Departament de Química Analítica i Química Orgànica, Universitat Rovira i Virgili, Campus Sescelades, Marcel·lí Domingo, s/n, 43007 Tarragona, Spain.
J Chromatogr A. 2011 Sep 2;1218(35):5975-80. doi: 10.1016/j.chroma.2010.12.028. Epub 2010 Dec 13.
The present study describes the first fully automated method based on on-line solid-phase extraction (SPE) coupled to hydrophilic interaction chromatography-electrospray-mass spectrometry (HILIC-(ESI)MS) to determine a group of polar drugs that includes illicit drugs (such as cocaine, morphine, codeine and metabolites) and pharmaceuticals in environmental water samples. The SPE was performed using a highly retentive polymeric sorbent. The HILIC separation was optimised and the initial high organic content of the chromatographic mobile phase, was also suitable for the proper on-line elution of the analytes retained in the SPE column and for enhancing the ESI ionisation efficiency. This method allows the loading of samples of up to 250ml of ultrapure water or 10ml of environmental water samples spiked at low ngl(-1) levels of the analytes. The method yields near 100% recoveries for all the analytes. The method was also validated with environmental water samples with linear ranges from 5 to 1000ngl(-1) and limits of detection ≤2ngl(-1) for most of the compounds.
本研究描述了一种完全基于在线固相萃取（SPE）结合亲水相互作用色谱-电喷雾质谱（HILIC-ESI-MS）的方法，用于测定一组极性药物，包括非法药物（如可卡因、吗啡、可待因和代谢物）和环境水样中的药物。SPE 采用高保留聚合物吸附剂进行。HILIC 分离得到优化，色谱流动相的初始高有机含量也适合 SPE 柱中保留的分析物的在线洗脱，并增强 ESI 离子化效率。该方法允许对高达 250ml 超纯水或 10ml 环境水样进行加载，水样中分析物的浓度低至 ngL(-1) 水平。该方法对所有分析物的回收率接近 100%。该方法还通过环境水样进行了验证，线性范围为 5 至 1000ngL(-1)，大多数化合物的检测限≤2ngL(-1)。
