An Alternative Approach for the Detection of Ethephon (2-Chlorethylphosphonic acid) Residues in Apples

Abstract

A rapid and simple GC/MS method to detect ethephon residues in apples is introduced using an internal standard and direct extraction of the analytes from the matrix at low pH with ethyl acetate. A one step derivatization procedure has been established using N-tert-butyldimethylsilyl-N-methyltrifluoracetamide (MTBSTFA) prior to GC/MS analysis performed in selected ion monitoring mode (SIM). Optimization of the derivatization and GC-parameters led to good method performance and measurement precision. Recovery experiments showed recovery rates ranging from 80.8 to 95.5% in the concentration range were investigated. The presented method provides significant improvements in laboratory safety, sample throughput and instrumentation cost compared with other methods to detect ethephon residues in apples.

Determination of 2‐chloroethylphosphonic acid and its intermediate vinylphosphonic acid from artificially ripened sapota fruit by modified dispersive solid‐phase extraction cleanup and gas chromatography/mass spectrometry analysis

“…The extraction efficiency of the solvents was estimated at a concentration of 2 μg/g levels of ethephon and VPA. The extraction of ethephon residues using ethyl acetate was reported in previous publications, 10,23 and this case yielded around 90% recoveries. Extraction using acetonitrile yielded very poor recovery due to the coelution of sugars and other various polar metabolites present in the fruit pulp samples.…”

“…The presence of ethephon was initially detected by identifying the ethylene gas released after alkaline treatment of the fruit pulp using headspace gas chromatography (GC)/MS 11,12,19–22 . Sensitive quantification of ethephon using GC/MS was also carried out after derivatization with N ‐( tert ‐butyldimethylsilyl)‐ N ‐methyl trifluoroacetamide 15,23 and methylation by diazomethane 9,24–27 . Ion‐pairing extraction followed by LC/MS/MS detection methods for the trace‐level quantification of ethephon from environmental water samples have also been reported 8,16 …”

A Multienzyme Reaction-Mediated Electrochemical Biosensor for Sensitive Detection of Organophosphorus Pesticides

“…For example, Niki et al developed ion exchange chromatography for indirect detection of ETH in soluble concentrate formulations [7]. Kröpfl et al developed a one-step derivatization procedure to improve the measurement accuracy of GC/MS analysis [8]. These methods, although highly sensitive, are subject to high background interference or have the disadvantages of high cost and large instrument size.…”

Analysis of highly polar anionic pesticides in food of plant and animal origin by ion chromatography and tandem mass spectrometry with emphasis on addressing adverse effects caused by matrix co-extractives

“…Due to their high polarity, these analytes are not amenable to the QuEChERS method [6,7], i.e., the most common multi-residue method in the area of pesticide residue analysis [8,9]. Former strategies for determining glyphosate and other highly polar analytes involved their derivatization in order to make them amenable to gas chromatography (GC) with mass spectrometry (MS) [10,11], nitrogen-phosphorus detection (NPD), or the flame photometric detection (FPD) [12]. Likewise, reversed-phase high-performance liquid chromatography in combination with fluorescence detection (HPLC-FLD) [13] or tandem mass spectrometry (LC-MS/ MS) [14,15] has been used for the determination of certain derivatives.…”