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The undemanding LC-MS/MS method was developed for the synchronized analysis of atropine and scopolamine in maize crop. The dSPE was carried out with 1% acetic acid in acetonitrile/water and a mixture of magnesium sulphate, sodium chloride and sodium citrate. The analytes were separated on a Zorbax XDB C18 column using methanol/water as the mobile phase in gradient mode. The detection was done using a tandem masss spectrometry (MS/MS) in the positive ESI. The tropane alkaloids exhibited excellent linearity in the range of 2-20 µg/kg with the LOQ of 5 µg/kg for maize. The extraction recoveries of atropine and scopolamine were 65.7 and 85.5% with the intraday RSDr 10.25 and 4.29%, respectively. The validated method was appled to real maze samples. One sample contained 18.8 µg/kg of atropine and 6.3 µg/kg of scopolamine.

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