如十溴二苯醚和得克隆（DP）。野生鸟蛋被用作含生物脂肪的模型基质。该方法优化后，能在30分钟内一步完成样品制备，且样品和试剂消耗极少，产生的废弃物也最少。与这类分析的大规模多步骤程序相比，这些特性有助于加快分析过程并使其更加绿色环保。该方法与气相色谱-四极杆质谱联用（GC-qMS）用于多氯联苯和有机氯农药分析，与气相色谱-负离子化学电离-四极杆质谱联用（NCI-qMS）用于多溴二苯醚和得克隆的测定。完整的分析方法对目标化合物的回收率令人满意（除了PBDE 209为63%外，所有分析物的回收率均高于83%），尽管使用的样品量低至0.300 g。完整程序的重复性小于16%（唯一例外是PCB 153，似乎受到干扰影响）。所有情况下的检测限均低于34 pg g干重（按实际样品计算），证明了所提程序在生物样品中准确测定目标化合物的可行性。所提程序应用于野生鸟类未孵化蛋中目标持久性有机污染物的分析。图摘要 用于野生鸟蛋中持久性有机污染物及相关化合物环境监测的小型化方法示意图
