Pereira Joana R P, Rocha Daniela C, Neng Nuno R, Maurício Paulo, Torres M Edite, Ahmad Samir M, Quintas Alexandre
Laboratório de Ciências Forenses e Psicológicas Egas Moniz, Molecular Pathology and Forensic Biochemistry Laboratory, Egas Moniz Center for Interdisciplinary Research, Egas Moniz School of Health and Science, Quinta da Granja, 2829-511 Almada, Portugal.
Centro de Química Estrutural, Institute of Molecular Sciences, Departamento de Química e Bioquímica, Faculdade de Ciências, Universidade de Lisboa, Campo Grande, 1749-016 Lisboa, Portugal.
Molecules. 2024 Dec 27;30(1):68. doi: 10.3390/molecules30010068.
The present work reports the development, optimization, and validation, of a methodology to determine lidocaine, procaine, tetracaine, and benzocaine in urine matrices. Two extractive preconcentration techniques, solid-phase microextraction (SPME) LC Tips and bar adsorptive microextraction (BAμE), were studied and applied to the four target anesthetics, followed by gas chromatography-mass spectrometry (GC-MS) analysis. Several parameters that could affect microextraction and back-extraction were optimized using two different designs of experiments (Box-Behnken and full-factorial) to maximize extraction efficiency from aqueous media. Under optimized experimental conditions, the BAμE technique showed better performance than SPME LC Tips and was chosen for validation assays and urine sample analysis. In blank urine, the BAµE/GC-MS methodology revealed suitable sensitivity (LOD between 2 and 18 ng/mL), good linearity ( ≥ 0.9945) between 0.5 and 30.0 µg/mL and recovery yields of 30.3-97.9%. Good precision (%RSD ≤ 8.8%) and accuracy (bias % between -15.9 and 15.0%) values were achieved. The developed methodology was successfully applied to the target anesthetics analysis of volunteers' urine matrices and proved to be an environmentally friendly alternative to monitor trace levels of local anesthetics in complex matrices compared to other extraction techniques.
本研究报告了一种用于测定尿液基质中利多卡因、普鲁卡因、丁卡因和苯佐卡因的方法的开发、优化及验证。研究了两种萃取预浓缩技术，即固相微萃取（SPME）LC 小柱和棒状吸附微萃取（BAμE），并将其应用于四种目标麻醉剂，随后进行气相色谱 - 质谱（GC - MS）分析。使用两种不同的实验设计（Box - Behnken 和全因子设计）对可能影响微萃取和反萃取的几个参数进行了优化，以最大限度地提高从水性介质中的萃取效率。在优化的实验条件下，BAμE 技术表现优于 SPME LC 小柱，并被选用于验证试验和尿液样本分析。在空白尿液中，BAµE/GC - MS 方法显示出合适的灵敏度（检测限在 2 至 18 ng/mL 之间），在 0.5 至 30.0 µg/mL 之间具有良好的线性（≥0.9945），回收率为 30.3 - 97.9%。实现了良好的精密度（%RSD≤8.8%）和准确度（偏差百分比在 - 15.9 至 15.0%之间）。所开发的方法成功应用于志愿者尿液基质中目标麻醉剂的分析，并且与其他萃取技术相比，被证明是一种监测复杂基质中局部麻醉剂痕量水平的环境友好型替代方法。
