Laboratory for Forensic Chemistry, Department of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University in Kraków, Gronostajowa St. 2, 30-387, Kraków, Poland; Jagiellonian University in Kraków, Doctoral School of Exact and Natural Sciences, Faculty of Chemistry, Poland.
Laboratory for Forensic Chemistry, Department of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University in Kraków, Gronostajowa St. 2, 30-387, Kraków, Poland.
Anal Chim Acta. 2024 Aug 8;1316:342874. doi: 10.1016/j.aca.2024.342874. Epub 2024 Jun 14.
The rapid development of micro-solid phase extraction (μ-SPE) procedures with new sorption materials, in particular, based on using natural materials, is currently reported. The production of these sorbents and the entire extraction procedure should support the implementation of Green Analytical Chemistry (GAC) principles. Promising materials are sorbents based on paper, which can be relatively easily modified, among others: by covering it with a polymer membrane. In this work, the practical application of paper-supported polystyrene used in the analysis of urine samples containing selected date-rape drugs (DRD) substances, and evaluation of the entire procedure using GAC metrics is presented.
The paper-supported polystyrene membranes were successfully fabricated and characterized. The successful polystyrene coating on the paper was confirmed through ATR-FTIR measurements, ensuring even coverage. The μ-SPE procedure using this material facilitated extraction with a throughput of approximately 120 samples per hour in just a few steps. Throughout the research, a mixture of 100 mM acetic acid:methanol:acetonitrile (70:15:15, v/v/v) was selected as an optimal background electrolyte for capillary electrophoresis - mass spectrometry analysis. Validation results of this method demonstrated its suitability, exhibiting good linearity (R > 0.95), low limits of detection (3.1-15 ng mL), acceptable precision (<15 %), and recovery for all tested analytes. Furthermore, the greenness evaluation conducted with six different metrics: AGREEprep, AGREE, ComplexGAPI, SPMS, hexagonal metric, and WAC indicated the overall eco-friendliness and sustainability of the method, with minor concerns regarding energy consumption.
The use of cellulose paper with polystyrene membranes for μ-SPE provides a versatile and eco-friendly extraction method for detecting DRDs in urine samples. The presented work is an example of the use of GAC metrics in the evaluation of the analytical procedure. The optimized PT-μ-SPE/CE-MS method allows for minimized reagent usage and waste production. Moreover, the method proves to be sustainable and efficient for forensic toxicology analysis.
目前有报道称，新型吸附材料（尤其是基于天然材料）的微固相萃取（μ-SPE）方法发展迅速。这些吸附剂的生产和整个萃取过程都应支持绿色分析化学（GAC）原则的实施。有前途的材料是基于纸张的吸附剂，这些吸附剂相对容易进行修饰，例如：用聚合物膜覆盖。在这项工作中，展示了用于分析尿液样本中选定的强奸药物（DRD）物质的基于纸张的聚苯乙烯的实际应用，并使用 GAC 指标对整个过程进行了评估。
成功制备并表征了基于纸张的聚苯乙烯膜。ATR-FTIR 测量结果证实了纸张上成功的聚苯乙烯涂层，确保了均匀的覆盖。使用这种材料的 μ-SPE 程序可以在短短几个步骤中以大约每小时 120 个样品的通量进行提取。在整个研究过程中，选择 100mM 乙酸：甲醇：乙腈（70:15:15，v/v/v）的混合物作为毛细管电泳-质谱分析的最佳背景电解质。该方法的验证结果表明其适用性良好，表现出良好的线性（R>0.95）、低检测限（3.1-15ngmL）、可接受的精密度（<15%）和所有测试分析物的回收率。此外，使用六种不同指标进行的绿色度评估：AGREEprep、AGREE、ComplexGAPI、SPMS、六边形指标和 WAC 表明该方法具有整体生态友好性和可持续性，仅对能源消耗存在较小的关注。
使用纤维素纸和聚苯乙烯膜的 μ-SPE 为检测尿液样本中的 DRD 提供了一种灵活且环保的萃取方法。所提出的工作是在评估分析程序中使用 GAC 指标的一个示例。经过优化的 PT-μ-SPE/CE-MS 方法可以最大程度地减少试剂的使用和废物的产生。此外，该方法被证明对法医毒理学分析具有可持续性和高效性。
