This paper describes the development and validation of a new procedure for the determination of phthalates in marine invertebrates, based on biocompatible solid-phase microextraction (BioSPME) followed by liquid chromatography coupled to mass spectrometry. The importance of this application relies on the current use of marine organisms as bioindicators for microplastic contamination through the detection of phthalates in their tissues. Challenges originate from the availability and/or possible restriction on the use of the biological materials, the need for user- friendly procedures for simplifying and speeding up operations in the marine environments, and the ubiquitous presence of phthalates in the laboratory environments that may cause background contamination. BioSPME served as an effective solution to all these issues, owing to the extreme minimization of the sample manipulation. Sampling operations were limited to the direct transfer of small amounts of the biological materials (150 mg) inside glass vials capped with aluminium lids; extractions were carried out by ultrasonication in acetone followed by dilution in ultrapure water and BioSPME clean-up; Electrospray (ESI) LC-MS/MS was employed for the final analytical determinations on the purified extracts. Tests were carried out on samples belonging to three different phyla, namely Cnidaria, Porifera, and Mollusca obtained from Maldivian coral reef environments and used for a current microplastic contamination biomonitoring project. Overall, very good sensitivity and repeatability, with negligible back contamination of the blanks were observed. The limits of detections were between 0.2 and 2.1 ng/g and precision, calculated as relative standard deviation (RSD), was below 14% for all the tested phthalates.

中文翻译：

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生物相容性固相微萃取结合液相色谱三重四极杆质谱分析法测定海洋无脊椎动物中的邻苯二甲酸盐。

本文介绍了一种基于生物相容性固相微萃取（BioSPME），然后将液相色谱与质谱联用的测定海洋无脊椎动物中邻苯二甲酸盐的新方法的开发和验证。此应用程序的重要性取决于当前通过检测海洋生物组织中的邻苯二甲酸盐来将海洋生物用作微塑性污染的生物指示剂。挑战来自于生物材料的可用性和/或可能的限制，对简化和加快海洋环境中操作操作的用户友好程序的需求以及实验室环境中普遍存在的邻苯二甲酸酯可能会导致背景污染。BioSPME是解决所有这些问题的有效解决方案，由于极大地减少了样品处理。采样操作仅限于将少量生物材料（150 mg）直接转移到盖有铝盖的玻璃小瓶中。通过在丙酮中超声处理，然后在超纯水中稀释和BioSPME净化进行萃取。电喷雾（ESI）LC-MS / MS用于纯化提取物的最终分析测定。对属于三个不同门的样品进行了测试，这些样品分别从马尔代夫的珊瑚礁环境中获得，属于矢车菊，紫叶菊和软体动物，并用于当前的微塑性污染生物监测项目。总体而言，观察到非常好的灵敏度和可重复性，而空白的背面污染可忽略不计。检出限在0.2到2之间。