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  • Pesticide determination in rose petals using dispersive solid-phase extraction followed by gas chromatography-tandem mass spectrometry.

Pesticide determination in rose petals using dispersive solid-phase extraction followed by gas chromatography-tandem mass spectrometry.

Analytical and bioanalytical chemistry (2014-10-27)
Oriane Tascone, Marina Shirshikova, Céline Roy, Uwe J Meierhenrich
ABSTRACT

Damascena and centifolia roses are cultivated worldwide for their petal extracts that contain key odorant ingredients of perfumes. The analytical identification and quantification of pesticides in rose petals have never been described in the literature. Here, we report on a newly developed method using dispersive solid-phase extraction (d-SPE) cleanup followed by gas chromatography-tandem mass spectrometry for the quantitative determination of multi-residue pesticides in rose petals. Analytes were extracted from the matrix using acetonitrile and a mixture of salts containing magnesium sulfate, sodium citrate, sodium chloride, and sodium sesquihydrate. Samples were cleaned up twice by d-SPE applying primary and secondary amines (PSAs), magnesium sulfate, C18, and graphitized carbon black (GCB). Two fortification levels of 0.05 and 0.5 mg kg(-1) were assessed for method validation purposes. The obtained pesticide recoveries were in the range of 70-120 % with a relative standard deviation (RSD) of less than 20 %. The newly developed method was allowed for the quantification of 57 pesticides residues. It was applied to pesticide residue detection in rose petals from an organic field, without treatment, compared to those from a field with classic phytosanitary treatment using fungicide and/or insecticide. We did not detect pesticide residues in rose petals from the organic field. The classically treated samples of roses contained pesticides such as chlorpyriphos and methidathion which are in accordance with the previous application of these pesticides on the roses. Insecticides were quantified at 0.05 mg kg(-1) rose petal maximum.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Acetic acid, glacial, ACS reagent, ≥99.7%
Sigma-Aldrich
Acetic acid, glacial, ReagentPlus®, ≥99%
Carbon - Vitreous, rod, 200mm, diameter 10mm, glassy carbon
Carbon - Vitreous, foil, 100x100mm, thickness 2.0mm, glassy carbon
Carbon - Vitreous, rod, 200mm, diameter 3.0mm, glassy carbon
Carbon - Vitreous, foam, 150x150mm, thickness 3.2mm, bulk density 0.05g/cm3, porosity 96.5%
Carbon - Vitreous, rod, 100mm, diameter 5.0mm, glassy carbon
Carbon - Vitreous, foam, 300x300mm, thickness 30mm, bulk density 0.05g/cm3, porosity 96.5%
Carbon - Vitreous, rod, 200mm, diameter 1.0mm, glassy carbon
Carbon - Vitreous, foam, 150x150mm, thickness 2.5mm, bulk density 0.05g/cm3, porosity 96.5%
Carbon - Vitreous, foil, 50x50mm, thickness 1.0mm, glassy carbon
Carbon - Vitreous, foil, 10x10mm, thickness 1.0mm, glassy carbon
Carbon - Vitreous, foam, 150x150mm, 0.05g.cmué, porosity 96.5%, 24 pores/cm
Carbon - Vitreous, rod, 100mm, diameter 7.0mm, glassy carbon
Carbon - Vitreous, rod, 200mm, diameter 7.0mm, glassy carbon
Carbon - Vitreous, foil, 10x10mm, thickness 4.0mm, glassy carbon
Carbon - Vitreous, rod, 200mm, diameter 5.0mm, glassy carbon
Carbon - Vitreous, rod, 100mm, diameter 1.0mm, glassy carbon
Carbon - Vitreous, rod, 50mm, diameter 1.0mm, glassy carbon
Carbon - Vitreous, foil, 100x100mm, thickness 6.0mm, glassy carbon
Carbon - Vitreous, rod, 5mm, diameter 3.0mm, glassy carbon
Carbon - Vitreous, foil, 25x25mm, thickness 0.5mm, glassy carbon
Carbon - Vitreous, rod, 100mm, diameter 3.0mm, glassy carbon
Carbon - Vitreous, foam, 300x300mm, thickness 20mm, bulk density 0.05g/cm3, porosity 96.5%
Carbon - Vitreous, foil, 100x100mm, thickness 1.0mm, glassy carbon
Carbon - Vitreous, foil, 25x25mm, thickness 4.0mm, glassy carbon
Carbon - Vitreous, foil, 50x50mm, thickness 4.0mm, glassy carbon
Sigma-Aldrich
Acetic acid solution, suitable for HPLC
Sigma-Aldrich
Acetic acid, glacial, ≥99.99% trace metals basis
Sigma-Aldrich
Magnesium sulfate, BioReagent, suitable for cell culture, suitable for insect cell culture