APPLICATION OF THE METHOD OF LIQUID CHROMATOGRAPHY WITH MASS SPECTROMETRY DETECTION FOR THE DETERMINATION OF DIQUATE IN OIL CULTURES
DOI:
https://doi.org/10.11603/mcch.2410-681X.2023.i2.13647Keywords:
diquat, oil cultures, limit of quantification, liquid chromatograph using the triple quadrupole mass spectrometerAbstract
Introduction. The article describes the scientific rationale for the choice of method, development of conditions for sample preparation of soybean, sunflower and rapeseed seeds, qualitative identification and quantification determination in these matrices of the highly polar herbicide diquat, which is part of crop protection systems.
The aim of the study – to develop methods for the determination of diquat in soybeans, sunflower seeds and rapeseed with the limit of quantitative determination 0.01 mg/kg.
Research Methods. Chromatographic analysis was performed by Shimazu (Japan) liquid chromatograph using the triple quadrupole mass spectrometer. Mass spectrometric detection upon multiple reaction recording (MRM) conditions with electrospray ionization (ESI) in positive mode occurred after chromatographic separation on a Kinetex HILIC column. The correctness and accuracy of the determination of the investigated compound in samples of agricultural crops were checked by the "introduced-found" method. The package of IBM SPSS StatisticsBase v.22 and MS Exel statistical programs was used for statistical processing of results.
Results and Discussion. The method is based on extraction with an acidified methanol-water mixture with the application of an heating step. Optimal conditions for sample preparation of soybean, sunflower and rapeseed seeds, chromatographic separation on a hydrophilic (normal-phase) column, and quantitative measurement of diquat using tri-quadrupole mass spectrometric detection were developed to provide the determination of the analyzed compound with a limit of quantification determination of 0.01 mg/kg with the required precision (on levels from 70 to 120 %) and accuracy (RSD≤20 %).
Conclusions. Developed method for determination diquat in soybeans, sunflower seeds and rapeseed by liquid chromatograph using the triple quadrupole mass spectrometer allow to control the established hygienic standards, to obtain representative information on the content of pesticide residues, which is a prerequisite for risk assessment of plant protection products.
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