Gas Purge Microextraction Coupled with Stable Isotope Labeling-Liquid Chromatography/Mass Spectrometry for the Analysis of Bromophenols in Aquatic Products.

Abstract

A green, sensitive, and accurate method was developed for the extraction and determination of bromophenols (BPs) from aquatic products by using organic solvent-free gas purge microsyringe extraction (GP-MSE) technique in combination with stable isotope labeling (SIL) strategy. BPs were extracted by NaHCO3 buffer solution, with recoveries varying from 92.0% to 98.5%. The extracted solution was analyzed by SIL strategy, during which analytes and standards were labeled by 10-methyl-acridone-2-sulfonyl chloride (d0-MASC) and its deuterated counterpart d3-MASC, respectively. The labeling reaction was finished within 10 min with good stability. The liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) sensitivity of BPs was greatly enhanced due to the mass-enhancing property of MASC, while the matrix effect was effectively minimized by the SIL strategy. The limits of detection (LODs) were in the range of 0.10-0.30 μg/kg, while the limits of quantitations (LOQs) were in the range of 0.32-1.0 μg/kg. The proposed method also showed great potential in the qualitative analysis of other bromophenols in the absence of standard.