Semi-automated liquid chromatography–mass spectrometry (LC–MS/MS) method for basic pesticides in wastewater effluents

Abstract

Effluent from wastewater treatment plants have been identified as an important source of micro-organic contaminants in the environment. An online high-performance liquid chromatography-heated electrospray ionization tandem mass spectrometric method was developed and validated for the determination of basic pesticides in effluent wastewaters. Most available methods for pesticide analysis of wastewater samples are time-consuming, require complex clean-up steps and are difficult to automate. The method developed used a simple solid-phase extraction clean-up for salt and lipid reduction. On-line sample pre-concentration was performed using a reversed phase (C(18)) column, and analytes were separated by back-flushing onto an analytical column (C(8)) with detection using QqQ MS. An option to increase MS resolution was exploited to minimize interference from endogenous compounds in the matrix. A better than unit mass resolution was used (Q1 full width half maximum (FWHM) = 0.2 Da and Q3 FWHM = 0.7 Da), which was as rugged as a unit resolution method, and improved signal/noise and better detection limits were achieved for the targeted basic pesticides. This method was applied to the determination of 11 pesticides, including methoxytriazine, chlorotriazines, chloroacetanilides, phenylurea and carbamate pesticides. The percentage recovery values for these pesticides using the online trapping column were within the range, 73-95%, with relative standard deviation (RSD) values <8.9%. The highest concentrations of these pesticides in wastewater effluents in County Cork, Ireland, were simazine (0.51 μg/L), prometon (0.14 μg/L), diuron (0.21 μg/L) and atrazine (0.19 μg/L).

Photoinduced chemiluminescence determination of carbamate pesticides

“…Therefore, prior derivatization is desirable when GC analysis is performed. 7 In LC, different detection techniques have been used, such as ultraviolet 8,9 or fluorescence, 10,11 but mass spectrometry is the preferred technique [12][13][14] because it provides high sensitivity and selectivity with LODs of a few pg mL -1 . However, this technique is not available for all laboratories due to the high cost and complexity of the instrumentation.…”

Synthesis of Isotopically Labeled 13C3-Simazine and Development of a Simultaneous UPLC-MS/MS Method for the Analysis of Simazine in Soil

“…Even though many studies use deuterium-labeled congeners to detect the simazine residues [16,17], the 13 C-labeled internal standard is more appropriate for accurate quantification, because its physico-chemical properties and chromatographic behavior are more similar to the native target analysed [23].…”

“…In previous studies, the quantitative analyses of simazine include pre-column derivatization liquid chromatographic fluorescence detection (LC-FL) [12], antigen-coated tube enzyme-linked immune Molecules 2016, 21, 89 2 of 8 sorbent assay (ELISA) [13], high-performance liquid (HPLC) [14], gas chromatography coupled with mass spectrometric detection (GC-MS) [15] as well as liquid chromatography-tandem mass spectrometry (LC-MS/MS) [16][17][18]. Recently, LC-MS/MS has been widely applied in trace analysis of pesticides.…”

Urban effluent discharges as causes of public and environmental health concerns in South Africa’s aquatic milieu

“…This drastically alters the natural balance in environmental water quality, thereby raising a plethora of public health and ecotoxicological concerns (Yadav et al 2005;Gabriel et al 2006;Schwarzenbach et al 2010;de Vargas et al 2014). Wastewater effluents, in particular, can harbour a potentially wide array of contaminants ranging from genotoxicants and cytotoxicants (Wirzinger et al 2007;Žegura et al 2009), heavy metals and metalloids (Lohner et al 2001;Ahmad et al 2013), nutrients (Carey and Migliaccio 2009), pesticides (Cahill et al 2011;Köck-Schulmeyer et al 2013), pathogens (Dungeni et al 2010;Odjadjare et al 2010), hydrocarbons, organic matter and endocrine disruptors (e.g. 17β-estradiol, estrone and testosterone) (Ying et al 2004;Comerton et al 2009), among others.…”