Improved Analytical Approach for Determination of Tropane Alkaloids in Leafy Vegetables Based on µ-QuEChERS Combined with HPLC-MS/MS

Abstract

This work presents an optimized methodology based on the miniaturization of the original QuEChERS (μ-QuEChERS) followed by liquid chromatography coupled to mass spectrometry (HPLC-MS/MS) for the determination of tropane alkaloids (TAs), atropine, and scopolamine in leafy vegetable samples. The analytical methodology was successfully validated, demonstrating quantitation limits (MQL) ≤2.3 ng/g, good accuracy, and precision, with recoveries between 90–100% and RSD ≤ 13% for both analytes. The method was applied to the analysis of TA-producing plants (Brugmansia versicolor, Solandra maxima, and Convolvulus arvensis). High concentrations of scopolamine were found in flowers (1771 mg/kg) and leaves (297 mg/kg) of B. versicolor. The highest concentration of atropine was found in flowers of S. maxima (10.4 mg/kg). Commercial mixed leafy vegetables contaminated with B. versicolor and S. maxima were analysed to verify the efficacy of the method, showing recoveries between 82 and 110% for both analytes. Finally, the method was applied to the analysis of eighteen samples of leafy vegetables, finding atropine in three samples of mixed leafy vegetables, with concentrations of 2.7, 3.2, and 3.4 ng/g, and in nine samples with concentrations ≤MQL. In turn, scopolamine was only found in a sample of chopped Swiss chard with a concentration ≤MQL.

The Bright and Dark Sides of Herbal Infusions: Assessment of Antioxidant Capacity and Determination of Tropane Alkaloids

“…Most of the studies determine the presence of atropine and scopolamine, or together with pyrrolizidine alkaloids. Moreover, other recently developed methods focus on the determination of TAs in cereals [31,32,38] and leafy vegetables [39].…”

Development of a Novel LC-MS/MS Multi-Method for the Determination of Regulated and Emerging Food Contaminants Including Tenuazonic Acid, a Chromatographically Challenging Alternaria Toxin

“…Thereafter, QuEChERS was tested and introduced as the sample preparation protocol for other LC-MS/MS methods as well [ 16 , 17 , 18 ]. Recently published papers and standards describe QuEChERS employed in the analysis of mycotoxins, ergot alkaloid or Alternaria toxin [ 19 , 20 , 21 , 22 , 23 ]. Although the extraction of Alternaria toxins from food is preferably done with a methanolic medium, QuEChERS can successfully be applied for their extraction in various food samples as well [ 22 ].…”

Evaluation of Tropane Alkaloids in Teas and Herbal Infusions: Effect of Brewing Time and Temperature on Atropine and Scopolamine Content

“…The population is exposed to these natural toxins through food, usually of plant origin, although some studies have reported the transfer of TAs to animal foods, such as honey and milk [ 3 , 8 ]. Cereals and pseudocereals are the most contaminated foods [ 11 , 12 , 13 , 14 , 15 ], followed by teas, herbal teas [ 16 , 17 , 18 , 19 , 20 ], spices [ 21 ], honey [ 22 , 23 ], and vegetables [ 24 , 25 ]. Furthermore, over the past few years, the European Rapid Alert System for the Food and Feed (RASFF) portal has reported numerous alerts on different foodstuffs contaminated by TA-producing plants, such as Atropa belladonna , Datura stramonium , Mandragora , Hyoscyamus niger , and Solanum nigrum [ 3 , 26 ].…”

“…Awareness of this potential contamination and good manufacturing practices will reduce the risk of mixing toxic and non-toxic plants [ 3 ]. However, recently, another route of contamination was proposed [ 25 ]. This route involves horizontal transfer through the soil, which has already been proposed for other families of alkaloids, such as pyrrolizidine alkaloids (PAs) [ 27 , 28 ].…”