Mesostructured Silicas as Cation-Exchange Sorbents in Packed or Dispersive Solid Phase Extraction for the Determination of Tropane Alkaloids in Culinary Aromatics Herbs by HPLC-MS/MS

• Published in: Toxins Vol. 14; no. 3; p. 218
• Main Authors: González-Gómez, Lorena, Gañán, Judith, Morante-Zarcero, Sonia, Pérez-Quintanilla, Damián, Sierra, Isabel
• Format: Journal Article
• Language: English
• Published: Switzerland MDPI AG 17.03.2022; MDPI
• Subjects: Acidification; Analytical chemistry; Aromatic compounds; Atropine; Cation exchange; Cation exchanging; Cations; Cereals; Chromatography, High Pressure Liquid - methods; culinary aromatic herbs; Dispersion; dispersive solid-phase extraction; Food contamination & poisoning; Food products; Herbs; High-performance liquid chromatography; Liquid chromatography; mesostructured silicas; Morphology; Particle size; Pore size; Scopolamine; Seeds; Silica; Silicon Dioxide; Solid Phase Extraction - methods; Solid phases; solid-phase extraction; Solvents; Sorbents; strong cation exchange; Sulfonic acid; Sulfur trioxide; Tandem Mass Spectrometry - methods; Thyme; Tropane alkaloids; Tropanes; tropane alkaloids; dispersive solid-phase extraction; mesostructured silicas; culinary aromatic herbs; strong cation exchange; solid-phase extraction
• ISSN: 2072-6651; 2072-6651
• DOI: 10.3390/toxins14030218

In this work, Hexagonal Mesoporous Silica (HMS) and Santa Barbara Amorphous-15 (SBA-15) mesostructured silicas were synthesized and functionalized with sulfonic acid groups. The materials (HMS-SO3− and SBA-15-SO3−) were evaluated as strong cation exchange sorbents for sample extract clean-up, by solid phase extraction (SPE) and dispersive solid phase extraction, to determine atropine (At) and scopolamine (Sc) in commercial culinary aromatic herbs. Under optimized conditions, 0.25 g of sample was subject to solid–liquid extraction with acidified water (pH 1.0), and good recovery percentages were achieved for At and Sc using 75 mg of HMS-SO3− in SPE as the clean-up stage, prior to their determination by HPLC-MS/MS. The proposed method was validated in a thyme sample showing recoveries in the range of 70–92%, good linearity (R2 > 0.999), adequate precision (RSD ≤ 14%) and low limits (MDL 0.8–2.2 µg/kg and MQL 2.6–7.2 µg/kg for both analytes). Sixteen aromatic herbs samples (dried thyme, basil and coriander leaves) were analysed and At was found in fourteen samples over an interval of <5–42 μg/kg, whereas Sc was found in three of the sixteen samples studied (between <5–34 μg/kg). The amount of At and Sc found in some analysed samples confirms the importance of setting maximum levels of At and Sc in culinary aromatic herbs.