Next Article in Journal
Limited Microcystin, Anatoxin and Cylindrospermopsin Production by Cyanobacteria from Microbial Mats in Cold Deserts
Next Article in Special Issue
Critical Comparison of Analytical Performances of Two Immunoassay Methods for Rapid Detection of Aflatoxin M1 in Milk
Previous Article in Journal
Expansion and Conservation of Biosynthetic Gene Clusters in Pathogenic Pyrenophora spp.
Previous Article in Special Issue
Rapid, Sensitive, and Accurate Point-of-Care Detection of Lethal Amatoxins in Urine
Open AccessArticle

Development and Validation of a UHPLC-ESI-MS/MS Method for Quantification of Oleandrin and Other Cardiac Glycosides and Evaluation of Their Levels in Herbs and Spices from the Belgian Market

1
Unit Toxins, Organic Contaminants and Additives, Sciensano, 1050 Brussels, Belgium
2
Wageningen Food Safety Research, Wageningen University and Research, 6708 WB Wageningen, The Netherlands
*
Author to whom correspondence should be addressed.
Toxins 2020, 12(4), 243; https://doi.org/10.3390/toxins12040243
Received: 6 March 2020 / Revised: 4 April 2020 / Accepted: 8 April 2020 / Published: 9 April 2020
Cardiac glycosides (CGs) are naturally occurring plant secondary metabolites that can be toxic to humans and animals. The aim of this work was to develop a targeted analytical method utilizing liquid chromatography—tandem mass spectrometry (LC-MS/MS) for quantification of these plant toxins in a herbal-based food and human urine. The method included oleandrin, digoxin, digitoxin, convallatoxin, and ouabain. Samples of culinary herbs were extracted with acetonitrile and cleaned using Oasis® MAX solid-phase extraction (SPE), while samples of urine were diluted with acidified water and purified on Oasis® HLB SPE cartridges. Limits of quantification were in the range of 1.5–15 ng/g for herbs and 0.025–1 ng/mL for urine. The mean recovery of the method complied with the acceptable range of 70–120% for most CGs, and relative standard deviations were at maximum 14% and 19% for repeatability and reproducibility, respectively. Method linearity was good with calculated R² values above 0.997. The expanded measurement uncertainty was estimated to be in the range of 7–37%. The LC-MS/MS method was used to examine 65 samples of culinary herbs and herb and spice mixtures collected in Belgium, from supermarkets and local stores. The samples were found to be free from the analyzed CGs. View Full-Text
Keywords: oleandrin; LC-MS/MS; plant toxins; validation; herbs; urine oleandrin; LC-MS/MS; plant toxins; validation; herbs; urine
Show Figures

Figure 1

MDPI and ACS Style

Malysheva, S.V.; Mulder, P.P.J.; Masquelier, J. Development and Validation of a UHPLC-ESI-MS/MS Method for Quantification of Oleandrin and Other Cardiac Glycosides and Evaluation of Their Levels in Herbs and Spices from the Belgian Market. Toxins 2020, 12, 243. https://doi.org/10.3390/toxins12040243

AMA Style

Malysheva SV, Mulder PPJ, Masquelier J. Development and Validation of a UHPLC-ESI-MS/MS Method for Quantification of Oleandrin and Other Cardiac Glycosides and Evaluation of Their Levels in Herbs and Spices from the Belgian Market. Toxins. 2020; 12(4):243. https://doi.org/10.3390/toxins12040243

Chicago/Turabian Style

Malysheva, Svetlana V.; Mulder, Patrick P.J.; Masquelier, Julien. 2020. "Development and Validation of a UHPLC-ESI-MS/MS Method for Quantification of Oleandrin and Other Cardiac Glycosides and Evaluation of Their Levels in Herbs and Spices from the Belgian Market" Toxins 12, no. 4: 243. https://doi.org/10.3390/toxins12040243

Find Other Styles
Note that from the first issue of 2016, MDPI journals use article numbers instead of page numbers. See further details here.

Article Access Map by Country/Region

1
Search more from Scilit
 
Search
Back to TopTop