Abstract
A new, rapid and sensitive multiresidue method is reported for the simultaneous determination of tropane alkaloids (tropine, atropine, scopolamine, homatropine, anisodamine) and glycoalkaloids (α-solanine, α-chaconine) in grains and seeds (wheat, rye, maize, soybean, linseed). Dispersive solid phase extraction (DSPE) was performed with 0.5% formic acid in acetonitrile/water and a mixture of magnesium sulphate, sodium chloride and sodium citrate. For a fast and effective clean-up procedure for oily matrices such as soybean and linseed, matrix solid phase dispersion (MSPD) C18 material was used to remove co-extracted non-polar components. No clean-up was necessary for less oily matrices following extraction. The analytes were separated by isocratic HPLC on a Chirobiotic V column and detected using a triple quadrupole mass spectrometer with electrospray ionization (ESI). All analytes were monitored in the positive ion mode. The method performance is presented in terms of linearity in the range 5–80 ng/g (r 2 = 0.998), specifity, selectivity, accuracy (recoveries from 61–111%), precision (CV < 5%) and ruggedness. The limits of quantitation (LOQ) were in the range 2.2–4.9 ng/g.