Koziarska Marta, Strzebońska Magdalena, Szalińska Ewa
Department of Environmental Protection, Faculty of Geology, Geophysics and Environmental Protection, AGH University of Kraków, Al. Mickiewicza 30, Kraków, 30-059, Poland.
Sci Rep. 2025 Aug 22;15(1):30902. doi: 10.1038/s41598-025-15614-4.
In response to the growing concerns regarding pharmaceutical contamination of our aquatic systems, targeted actions are being implemented to align with the recommendations of the European Commission. However, a challenge lies in finding effective, accurate, and green chemistry-compliant methods for analyzing these compounds in complex matrices. This study introduces a highly sensitive and sustainable ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method for simultaneously determining carbamazepine, caffeine, and ibuprofen in water and wastewater. This method exhibits impressive advantages: exceptional sensitivity, high selectivity, and an economical sample preparation strategy resulting from the absence of an evaporation step after solid-phase extraction (SPE), as well as a short analysis time (10 min). Following the International Council for Harmonization (ICH) guidelines Q2(R2), the developed and validated method proved to be specific, linear (correlation coefficients ≥ 0.999), precise (RSD < 5.0%), and accurate (recovery rates ranging from 77 to 160%). The limits of detection were 300 ng/L for caffeine, 200 ng/L for ibuprofen, and 100 ng/L for carbamazepine, respectively. The limits of quantification (LOQs) were 1000 ng/L for caffeine, 600 ng/L for ibuprofen, and 300 ng/L for carbamazepine. The advanced UHPLC-MS/MS method presented in this article constitutes a green and blue analytical technique for the precise detection and quantification of trace levels of pharmaceutical contaminants in aquatic environments. This method has been validated and exemplified using a case study from the Kraków area, highlighting its high efficiency, reliability, and minimal environmental impact. This approach aligns with the concept of sustainable analytics, combining ecological aspects with high-quality results. This study is therefore crucial for the effective monitoring of pollutants, the assessment of environmental and health risks, and ensuring water quality.
针对人们对水生系统中药物污染日益增长的担忧，正在采取针对性行动以符合欧盟委员会的建议。然而，挑战在于找到有效、准确且符合绿色化学的方法来分析复杂基质中的这些化合物。本研究介绍了一种高灵敏度且可持续的超高效液相色谱 - 串联质谱法（UHPLC - MS/MS），用于同时测定水和废水中的卡马西平、咖啡因和布洛芬。该方法具有显著优势：灵敏度极高、选择性高，且由于固相萃取（SPE）后无需蒸发步骤，具有经济的样品制备策略，同时分析时间短（10分钟）。遵循国际协调会议（ICH）指南Q2(R2)，所开发并验证的方法具有特异性、线性（相关系数≥0.999）、精密度高（RSD＜5.0%）且准确度高（回收率在77%至160%之间）。咖啡因的检测限为300 ng/L，布洛芬为200 ng/L，卡马西平为100 ng/L。定量限（LOQ）方面，咖啡因为1000 ng/L，布洛芬为600 ng/L，卡马西平为300 ng/L。本文介绍的先进UHPLC - MS/MS方法构成了一种绿色和蓝色分析技术，用于精确检测和定量水生环境中痕量药物污染物。该方法已通过克拉科夫地区的案例研究进行了验证和举例说明，突出了其高效率、可靠性和最小的环境影响。这种方法符合可持续分析的概念，将生态方面与高质量结果相结合。因此，本研究对于有效监测污染物、评估环境和健康风险以及确保水质至关重要。
