通过超高效液相色谱-紫外检测法分析不同吸附剂材料用于固相萃取人尿中选定药物的比较。
Comparison of different sorbent materials for solid-phase extraction of selected drugs in human urine analyzed by UHPLC-UV.
作者信息
Magiera Sylwia, Hejniak Judyta, Baranowski Jacek
机构信息
Department of Inorganic, Analytical Chemistry and Electrochemistry, Silesian University of Technology, 7 M. Strzody Str., 44-100 Gliwice, Poland.
Department of Inorganic, Analytical Chemistry and Electrochemistry, Silesian University of Technology, 7 M. Strzody Str., 44-100 Gliwice, Poland.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 May 1;958:22-8. doi: 10.1016/j.jchromb.2014.03.014. Epub 2014 Mar 15.
A procedure based on solid-phase extraction (SPE) followed by ultra-high-performance liquid chromatography (UHPLC) with UV detection has been developed for the analysis of multiple drugs in human urine. The compounds evaluated were aliskiren, prasugrel, rivaroxaban, prednisolone, propranolol, ketoprofen, nifedipine, naproxen, terbinafine, ibuprofen, diclofenac, sildenafil and acenocoumarol. Seventeen different solid phase extraction (SPE) cartridges were tested to evaluate their applicability for the isolation of drugs from human urine. Comparison were recovery of different drugs and reproducibility. The samples were analyzed by UHPLC using a Poroshell 120 EC-C18 column and acetonitrile -0.05% TFA in water as the mobile phase under gradient elution conditions. SPE combined with UHPLC-UV allowed the determination of drugs over a linear range of 0.01-30.0μg/mL, with limits of detection at 0.003-0.217μg/mL and precision of 0.8-7.1%. Phenyl (C6H5) sorbent was found to provide the most effective clean-up, removing the greatest amount of interfering substance and simultaneously ensuring analyte recoveries higher than 85.5% with relative standard deviations (RSD) <10%. The method was applied with good accuracy and precision in the determination of drugs in human urine obtained from patients treated with selected drugs.
已开发出一种基于固相萃取（SPE），随后进行超高效液相色谱（UHPLC）并采用紫外检测的方法，用于分析人尿中的多种药物。所评估的化合物有阿利吉仑、普拉格雷、利伐沙班、泼尼松龙、普萘洛尔、酮洛芬、硝苯地平、萘普生、特比萘芬、布洛芬、双氯芬酸、西地那非和醋硝香豆素。测试了17种不同的固相萃取（SPE）小柱，以评估它们从人尿中分离药物的适用性。比较了不同药物的回收率和重现性。采用Poroshell 120 EC-C18色谱柱，以乙腈-0.05%三氟乙酸水溶液为流动相，在梯度洗脱条件下，通过UHPLC对样品进行分析。SPE与UHPLC-UV联用可测定线性范围为0.01 - 30.0μg/mL的药物，检测限为0.003 - 0.217μg/mL，精密度为0.8 - 7.1%。发现苯基（C6H5）吸附剂能提供最有效的净化效果，去除最多的干扰物质，同时确保分析物回收率高于85.5%，相对标准偏差（RSD）<10%。该方法在测定接受选定药物治疗患者的人尿中的药物时，具有良好的准确度和精密度。
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