REQUIMTE, Faculty of Pharmacy, University of Porto, Rua Jorge Viterbo Ferreira 228, 4050-313 Porto, Portugal.
J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Jul 1;930:75-81. doi: 10.1016/j.jchromb.2013.04.032. Epub 2013 Apr 29.
Paracetamol is among the most worldwide consumed pharmaceuticals. Although its occurrence in the environment is well documented, data about the presence of its metabolites and transformation products is very scarce. The present work describes the development of an analytical method for the simultaneous determination of paracetamol, its principal metabolite (paracetamol-glucuronide) and its main transformation product (p-aminophenol) based on solid phase extraction (SPE) and high performance liquid chromatography coupled to diode array detection (HPLC-DAD). The method was applied to analysis of river waters, showing to be suitable to be used in routine analysis. Different SPE sorbents were compared and the use of two Oasis WAX cartridges in tandem proved to be the most adequate approach for sample clean up and pre-concentration. Under optimized conditions, limits of detection in the range 40-67ng/L were obtained, as well as mean recoveries between 60 and 110% with relative standard deviations (RSD) below 6%. Finally, the developed SPE-HPLC/DAD method was successfully applied to the analysis of the selected compounds in samples from seven rivers located in the north of Portugal. Nevertheless all the compounds were detected, it was the first time that paracetamol-glucuronide was found in river water at concentrations up to 3.57μg/L.
对乙酰氨基酚是全球应用最广泛的药物之一。尽管其在环境中的存在已有大量文献记载，但有关其代谢物和转化产物存在的数据却非常有限。本工作描述了一种基于固相萃取（SPE）和高效液相色谱-二极管阵列检测（HPLC-DAD）联用技术的同时测定对乙酰氨基酚、其主要代谢物（对乙酰氨基酚葡萄糖醛酸苷）和主要转化产物（对氨基酚）的分析方法的建立。该方法应用于河水的分析，结果表明该方法适用于常规分析。比较了不同的 SPE 吸附剂，串联使用两个 Oasis WAX 小柱被证明是样品净化和预浓缩的最适宜方法。在优化条件下，检测限在 40-67ng/L 范围内，平均回收率在 60-110%之间，相对标准偏差（RSD）低于 6%。最后，所建立的 SPE-HPLC/DAD 方法成功地应用于葡萄牙北部 7 条河流中选定化合物的分析。尽管所有化合物都被检测到，但这是首次在河水中发现对乙酰氨基酚葡萄糖醛酸苷，其浓度高达 3.57μg/L。
