Piovesana Susy, Capriotti Anna Laura, Cavaliere Chiara, La Barbera Giorgia, Samperi Roberto, Zenezini Chiozzi Riccardo, Laganà Aldo
Dipartimento di Chimica, Sapienza Università di Roma, Box no 34 - Roma 62, Piazzale Aldo Moro 5, 00185, Rome, Italy.
Anal Bioanal Chem. 2017 Jul;409(17):4181-4194. doi: 10.1007/s00216-017-0368-9. Epub 2017 May 18.
Magnetic solid-phase extraction is one of the most promising new extraction methods for liquid samples before ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis. Several types of materials, including carbonaceous ones, have been prepared for this purpose. In this paper, for the first time, the preparation, characterization, and sorption capability of FeO-graphitized carbon black (mGCB) composite toward some compounds of environmental interest were investigated. The synthesized mGCB consisted of micrometric GCB particles with 55 m g surface area bearing some carbonyl and hydroxyl functionalities and the surface partially decorated by FeO microparticles. The prepared mGCB was firstly tested as an adsorbent for the extraction from surface water of 50 pollutants, including estrogens, perfluoroalkyl compounds, UV filters, and quinolones. The material showed good affinity to many of the tested compounds, except carboxylates and glucoronates; however, some compounds were difficult to desorb. Ten UV filters belonging to the chemical classes of benzophenones and p-aminobenzoates were selected, and parameters were optimized for the extraction of these compounds from surface water before UHPLC-MS/MS determination. Then, the method was validated in terms of linearity, trueness, intra-laboratory precision, and detection and quantification limits. In summary, the method performance (trueness, expressed as analytical recovery, 85-114%; RSD 5-15%) appears suitable for the determination of the selected compounds at the level of 10-100 ng L, with detection limits in the range of 1-5 ng L. Finally, the new method was compared with a published one, based on conventional solid-phase extraction with GCB, showing similar performance in real sample analysis. Graphical Abstract Workflow of the analytical method based on magnetic solid-phase extraction followed by LC-MS/MS determination.
磁性固相萃取是超高效液相色谱-串联质谱（UHPLC-MS/MS）分析前用于液体样品的最具前景的新型萃取方法之一。为此已经制备了包括含碳材料在内的几种类型的材料。本文首次研究了FeO-石墨化炭黑（mGCB）复合材料对一些环境相关化合物的制备、表征及吸附能力。合成的mGCB由表面积为55 m²/g的微米级GCB颗粒组成，带有一些羰基和羟基官能团，表面部分被FeO微粒修饰。制备的mGCB首先作为吸附剂用于从地表水中萃取50种污染物，包括雌激素、全氟烷基化合物、紫外线过滤剂和喹诺酮类。该材料对许多测试化合物表现出良好的亲和力，但羧酸盐和葡糖醛酸盐除外；然而，一些化合物难以解吸。选择了属于二苯甲酮和对氨基苯甲酸酯化学类别的10种紫外线过滤剂，并优化了从地表水萃取这些化合物以进行UHPLC-MS/MS测定的参数。然后，该方法在线性、准确性、室内精密度以及检测限和定量限方面进行了验证。总之，该方法性能（准确性，以分析回收率表示，85-114%；相对标准偏差5-15%）似乎适用于在10-100 ng/L水平下测定所选化合物，检测限在1-5 ng/L范围内。最后，将该新方法与基于用GCB进行常规固相萃取的已发表方法进行了比较，结果表明在实际样品分析中性能相似。图形摘要基于磁性固相萃取随后进行LC-MS/MS测定的分析方法工作流程。
