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 NaHCO 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 (d-MASC) and its deuterated counterpart d-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.

Comprehensive Insights into the Interactions of Two Emerging Bromophenolic DBPs with Human Serum Albumin by Multispectroscopy and Molecular Docking

“…For example, 4-bromophenol was 181 and 39 times more toxic than bromoacetic acid in terms of developmental toxicity and growth inhibition, respectively. , Their occurrence can cause off-flavor problems from the perspective of high-quality water supply, and the odor threshold concentrations of some bromophenols are in the ng/L level . In addition, bromophenols can be extensively found in various seafoods (such as prawns, fish, and crustaceans) and are considered to be ubiquitous in the lower levels of marine food webs. , Also, they are widely used in various industrial products (e.g., flame retardant intermediates and polymer intermediates) and thus are known as environmental micropollutants in freshwater environments. − Accordingly, two bromophenolic DBPs 4-bromophenol (4-BrPh) and 2,4-dibromophenol (2,4-DiBrPh) were chosen as representatives of emerging aromatic DBPs and target compounds in this study. The primary objective of this work was to investigate the binding interactions of the two bromophenolic DBPs with HSA under simulated physiological conditions of human blood, by using multiple spectroscopic techniques (i.e., fluorescence, absorption, and circular dichroism (CD) spectroscopy) and a molecular docking method.…”

“…27 In addition, bromophenols can be extensively found in various seafoods (such as prawns, fish, and crustaceans) and are considered to be ubiquitous in the lower levels of marine food webs. 28,29 Also, they are widely used in various industrial products (e.g., flame retardant intermediates and polymer intermediates) and thus are known as environmental micropollutants in freshwater environments. 30−32 Accordingly, two bromophenolic DBPs 4bromophenol (4-BrPh) and 2,4-dibromophenol (2,4-DiBrPh) were chosen as representatives of emerging aromatic DBPs and target compounds in this study.…”

Analysis of Potent Odour-Active Volatile Thiols in Foods and Beverages with a Focus on Wine

“…The maleimide moiety in PIPD can rapidly react with thiols to form derivatives that are stable (4 °C for at least three days) and detectable by HPLC–fluorescence (with atmospheric pressure chemical ionisation (APCI)-MS used for identification) [45]. Thiol extraction was performed with GP–MSE (N 2 at 2.5 mL/min for 30 min at 190 °C) in a customised apparatus prior to derivatisation (10 min at 35 °C in phosphate buffered saline, pH 7.5) [54]. After extraction and derivatisation, the mixtures were diluted with methanol (MeOH), filtered, and directly injected [45].…”

Stable isotope labeling assisted liquid chromatography–tandem mass spectrometry for the analysis of perfluorinated carboxylic acids in serum samples

“…The light and heavy versions of the labeling reagents show highly similar chemical property and thus the derivatization can be carried out under the same conditions. After derivatization, light and heavy labeled analytes are mixed and analyzed by liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) [9][10][11][12][13][14]. The isotopic pairs of the labeled analytes are analyzed within a single run and thus have identical retention times.…”

“…Charge reversal derivatization can be achieved by this strategy to enhance the HPLC-MS/MS sensitivity of compounds like carboxylic acids and phenols [14,15].…”