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Determination of atropine and scopolamine in honey using a miniaturized polymer-based solid-phase extraction protocol prior to the analysis by HPLC-MS/MS
Polymer ( IF 4.6 ) Pub Date : 2024-03-13 , DOI: 10.1016/j.polymer.2024.126904
Begoña Fernández-Pintor , Gema Paniagua , Judith Gañán , Sonia Morante-Zarcero , Rosa María Garcinuño , Pilar Fernández , Isabel Sierra

Two homopolymers have been prepared employing methacrylic acid and 4-vynylpiridine as functional monomers (p-MAA, p-4-VP) through an easy and quick precipitation polymerization method for application as sorbents in solid-phase extraction (SPE) to determine atropine and scopolamine in honey. The optimized SPE conditions were as follows: 25 mg of p-MAA, 4 mL of sample loading volume (diluted honey 1:10 with water), 4 mL of elution solvent (methanol/water with 1 % formic acid, 80/20, v/v). The extracts were analyzed by HPLC-MS/MS. The cartridges were reusable for forty cycles demonstrating an environmentally friendly approach. The methodology was validated in terms of linearity, accuracy, precision, selectivity, matrix effect and sensibility, highlighting the absence of matrix effect. The miniaturized polymer-based SPE was successfully applied to fifteen honeys, showing concentrations up to 7.23 ng/g in the most contaminated honey. All quantified honey samples (5 in total) were of multifloral type.

中文翻译:

在 HPLC-MS/MS 分析之前,使用基于小型聚合物的固相萃取方案测定蜂蜜中的阿托品和东莨菪碱

采用甲基丙烯酸和 4-乙烯基吡啶作为功能单体(p-MAA、p-4-VP),通过简单快速的沉淀聚合方法制备了两种均聚物,用作固相萃取(SPE)中的吸附剂来测定阿托品和蜂蜜中的东莨菪碱。优化的 SPE 条件如下:25 mg p-MAA,4 mL 上样体积(蜂蜜按 1:10 与水稀释),4 mL 洗脱溶剂(甲醇/水,含 1% 甲酸,80/20, v/v)。通过 HPLC-MS/MS 分析提取物。该墨盒可重复使用四十次,展示了一种环保方法。该方法在线性、准确度、精密度、选择性、基质效应和敏感性方面进行了验证,强调不存在基质效应。基于小型聚合物的 SPE 成功应用于 15 种蜂蜜,污染最严重的蜂蜜中浓度高达 7.23 ng/g。所有定量蜂蜜样品(共 5 个)均为多花型。
更新日期:2024-03-13
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