Optimization of a Multiresidue Analysis of 65 Pesticides in Surface Water Using Solid-Phase Extraction by LC-MS/MS

Abstract

An analytical method was developed and validated for simultaneous quantitation of 65 pesticides, including one single solid-phase extraction (SPE) procedure in surface water by liquid chromatography coupled to tandem mass spectroscopy. Different parameters that have an influence on extraction efficiency were evaluated in this research. Different types of cartridges, elution solvents, and sorbent drying time were investigated, and the most appropriate one was selected. Moreover, various pretreatment techniques were applied to remove sediments from water without the loss of pesticides. Centrifugation was introduced as the best option at the beginning of sample preparation to resolve the clogging of the sorbent cartridges. The recoveries of all pesticides ranged from 70% to 120%, with a relative standard deviation of less than 13.7%. The feasibility of the method was evaluated on 10 surface water samples with different concentrations of sand, sediment, and particles.

An Alternative Strategy for Screening and Confirmation of 330 Pesticides in Ground- and Surface Water Using Liquid Chromatography Tandem Mass Spectrometry

“…The mobile phase consisting only of ammonium formate as eluent additives enabled the simultaneous analysis of 480 pesticides using scheduled multiple reaction monitoring (MRM) detection in the MS/MS instrument ( Table S1 ). This eluent composition is rather different from those used earlier [ 2 , 14 , 15 , 16 , 18 , 19 , 20 , 21 , 26 , 29 , 30 , 31 , 32 ].…”

“…Additionally, both GC and HPLC analysis may be used to cover as many compounds as possible. In recent papers, the detection of 20–300 pesticides in water could be achieved if both GC-MS and LC-MS were used in the method [ 5 , 7 , 8 , 9 , 18 , 19 , 20 , 21 , 29 , 30 , 31 , 32 ]. For GC-MS analysis, the liquid–liquid extraction (LLE) of water with immiscible organic solvent such as diethyl ether or dichloromethane is a preferable approach to enrich pesticides [ 2 , 27 , 33 , 34 ].…”

“…This sample pre-concentration method is quite selective and is a good tool to pre-concentrate more volatile compounds; however, it requires a high volume of organic solvent that does not meet the purpose of green analytical chemistry [ 35 ]. The extraction of more hydrophilic compounds with LLE results in losses during sample preparation, therefore solid-phase extraction (SPE) shall be employed to obtain fit-for-purpose recovery for a broader range of analytes [ 2 , 18 , 19 , 20 , 21 , 29 , 30 , 31 , 36 , 37 ]. SPE utilizing modified hydrophilic polymeric cartridges enables the extraction of both polar and non-polar compounds if the sample pH is optimal [ 22 , 23 , 24 , 28 , 33 , 36 , 37 ].…”

A new on-line SPE LC-HRMS method for simultaneous analysis of selected emerging contaminants in surface waters

“…This is generally done using either sample ltration or centrifugation. 95 Some studies have shown that ltration is not a viable pretreatment step because some lters such as glass wool and nylon might adsorb PFASs and pesticides from water sample and therefore, reduce recovery of those compounds. [81][82][83][84][85][86][87][88][89][90][91][92][93][94][95] Also, several PFASs have been reported to leach out from some lters such as PTFE and thus can potentially contaminate samples during ltration.…”

“…95 Some studies have shown that ltration is not a viable pretreatment step because some lters such as glass wool and nylon might adsorb PFASs and pesticides from water sample and therefore, reduce recovery of those compounds. [81][82][83][84][85][86][87][88][89][90][91][92][93][94][95] Also, several PFASs have been reported to leach out from some lters such as PTFE and thus can potentially contaminate samples during ltration. 50 Therefore, centrifugation was chosen to remove sediment and suspended solids from surface water samples in our study.…”