Semail Nadhiratul-Farihin, Keyon Aemi Syazwani Abdul, Saad Bahruddin, Kamaruzaman Sazlinda, Zain Nur Nadhirah Mohamad, Lim Vuanghao, Miskam Mazidatulakmam, Abdullah Wan Nazwanie Wan, Raoov Muggundha, Yahaya Noorfatimah
Department of Toxicology, Advanced Medical and Dental Institute (AMDI), Universiti Sains Malaysia, Bertam, 13200 Kepala Batas, Penang, Malaysia.
Department of Chemistry, Faculty of Science and Centre for Sustainable Nanomaterials, Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM, Johor Bahru, Johor, Malaysia.
J Chromatogr A. 2022 Dec 6;1685:463616. doi: 10.1016/j.chroma.2022.463616. Epub 2022 Oct 30.
Realising the need to devise a simple, sensitive, and reliable detection method, this study investigated the development of a dual-stacking transient isotachophoresis (t-ITP) and sweeping in micellar electrokinetic chromatography with diode array detector (t-ITP/sweeping-MEKC-DAD) for the determination of selected non-steroidal anti-inflammatory drugs (NSAIDs); ketoprofen, diclofenac and naproxen from aqueous matrices. Prior to the system setup, various parameters were optimised to assess the potential use of the t-ITP paired with the sweeping stacking technique in micellar background electrolyte for dual preconcentration and separation of trace amounts of NSAIDs. Once the optimum conditions have been established, the method performance was validated and applied to 17 environmental water samples. Based on the results, the combined t-ITP and sweeping approach significantly improved the stacking and separation sensitivity. A large volume of samples could also be introduced and subsequently separated by MEKC with greater focusing effects due to the sweeping. Under optimised conditions, the developed method exhibited excellent linearity at a high range (0.1-500 ng/mL, r ≥ 0.998), low limits of detection (LODs) of 0.01-0.07 ng/mL, and a remarkable relative recovery (RR) of 99.6-101.9% with a relative standard deviation (RSD) of 1.4-8.6% (n = 9). Ultimately, the sensitivity enhancement factors improved up to 666-fold using the optimised method. Therefore, the proposed method presents a simplified yet effective and suitable for the determination of NSAIDs from aqueous matrices.
认识到需要设计一种简单、灵敏且可靠的检测方法,本研究探索了一种用于测定选定非甾体抗炎药(NSAIDs)的双堆积瞬态等速电泳(t-ITP)和胶束电动色谱中的扫集联用二极管阵列检测器(t-ITP/扫集-MEKC-DAD)方法;从水性基质中检测酮洛芬、双氯芬酸和萘普生。在建立该系统之前,对各种参数进行了优化,以评估t-ITP与扫集堆积技术在胶束背景电解质中对痕量NSAIDs进行双重预浓缩和分离的潜在用途。一旦确定了最佳条件,便对该方法的性能进行了验证,并将其应用于17个环境水样。基于结果,t-ITP和扫集联用方法显著提高了堆积和分离灵敏度。由于扫集作用,还可以引入大量样品,随后通过MEKC进行分离,并具有更大的聚焦效果。在优化条件下,所开发的方法在高浓度范围(0.1-500 ng/mL,r≥0.998)内表现出优异的线性、0.01-0.07 ng/mL的低检测限(LOD)、99.6-101.9%的显著相对回收率(RR)以及1.4-8.6%的相对标准偏差(RSD)(n = 9)。最终,使用优化后的方法,灵敏度增强因子提高到了666倍。因此,所提出的方法提供了一种简化但有效且适用于从水性基质中测定NSAIDs的方法。