Departamento de Tecnología Química y Ambiental, E.S.C.E.T, Universidad Rey Juan Carlos, C/Tulipán s/n, Móstoles, 28933 Madrid, Spain.
Toxins (Basel). 2022 Mar 17;14(3):218. 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.
在这项工作中，合成了六方介孔硅（HMS）和圣巴巴拉无定形-15（SBA-15）介孔硅，并将磺酸基团功能化。这些材料（HMS-SO3−和 SBA-15-SO3−）被评估为用于样品提取净化的强阳离子交换吸附剂，采用固相萃取（SPE）和分散固相萃取，用于测定商业烹饪香草中的阿托品（At）和东莨菪碱（Sc）。在优化条件下，用酸化水（pH 1.0）对 0.25 g 样品进行固液萃取，使用 75 mg HMS-SO3−进行 SPE 作为净化阶段，可获得较高的 At 和 Sc 回收率，然后采用 HPLC-MS/MS 进行测定。该方法在百里香样品中得到验证，回收率在 70-92%范围内，具有良好的线性（R2>0.999），适当的精密度（RSD≤14%）和较低的检测限（MDL 0.8-2.2 µg/kg 和 MQL 2.6-7.2 µg/kg 用于两种分析物）。对 16 种芳香草本植物样品（干百里香、罗勒和香菜叶）进行分析，发现 14 种样品中含有 At，其浓度范围为 5-42 µg/kg，而 16 种研究样品中有 3 种含有 Sc（浓度范围为 5-34 µg/kg）。一些分析样品中发现的 At 和 Sc 含量证实了在烹饪香草中设定 At 和 Sc 最大限量的重要性。
