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.
JANDRIC, Z., MOHAMMAD, R., ŠVARC-GAJIĆ, J., MAESTRONI, B., SASANYA, J., RADENKO, Đ., CANNAVAN, A.: Development of a liquid chromatography-tandem mass spectrometric method for the simultaneous determination of tropane alkaloids and glycoalkaloids in crops, Food additives and contaminants, 28(9), 1205-1219, 2011.
RECOMMENDATIONS COMMISSION RECOMMENDATION (EU) 2015/976 of 19 June 2015 on the monitoring of the presence of tropane alkaloids in food.
CIRLINI, M., DEMUTH, T.M., BIANCARDI, A., RYCHLIK, M., DALL’ASTA, C., BRUNI, R.: Are tropane alkaloids present in organic foods? Detection of scopolamine and atropine in organic buckwheat (Fagopyron esculentum L.) products by UHPLC– MS/MS, Food Chemistry 239, 141–147, 2018.
SANTE/11813/2017: Method validation and quality control procedures for pesticide residues analysis in food and feed.
ZHENG, W., YOO, K.H., MINCHOI, J., PARK, D., KIM, S., KANG, Y., ABD EL-ATY, A.M., HACIMÜFTÜOĞLU, A., JEONG, J.H., EL-DIN BEKHIT, A., SHIM, J., SHIN, H.: A modified QuEChERS method coupled with liquid chromatography-tandem mass spectrometry for the simultaneous detection and quantification of scopolamine, L- hyoscyamine, and sparteine residues in animal-derived food products, Journal of Advanced Research, 2018. https://doi.org/10.1016/j.jare.2018.09.004
JAKABOVÁ, S., VINCZE, L., FARKAS, Á., KILÁR, F., BOROS, B., FELINGER, A.: Determination of tropane alkaloids atropine and scopolamine by liquid chromatography-mass spectrometry in plant organs of Datura species. Journal of Chromatography A, 1232, 295–301, 2012.
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CHEN, H., MARÍN-SÁEZ, J., ROMERO-GONZÁLEZ, R., GARRIDO FRENICH, A. (2017). Simultaneous determination of atropine and scopolamine in buckwheat and related products using modified QuEChERS and liquid chromatography tandem mass spectrometry. Food Chemistry, 218, 173–180.