Evaluation of the Transfer and Occurrence of Opium Alkaloids in Poppy Seed Teas Using Preconcentrations with µSPEed^® Followed by GC-MS Analysis

Intoxication due to the consumption of poppy seed teas has been reported due to their contamination with opium alkaloids (OAs). In this work, an efficient methodology based on microsolid-phase extraction (µSPEed®) followed by gas chromatography–mass spectrometry (GC-MS) has been optimized to quantify five OAs in poppy seed teas. Nine cartridges (C4, C8, C18, silica, APS, PFAs, PS/DVB-RP, PS/DVB-SCX and PS/DVB-SAX), pH levels, cycles and elution solvents were evaluated. The method was validated and applied to study the transfer of OAs by evaluating water temperatures, infusion times and seed amounts. The highest transfer rates (71% for morphine, 96% for thebaine, and 100% for codeine, noscapine and papaverine) were achieved at 90°C, 5 min, with 4 g. These conditions were used to quantify the OAs in four teas prepared from different seeds. A high amount of morphine (1563 µg/L) was found in one tea, indicating that the seeds had a concentration twice the maximum limit, highlighting the need to warn the population of this dangerous practice

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

Atropine and scopolamine belong to the tropane alkaloid (TA) family of natural toxins. They can contaminate teas and herbal teas and appear in infusions. Therefore, this study focused on analyzing atropine and scopolamine in 33 samples of tea and herbal tea infusions purchased in Spain and Portugal to determine the presence of these compounds in infusions brewed at 97 °C for 5 min. A rapid microextraction technique (µSPEed®) followed by high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS) was used to analyze the selected TAs. The results showed that 64% of the analyzed samples were contaminated by one or both toxins. White and green teas were generally more contaminated than black and other herbal teas. Of the 21 contaminated samples, 15 had concentrations above the maximum limit for liquid herbal infusions (0.2 ng/mL) set by Commission Regulation (EU) 2021/1408. In addition, the effects of heating conditions (time and temperature) on atropine and scopolamine standards and naturally contaminated samples of white, green, and black teas were evaluated. The results showed that at the concentrations studied (0.2 and 4 ng/mL), there was no degradation in the standard solutions. Brewing with boiling water (decoction) for 5 and 10 min allowed for higher extraction of TAs from dry tea to infusion water

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

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