a Department of Chemical Engineering, Aristotle University of Thessaloniki , Thessaloniki , Greece.
b Sewerage Quality Control Laboratory, Management of Facilities and Sewerage Networks, Thessaloniki Water Supply & Sewerage Company S.A ., Thessaloniki , Greece.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2019 Aug;36(8):1253-1260. doi: 10.1080/19440049.2019.1615642. Epub 2019 Jun 4.
Mussels, a marine filter organism, constitute a food product and an established sentinel organism for marine pollution. An analytical method following a QuEChERS extraction and clean-up protocol has been developed for the determination of phthalic acid esters (PAE), including di-n-octyl phthalate (DnOP), di-(2-ethyl hexyl) phthalate (DEHP), butyl benzyl phthalate (BBP), di-methyl phthalate (DMP) and di-n-butyl phthalate (DnBP), as well as 3,4-dichloroaniline and 3,5-dichloroaniline in lyophilised mussels samples. A gradient elution program starting from 40% A (methanol-0.1% formic acid) - 60% B (HO-0.1% formic acid) up to 100% A was applied, with a total duration of 15 min, at a flow rate of 200 μL min using a 1.8 μm particle size C18 analytical column. All target analytes were detected with a triple quadrupole MS, using electrospray ionisation (ESI) in positive ionisation mode, in SRM mode under optimised conditions. Sample preparation consisted of lyophilisation of the mussels sample and grinding, followed by a QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) protocol. Among the different dispersants evaluated for sample clean-up effectiveness, primary secondary amine (PSA) was found to be the most efficient. Results indicated good chromatographic separation, fast sample preparation procedure, low LODs and LOQs, good trueness expressed as recovery and good precision as evaluated by RSD. In the mussels samples examined DEHP was the most abundant PAE, reaching a maximal concentration of 280 μg/kg of lyophilised weight whereas the levels of DnBP were at approximately 36% of the legal migration limit in foods determined by the EU.
贻贝是一种海洋滤食生物，既是一种食品，也是海洋污染的一种既定监测生物。本研究建立了一种基于 QuEChERS 提取和净化方法的分析方法，用于测定冷冻贻贝样品中的邻苯二甲酸酯（PAE），包括邻苯二甲酸二辛酯（DnOP）、邻苯二甲酸二（2-乙基己基）酯（DEHP）、邻苯二甲酸丁基苄基酯（BBP）、邻苯二甲酸二甲酯（DMP）和邻苯二甲酸二正丁酯（DnBP），以及 3,4-二氯苯胺和 3,5-二氯苯胺。采用 40%A（甲醇-0.1%甲酸）-60%B（水-0.1%甲酸）的梯度洗脱程序，总洗脱时间 15 min，流速 200 μL/min，使用 1.8 μm 粒径 C18 分析柱。在优化条件下，采用电喷雾离子化（ESI）正离子模式，三重四极杆质谱（MS），以选择反应监测（SRM）模式对所有目标分析物进行检测。贻贝样品制备过程包括冷冻干燥和研磨，然后采用 QuEChERS（快速、简单、廉价、有效、坚固、安全）方法进行净化。在评价的几种分散剂中，发现伯仲胺（PSA）对样品净化效果最好。结果表明，该方法具有良好的色谱分离效果、快速的样品制备程序、较低的检出限和定量限、以回收率表示的良好准确度和以相对标准偏差（RSD）表示的良好精密度。在所检测的贻贝样品中，DEHP 是最丰富的 PAE，达到 280 μg/kg 冻干重量的最高浓度，而 DnBP 的浓度约为欧盟规定的食品中迁移限量的 36%。
