tion of 10 mycotoxins. This procedure was optimised using barley
syrup as representative matrix. With this purpose different solvents
and different Agilent SampliQ EN QuEChERS extraction kits
were tested: (a) 8 mL of H2O + 10 mL of MeCN with 5% formic
acid + non-buffered QuEChERS Extraction packed (4 g MgSO4, 1 g
NaCl); (b) 8 mL of H2O + 10 mL of MeCN with 5% formic acid + buffered
QuEChERS extraction packed (4 g MgSO4, 1 g NaCl, 1 g
sodium citrate, 0.5 g disodium hydrogen citrate sesquihydrate);
(c) 8 mL of 30 mM NaH2PO4 pH 7.1 + 10 mL of MeCN with 5% formic
acid + buffered QuEChERS extraction packed. We also tested
simple solid–liquid extraction by using: (d) 10 mL of MeCN and
(e) 10 mL of MeOH as extraction solvents; however in these cases
dilution of the sample on those less polar media was not possible.
The best results in terms of recovery were obtained with (c), with
no further clean up required; so we selected those conditions for
further experiments.
The procedure is described in detail in Section 2.3. A typical
chromatogram corresponding to a spiked barley syrup sample submitted
to the proposed method is shown in Fig. 1.
3.2. Characterisation of the method
In order to check the suitability of the method for the determination
of mycotoxins in cereal syrups, matrix effect, linear dynamic
ranges, limits of detection (LOD) and quantification (LOQ), precision
and trueness were evaluated using barley syrup as representative
matrix.
3.2.1. Matrix effect, calibration curves and performance characteristics
Table 2 shows the values of the matrix effect at three concentration
levels, which was calculated as 100 [(signal of spiked
extract signal of standard solution)/signal of standard solution].
As can be seen, for FB1, FB2, HT-2, DON and ZEN matrix effect was
tion of 10 mycotoxins. This procedure was optimised using barleysyrup as representative matrix. With this purpose different solventsand different Agilent SampliQ EN QuEChERS extraction kitswere tested: (a) 8 mL of H2O + 10 mL of MeCN with 5% formicacid + non-buffered QuEChERS Extraction packed (4 g MgSO4, 1 gNaCl); (b) 8 mL of H2O + 10 mL of MeCN with 5% formic acid + bufferedQuEChERS extraction packed (4 g MgSO4, 1 g NaCl, 1 gsodium citrate, 0.5 g disodium hydrogen citrate sesquihydrate);(c) 8 mL of 30 mM NaH2PO4 pH 7.1 + 10 mL of MeCN with 5% formicacid + buffered QuEChERS extraction packed. We also testedsimple solid–liquid extraction by using: (d) 10 mL of MeCN and(e) 10 mL of MeOH as extraction solvents; however in these casesdilution of the sample on those less polar media was not possible.The best results in terms of recovery were obtained with (c), withno further clean up required; so we selected those conditions forfurther experiments.The procedure is described in detail in Section 2.3. A typicalchromatogram corresponding to a spiked barley syrup sample submittedto the proposed method is shown in Fig. 1.3.2. Characterisation of the methodIn order to check the suitability of the method for the determinationof mycotoxins in cereal syrups, matrix effect, linear dynamicranges, limits of detection (LOD) and quantification (LOQ), precisionand trueness were evaluated using barley syrup as representativematrix.
3.2.1. Matrix effect, calibration curves and performance characteristics
Table 2 shows the values of the matrix effect at three concentration
levels, which was calculated as 100 [(signal of spiked
extract signal of standard solution)/signal of standard solution].
As can be seen, for FB1, FB2, HT-2, DON and ZEN matrix effect was
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