Abstract

In this work, a method for the determination of nine polychlorinated biphenyls (PCBs) in three polymer types (polyethylene terephthalate, PET; unplasticized polyvinyl chloride, u-PVC; and low density polyethylene, LDPE) present in marine samples (mussel and marine water) was developed. To optimize extraction methods for PCBs in microplastics, a 2^4-1 fractional factorial design was applied. Four factors were optimized, namely, sample amount, number of extraction cycles, solvent volume and extraction time. For PET analysis, sample amount was statistically significant for 5 congeners (PCBs 105, 118, 153, 138 and 180), number of extraction cycles and solvent volume were statistically significant only for PCB 101 and extraction time was statistically significant for PCBs 153 and 101. In the case of u-PVC, statistical analysis revealed no relevant variables. For LDPE, sample amount and solvent volume were statistically significant for the lower chlorinated compounds and sample amount was also statistically significant for PCB 52. PCB extracts were analyzed by GC-MS/MS system (triple quadrupole). The separation step of microplastics from marine samples was also tested. For this purpose, studies of behavior of PCBs during the digestion of organic matter were also performed by using KOH and H₂O₂ solutions. The best results were achieved when 30% H₂O₂ solution was used. The analytical performance of extraction method demonstrated a broad linear concentration range (R² < 0.998), in general recoveries around 80–100% and relative standard deviation below 15%. The methodology was applied to the analysis of spiked mussel and seawater samples coming from Galicia coast (NW, Spain).

中文翻译：

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开发一种测定海洋样品中微塑料中多氯联苯的方法

摘要

在本工作中，一种测定海洋样品（贻贝和海水）中三种聚合物类型（聚对苯二甲酸乙二醇酯，PET；未增塑聚氯乙烯，u-PVC和低密度聚乙烯，LDPE）中的九种多氯联苯 ( PCB )的方法） 发展了。为了优化微塑料中 PCB 的提取方法，a 2 ^4-1应用了部分因子设计。优化了四个因素，即样品量、萃取循环次数、溶剂体积和萃取时间。对于 PET 分析，5 种同系物（PCB 105、118、153、138 和 180）的样品量具有统计学意义，萃取循环次数和溶剂体积仅对 PCB 101 具有统计学意义，萃取时间对 PCB 153 和 101 具有统计学意义. 在 u-PVC 的情况下，统计分析显示没有相关变量。对于 LDPE，低氯化化合物的样品量和溶剂体积具有统计学意义，PCB 52 的样品量也具有统计学意义。通过 GC-MS/MS 系统（三重四极杆）分析 PCB 提取物。还测试了从海洋样品中分离微塑料的步骤。以此目的，₂ O ₂溶液。当使用 30% H ₂ O ₂溶液时获得最佳结果。萃取方法的分析性能表现出较宽的线性浓度范围 ( R ² < 0.998)，一般回收率约为 80-100%，相对标准偏差低于 15%。该方法用于分析来自加利西亚海岸（西班牙西北部）的加标贻贝和海水样品。