Determination of Glyphosate, Maleic Hydrazide, Fosetyl Aluminum, and Ethephon in Grapes by Liquid Chromatography/Tandem Mass Spectrometry

Abstract

A simple high-throughput liquid chromatography/tandem mass spectrometry (LC-MS-MS) method was developed for the determination of maleic hydrazide, glyphosate, fosetyl aluminum, and ethephon in grapes using a reversed-phase column with weak anion-exchange and cation-exchange mixed mode. A 5 g test portion was shaken with 50 mM HOAc and 10 mM NaEDTA in 1/3 (v/v) MeOH/HO for 10 min. After centrifugation, the extract was passed through an Oasis HLB cartridge to retain suspended particulates and nonpolar interferences. The final solution was injected and directly analyzed in 17 min by LC-MS-MS. Two MS-MS transitions were monitored in the method for each target compound to achieve true positive identification. Four isotopically labeled internal standards corresponding to each analyte were used to correct for matrix suppression effects and/or instrument signal drift. The linearity of the detector response was demonstrated in the range from 10 to 1000 ng/mL for each analyte with a coefficient of determination (R) of ≥0.995. The average recovery for all analytes at 100, 500, and 2000 ng/g (n = 5) ranged from 87 to 111%, with a relative standard deviation of less than 17%. The estimated LOQs for maleic hydrazide, glyphosate, fosetyl-Al, and ethephon were 38, 19, 29, and 34 ng/g, respectively.

Glyphosate influences cell proliferation in vitro

“…The control and sample were diluted to 1:10 for the measurement, and 12 μM (2 ng/μl) glyphosate and AMPA at the same concentration were used as references for quantification. Peaks were confirmed to be ionized glyphosate or AMPA through product ion identification (glyphosate 150.5 m/z; AMPA 63.15 m/z) ( Figures S3-4) (Chamkasem 2017).…”

Real-Time Monitoring of Translocation, Dissipation, and Cumulative Risk of Maleic Hydrazide in Potato Plants and Tubers by Ion Exclusion Chromatography

“…Chromatographic techniques have been carried out to analyze MH residues in plants. For example, MH residues were determined in cured tobacco by gas chromatography, in garlic bulbs, potatoes, and onions by high-performance liquid chromatography, , and in tobacco and grapes by liquid chromatography with tandem mass spectrometry. , The improvement in instrumentation and analytical techniques has provided more sensitive detection of MH residues. , However, MH translocation and distribution in plants have been less studied due to the technical difficulties associated with simultaneous multiple tissues and soil experiments . Ion chromatography (IC) is a powerful analytical tool in the detection of small-molecule organic compounds and enables the multiresidue simultaneous determination of polar anionic pesticides in fruit and vegetables. , The IC techniques offer an enormous range of possibilities for selecting stationary and mobile phases and have a broad range of application in agriculture, pharmaceutical, and clinical studies because of ease of operation, high sensitivity, and online performance. , We previously reported the use of an effective IC method for real-time accurate analysis of tricarboxylic acid cycle metabolites in insect hemocytes .…”

Development and Application of a Novel Pluri-Residue Method to Determine Polar Pesticides in Fruits and Vegetables through Liquid Chromatography High Resolution Mass Spectrometry

“…The QuPPe method was modified by several authors. Some of them used additional cleaning steps with OASIS cartridges [10,11] or carbon nanotubes [12]. Other authors utilized alternative methods, such as extraction with acetonitrile and n-hexane for the extraction of ethephon from tomatoes [13], or the use of an aqueous solution of ethylenediaminetetraacetic acid (EDTA) acidified with acetic acid to improve the extraction of glyphosate, glufosinate and AMPA from grapes [11].…”