Determination of selected emerging contaminants in freshwater invertebrates using a universal extraction technique and liquid chromatography accurate mass spectrometry

Abstract

A simple sample preparation method based on a modified liquid-phase extraction approach to extract selected pharmaceuticals and personal care products from freshwater organisms is described. Extracted samples were analysed using liquid chromatography with Q-Exactive plus hybrid quadrupole Orbitrap mass spectrometry, using 2.6 μm C18 media. A 0.1% v/v acetic acid/acetonitrile mobile phase was applied over a 20 min gradient. Method detection limits in full scan mode were ca. 0.04-2.38 ng of analyte per g of sample. Linearity ranged from 0.9750 to 0.9996 over the calibration range of 0.01-100 μg/L; MS mass accuracy was <2 ppm for most analytes. This method was applied to quantify six pharmaceuticals and personal care products in seven invertebrate samples. For tandem mass spectrometry analysis, selection of precursor ions was performed for each pharmaceutical, with Mass Frontier software illustrating the fragmentation mechanism. Effects of collision energy on intensities of ions was further investigated. The tandem mass spectrometry condition resulting in the highest signal of respective selected product ion was selected to confirm each pharmaceutical, which was initially observed in the full scan mode. Results indicate that pharmaceuticals and personal care products found to be present in water-ways, may be incorporated into organisms that live in the environment of affected water streams.

Biomonitoring of pesticides, pharmaceuticals and illicit drugs in a freshwater invertebrate to estimate toxic or effect pressure

“…The sensitivity of the method was comparable to others that have determined pharmaceuticals and pesticides in invertebrates. For example, Inostroza et al, had method quantification limits (MQLs) of 0.01–2.13 ng g −1 wet weight (Inostroza et al, 2016), Althakafy et al, reported detection limits ranging 0.04–2.38 ng g −1 wet weight (Althakafy et al, 2018) and Munz et al, achieved LOQs of 0.1 to 9 ng g −1 wet weight (Munz et al, 2018). Linearity was acceptable (R 2 > 0.98) and the chromatographic separation showed good reproducibility with an average standard deviation in retention time of ±0.015 min ( n = 5).…”

An efficient resin for solid-phase extraction and determination by UPLCMS/MS of 44 pharmaceutical personal care products in environmental waters

“…With the high usage of pharmaceutical and personal care products (PPCPs) in the last two decades, various PPCPs have been frequently detected in environmental matrices around the world (Althakafy et al, 2018;Spongberg et al, 2011;Zhang et al, 2015). Most PPCPs with potential hazards are present at low levels in the environment, accompanied by high polarity, and various physicochemical properties, which lead to difficulties in detection.…”

Multi‐residue analysis of 44 pharmaceutical compounds in environmental water samples by solid‐phase extraction coupled to liquid chromatography‐tandem mass spectrometry

“…Among the great diversity of pollutants reaching our water supplies, pharmaceutically active compounds are one of the largest inputs . As pharmaceuticals consumption is continuously increasing , it raises concerns about their impact on the environment and undesired physiological effects they can cause to aquatic organisms . Their presence was investigated worldwide in different aquatic matrices (e.g., water, sediments, and biota) , and a large number of compounds were detected, especially in wastewaters at concentrations ranging from nanogram to microgram per liter .…”