In this work, the thermal degradation of tropane and opium alkaloids was studied in samples of breadsticks prepared with corn flour, contaminated with seeds of Datura stramonium, and containing seeds of Papaver somniferum L. A total of seven different samples were prepared and eight alkaloids were studied, three tropane (atropine, scopolamine, and anisodamine) and five opium (morphine, codeine, thebaine, papaverine, and noscapine) alkaloids. For this purpose, a fast, easy and efficient method based on solid-liquid extraction (SLE) prior to the analysis by high-performance liquid chromatography with a diode array detector (HPLC-DAD) was developed and validated. Thermal degradation studies showed a decrease in the TAs and OAs content under baking (180 °C for 20 min) that was between 7–65% for atropine, depending on the preparation conditions used, between 35–49% for scopolamine and anisodamine, up to 100% for morphine and codeine and between 14–58% for thebaine, papaverine, and noscapine. Results also evidenced that degradation of morphine and codeine was higher when the seeds were added as topping to the breadsticks.

The exponential number of food alerts about concerning levels of some plant-alkaloids, such as pyrrolizidine, tropane and opium alkaloids, have stressed the need to monitor their occurrence in foods to avoid toxic health effects derived from their intake. Therefore, analytical strategies to simultaneously monitor the occurrence of these alkaloids should be developed to ensure food safety an comply with regulations. Accordingly, this work proposes an efficient multicomponent analytical strategy for the simultaneous extraction of these alkaloids from commercial bakery products. The analytical method was validated and applied to the analysis of 15 samples, revealing that 100% of them contained at least one of the target alkaloids, in some cases exceeding the maximum limits legislated. Moreover, in two samples the 3 different alkaloid families were detected. These results confirm the importance of simultaneously monitoring these alkaloids in food and highlight also considering some opium alkaloids in current legislation.

Rice husk (RH), a globally abundant agri-food waste, presents a promising renewable silicon source for producing SBA-15 mesoporous silica-based materials. This study aimed to synthesize and bifunctionalize SBA-15 using RH as a silica precursor, incorporating sulfonic and octadecyl groups to create a mixed-mode sorbent, RH-SBA-15-SO₃H-C18, with reversed-phase and cation exchange properties. The material’s structure and properties were characterized using advanced techniques, including X-ray diffraction, infrared spectroscopy, N₂ adsorption–desorption isotherms, nuclear magnetic resonance, and electron microscopy. These analyses confirmed an ordered mesoporous structure with a high specific surface area of 238 m²/g, pore volume of 0.45 cm³/g, pore diameter of 32 Å, and uniform pore distribution, highlighting its exceptional textural qualities. This sorbent was effectively utilized in solid-phase extraction to purify 29 alkaloids from three families—tropane, pyrrolizidine, and opium—followed by an analysis using ultra-high performance liquid chromatography coupled to ion-trap tandem mass spectrometry. The developed analytical method was validated and applied to gluten-free bread samples, revealing tropane and opium alkaloids, some at concentrations exceeding regulatory limits. These findings demonstrate that RH-derived RH-SBA-15-SO₃H-C18 is a viable, efficient alternative to commercial sorbents for monitoring natural toxins in food, offering a sustainable solution for repurposing agri-food waste while addressing food safety challenges.

In this work, mesoporous silicas with two types of mesoporous structures were synthesized and functionalized with sulfonic acid groups: MCM-41-SO₃H (honeycomb-like hexagonal structure) and MSU-2-SO₃H (three-dimensional porous structure with wormhole pores). The synthesized materials were characterized by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, nitrogen adsorption–desorption, Fourier-transform infrared spectroscopy, ²⁹Si solid-state nuclear magnetic resonance spectroscopy, and elemental analysis. The obtained functionalized materials were evaluated as sorbents for strong cation-exchange solid-phase extraction (SPE) to determine their efficiency in the adsorption and desorption of tropane alkaloids (atropine and scopolamine). The loading solvents, loading volume, analyte concentration, and elution volume were studied, using 50 mg of both materials. Analyses were carried out by ultra-high performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry. The synthesized MCM-41-SO₃H material presented the highest recovery efficiency and has proven to be a promising sorbent for strong cation-exchange SPE of atropine and scopolamine in aqueous media. The high degree of functionalization of MCM-41-SO₃H and the high accessibility of the sulfonic groups for the target analytes, due to the regularity and uniformity of their pores, maximize the contact between the alkaloids and the sorbent, favoring efficient adsorption.

This review examines recent advances in the enantiomeric separation of tropane alkaloids (TAs), focusing on atropine, a racemic mixture of (+)- and (−)-hyoscyamine whose enantiomers differ significantly in pharmacological activity, with (−)-hyoscyamine being the more potent antimuscarinic agent. Enantiomeric purity and racemisation control are therefore essential in pharmaceutical formulations, biological samples, and food, where TAs are regulated contaminants due to their toxicological effects. The review covers analytical strategies reported from 2010 to 2026, with emphasis on high-performance liquid chromatography (HPLC), often coupled with tandem mass spectrometry (MS/MS) to improve sensitivity and selectivity. Polysaccharide-based chiral stationary phases operated in normal-phase or polar organic modes, usually with amine additives, represent the most widely employed approach. Protein-, cyclodextrin-, and antibiotic-based chiral selectors have also demonstrated successful enantiomeric resolution. Sample preparation is particularly challenging for food matrices, requiring efficient extraction and clean-up while preventing enantiomeric racemisation. Published strategies include solid-phase extraction (SPE), matrix solid-phase dispersion (MSPD), and QuEChERS protocols. Despite significant analytical advances, chiral analysis of TAs in foods remains underexplored. Recent studies have reported (−)-hyoscyamine concentrations exceeding regulatory limits in herbal infusions, underscoring the need for further research to support European Food Safety Authority (EFSA) recommendations and improve consumer risk assessment.