engleski

OPTIMIZATION OF SAMPLE PREPARATION METHOD FOR DETERMINATION ATROPINE AND SCOPOLAMINE BY LIQUID CHROMATOGRAPHY TANDEM MASS SPECTROMETRY IN CEREALS AND CEREAL BASED FOODS

Plants grow up surrounded by various threats from environment such as microorganisms, insects and predators. In order to existence, many of them produce a wide variety of toxic compounds commonly called secondary metabolites to discourage predators, as well as to dominance competitive organisms in their surroundings. Humans can be exposed to these toxins by consumption of contaminated food like cereals or cereal based products and some of them can be very harmful to human health. The most sensitive groups are infants and young children because of lower body weight toxic substances reach higher concentrations. Atropine and Scopolamine belong to group of natural plant toxins called Tropane alkaloids which occur mainly in Solanaceae plants (including mandrake, henbane, deadly nightshade, datura) but also in numerous other plant families such as Erythroxylaceae and Brassicaceae. These plants are weeds of courtyards and wild habitats but also of cultivated fields like cereal. Coexisting of cereals and plants that produce tropane alkaloids can lead to contamination of cereal grains during harvest. So far, processed cereal-based foods and baby foods for infants and young children are the only products with established maximum permitted levels of atropine and scopolamine, 1.0 μg/kg each. In this work the focus was on simplifying the extraction and clean-up procedures for determination atropine and scopolamine by liquid chromatography tandem mass spectrometry (LC-MS/MS). Investigated matrices were buckwheat, wheat, barley, maize and processed cereal-based foods for infants and young children. Mixtures of acetonitrile, water and formic acid in different percentage and solvent volumes were explored for the extraction of the target compounds. Further optimization of extraction/purification procedure was included two ways of sample treatment. Solid‑phase extraction with various adsorbents like HLB, C18, SCX and modified QuEChERS approach based on the use of different salt formulation (magnesium sulphate, sodium chloride and sodium citrate) were tested. Quantification was performed by using isotope labelled internal standards of atropine and scopolamine added to the samples before the extraction. The optimized sample preparation based on QuEChERS approach provided recoveries from 70 to 120% with intra-day precisions ≤ 15% and inter-day precisions ≤ 22%. Limits of quantification were 0.40 μg/kg in baby food and 1.0 μg/kg in cereals for atropine and scopolamine respectively.

atropine, scopolamine, sample preparation, cereals, baby food

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