A protocol for wide-scope non-target analysis of contaminants in small amounts of biota using bead beating tissuelyser extraction and LC-HRMS

Abstract

This work describes a robust and powerful method for wide-scope target and non-target analysis of xenobiotics in biota samples based on bead beating tissuelyser extraction, solid phase extraction (SPE) clean-up and further detection by liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS). Unlike target methodologies, non-target methods usually aim at determining a wide range of still unknown substances with different physicochemical properties. Therefore, losses during the extraction process were minimised. Apart from that, the reduction of possible interferences showed to be necessary to expand the number of compounds that can be detected. This was achieved with an additional SPE clean-up step carried out with mixed-bed multi-layered cartridges. The method was validated with a set of 27 compounds covering a wide range of physicochemical properties, and further applied to the analysis of krill and fish samples. The bead beating extraction was efficient for a wide range of organic pollutants in small quantities of biota samples. Multi-layered solid phase extraction clean-up yield a wide xenobiotics coverage reducing matrix effects. Method validation with 27 compounds led to a suitable method for non-target analysis of organic pollutants in biota.

Exploring the Occurrence of Organic Contaminants in Human Semen through an Innovative LC-HRMS-Based Methodology Suitable for Target and Nontarget Analysis

“…Due to the nature of the method, the sample ends up being diluted. However, since some exogenous chemicals may be present at very low levels, we tested whether adding a preconcentration step could improve LODs in real samples using an already validated SPE methodology (named Method 2), which has given acceptable results in other matrices such as wastewater, 52 biota, 54 or placenta. 55 Method 2 was analogous to Method 1, but the supernatant was collected after protein precipitation (see SI-4).…”

An Overview of Analytical Methods to Determine Pharmaceutical Active Compounds in Aquatic Organisms

“…This is one of the simplest extraction techniques as it consists of stirring the sample with the extraction solvent for a certain time to ensure the migration of the analytes from the solid phase to the liquid one. Generally, this agitation is followed by centrifugation so that the decantation can take place and the phases can be separated correctly, leaving the target analytes dissolved in the liquid [ 92 , 93 ]. Not many studies based on the use of this technique have been found, as the time required is usually longer.…”

The Potential of Sewage Sludge to Predict and Evaluate the Human Chemical Exposome

“…Placenta samples (200 mg) were extracted with a mixture of ACN, citric acid buffer, and zirconium beads in a tissuelyser. Then, a SPE cleanup step with mixed mode cartridges was carried out as described elsewhere. , Sewage sludge (1 g) was extracted with a digital sonifier using ACN and water, and further cleanup and preconcentration steps were conducted through SPE. Procedural blanks ( n = 5 for each matrix) were processed following the same protocols, in order to assess potential contaminations.…”