Accelerated solvent extraction then liquid chromatography coupled with mass spectrometry for determination of 4-t-octylphenol, 4-nonylphenols, and bisphenol A in fish liver

Abstract

SummaryAnalysis of extracts from fish liver containing alkylphenol contaminants can be hindered by the presence of co-extracted fats and proteins that interfere with chromatographic analysis. In this study accelerated solvent extraction (ASE), Florisil clean-up, then combined liquid chromatography -mass spectrometry (LC-MS) with an electrospray (ESI) interface have been used to optimize an analytical procedure for the analysis of octylphenol, nonylphenol, and bisphenol A in fish liver. After comparison of the efficiency of ASE with conventional Soxhlet extraction the developed procedure was applied to the analysis of liver samples. Calibration plots of the relationship between concentration and the ratio of the responses to the analyte and to the internal standard, 4-n-nonylphenol, were determined by linear regression analysis over the concentration range 0.05 to 10 ppm and resulted in good fits (r 2 > 0.994). Recoveries (evaluated for each liver sample as the ratio between response to the surrogate compound, 4-n-nonylphenol, and that to the internal standard, 4-n-heptylphenol, relative to the same ratio for a reference standard solution) were 53 • 20%.Under the experimental conditions used in this work the limits of detection (LOD), calculated by use of a signal-to-noise ratio of 3:1, were 5 ng g 1 for4-t-odylphenol, 15 ng g 1 for bisphenol A, and 20 ng g 1 for nonylphenol. The method can be satisfactorily applied to screening analysis of odyl-and no@phenols and bisphenol A in biological samples such as fish liver.

Development of Direct ELISA for the Determination of 4-Nonylphenol and Octylphenol

“…10 Correlation between exposure to alkylphenols and deleterious reproductive consequences has led to widespred surveys of levels NP and OP in the rivers, sewage efluent, and estuaries of many countries. 11 Several papers have been published on the contamination of fish and other aquatic organisms by octyl-and nonylphenols. [12][13][14][15][16] It has appeared from the recent studies that NP, OP, and to some extent also the shorter APEO homologues and carboxylic metabolites exert estrogenic effects in the above species.…”

Bisphenol A and Metabolites in Meat and Meat Products: Occurrence, Toxicity, and Recent Development in Analytical Methods

“…As an example, MAE has been used in the extraction of BPA from fish and seafood samples (prawns, crabs, cockles, white clams, and squids) using dichloromethane/methanol or tetramethylammonium hydroxide (TMOH) as solvents [ 90 , 91 ]. In addition, BPA extraction from fish liver [ 92 ] and meat products (pork, meat, rabbit, duck, and chicken) [ 84 ] has been performed using PLE and acetone/-n-hexane and dichloromethane as solvents, respectively. To optimize the extraction of BPA-diglycidyl ether (BADGE) from canned fish samples, Lapviboonsuk and Leepipatpiboon investigated the use of a QuEChERS method applying primary secondary amine (PSA) and C18 sorbents for the clean-up [ 93 ].…”

Analysis of estrogens and estrogen mimics in edible matrices—A review

“…ASE has been applied for analyzing BPA, OP, and NP in meat by LC–MS/MS . Other authors have extracted APs from fish liver using ASE and Florisil clean‐up, comparing the efficiency of ASE with conventional Soxhlet extraction. Carabias et al determined the levels of BPA and NP in cereals using ASE.…”