Determination of the Phenoxyacid Herbicides MCPA, Mecoprop and 2,4-D in Kidney Tissue Using Liquid Chromatography with Electrospray Tandem Mass Spectrometry

Abstract

An analytical method was developed to determine the phenoxyacid herbicides 2,4-D, MCPA and mecoprop in kidney tissue from animals where poisoning is suspected. Samples were Soxhlet extracted using diethyl ether and the extracts cleaned-up using anion exchange solid phase extraction cartridges. Analysis was performed using liquid chromatography with negative-ion electrospray tandem mass spectrometry (LC-MS/MS). The method was evaluated by analysing control kidney samples fortified at 1 and 5 mg/kg. Mean recoveries ranged from 82 to 93% with relative standard deviations from 3.2 to 19%. The limit of detection was estimated to be 0.02 mg/kg.

Chemical Analysis of Pesticides Using GC/MS, GC/MS/MS, and LC/MS/MS

“…The chlorophenols which are transformation products of the phenoxy acid herbicides can also be converted to their carbonates for GC/MS analysis using alkylchloroformates (Henriksen et al, 2001). These approaches can suffer from deteriorating peak shapes over time and reduced column lifetime (Charlton et al, 2009). Carbamates are thermally labile and can breakdown in the injector port or on-column to their corresponding phenols and amines and consequently derivatization using acetylation, silylation, alkylation, or perfluorination is required.…”

“…On-column derivatization with trimethylphenylammonium hydroxide and trimethylsulfonium hydroxide has been used to give thermally stable products for a variety of carbamates including carbaryl, methiocarb, chlorpropham, propham, and promecarb that can be analyzed by GC-EI/MS (Zhang and Lee, 2006). In more recent years there has been a shift to LC/MS/MS methods (see section 3.2) for both phenoxyacid herbicides and carbamates as these methods do not require the derivatization step and can provide an ability to simultaneous analyze transformation products and often a wider range of pesticides within the same chemical class (Raina and Etter, 2010;Charlton et al, 2009;Chung and Chan, 2010). To achieve the necessary MDLs required for environmental or food analysis the majority of GC/MS pesticide analysis methods are in SIM mode with either single quadrupole or iontrap systems with ion-traps providing similar or slightly higher MDLs than the more popular quadrupole systems.…”

Deposition of CdTe quantum dots on microfluidic paper chips for rapid fluorescence detection of pesticide 2,4-D

“…3 Upon accumulation in food chain, indeed, 2,4-D is associated with the occurrence of human cancer, endocrine disruption, acute congestion, and neurodegeneration. 4 2,4-D concentration has already been evaluated by different analytical methods, such as LC-MS, 1,5 chromatography, 2,6 electrochemistry, 7 and surface-enhanced Raman spectroscopy. 8 These technologies are powerful analytical techniques that provide high sensitivity and specificity.…”

Rapid and sensitive detection of the phenoxy acid herbicides in environmental water samples by magnetic solid‐phase extraction combined with liquid chromatography–tandem mass spectrometry

“…CE and HPLC–UV are not very sensitive and selective for the trace analysis. HPLC–MS/MS in multiple reaction monitoring mode could provide better sensitivity, selectivity, and molecular weight information for exact identification, making this technique very suitable for the trace analysis of phenoxy acid herbicides in environmental water samples .…”