Optimization of a method based on micro-matrix solid-phase dispersion (micro-MSPD) for the determination of PCBs in mussel samples

Nieves Carro, Laura Vilas, Isabel García, María Ignacio, Ana M. Mouteira
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引用次数: 12

Abstract

This paper reports the development and optimization of micro-matrix solid-phase dispersion (micro-MSPD) of nine polychlorinated biphenyls (PCBs) in mussel samples (Mytilus galloprovincialis) by using a two-level factorial design. Four variables (amount of sample, anhydrous sodium sulphate, Florisil and solvent volume) were considered as factors in the optimization process. The results suggested that only the interaction between the amount of anhydrous sodium sulphate and the solvent volume was statistically significant for the overall recovery of a trichlorinated compound, CB 28. Generally most of the considered species exhibited a similar behaviour, the sample and Florisil amounts had a positive effect on PCBs extractions and solvent volume and sulphate amount had a negative effect. The analytical determination and confirmation of PCBs were carried out by using GC-ECD and GC-MS/MS, respectively. The method was validated having satisfactory precision and accuracy with RSD values below 6% and recoveries between 81 and 116% for all congeners. The optimized method was applied to the extraction of real mussel samples from two Galician Rías.

微基质固相色散法测定贻贝样品中多氯联苯的优化研究
采用双水平析因设计,研究了贻贝样品(Mytilus galloprovincialis)中9种多氯联苯(PCBs)的微基质固相分散(micro-MSPD)。在优化过程中考虑了样品量、无水硫酸钠、Florisil和溶剂体积四个变量。结果表明,只有无水硫酸钠用量与溶剂体积的相互作用对三氯化合物cb28的整体回收率有统计学意义。一般来说,大多数被考虑的物种表现出类似的行为,样品和Florisil的量对多氯联苯的提取有积极影响,而溶剂体积和硫酸盐的量有消极影响。采用GC-ECD和GC-MS/MS对样品中多氯联苯进行分析测定和确证。结果表明,该方法精密度和准确度均较好,RSD值在6%以下,加样回收率在81 ~ 116%之间。将优化后的方法应用于两个加利西亚Rías贻贝样品的提取。
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