Ferrer-Aguirre Alejandra, Romero-González Roberto, Vidal J L Martínez, Frenich Antonia Garrido
Group "Analytical Chemistry of Contaminants", Department of Chemistry and Physics (Analytical Chemistry Area), Andalusian Center for the Assessment and Monitoring of Global Change (CAESCG), University of Almería, Agrifood Campus of International Excellence, ceiA3, Carretera de Sacramento s/n, E-04120, Almería, Spain.
Group "Analytical Chemistry of Contaminants", Department of Chemistry and Physics (Analytical Chemistry Area), Andalusian Center for the Assessment and Monitoring of Global Change (CAESCG), University of Almería, Agrifood Campus of International Excellence, ceiA3, Carretera de Sacramento s/n, E-04120, Almería, Spain.
J Chromatogr A. 2016 May 13;1446:27-33. doi: 10.1016/j.chroma.2016.04.009. Epub 2016 Apr 4.
A simple and quick analytical method has been developed for the determination of pharmaceutical compounds in water. An on-line solid-phase extraction (SPE) coupled to liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been optimized to determine 7 contaminants of emerging concern in environmental waters at ngL(-1) levels. This procedure requires minimal sample handling and small sample volume (900μL) with a total running time of 18min. Several SPE parameters were evaluated and optimized in order to achieve a high sample throughput. Therefore sample volume, carryover and reusability of the cartridges were evaluated. Performance characteristics were evaluated and good linearity was obtained (R(2)>0.98). Recoveries were evaluated in spiked samples at three concentrations and the values ranged from 71 to 104%. Intra and inter-day precision was lower than 10 and 13% respectively. Limits of quantification were equal to or lower than 10ngL(-1), except for 1,7-dimethylxanthine (20ngL(-1)) and ibuprofen (50ngL(-1)). The method was applied to 20 environmental water samples, and ibuprofen was the compound most widely detected at concentrations up to 42.06μgL(-1), whereas the other compounds were detected in fewer samples at lower concentrations (up to 15.99μgL(-1)).
已开发出一种简单快速的分析方法用于测定水中的药物化合物。一种在线固相萃取（SPE）与液相色谱-串联质谱（LC-MS/MS）联用的方法已得到优化，用于测定环境水体中7种新兴关注污染物，检测限为纳克/升（ngL⁻¹）级别。该方法所需的样品处理最少，进样体积小（900微升），总运行时间为18分钟。对多个固相萃取参数进行了评估和优化，以实现高样品通量。因此，对样品体积、残留和小柱的可重复使用性进行了评估。对性能特征进行了评估，获得了良好的线性关系（R²>0.98）。在加标样品中对三种浓度下的回收率进行了评估，回收率范围为71%至104%。日内和日间精密度分别低于10%和13%。除1,7-二甲基黄嘌呤（20 ngL⁻¹）和布洛芬（50 ngL⁻¹）外，定量限等于或低于10 ngL⁻¹。该方法应用于20个环境水样，布洛芬是检测到的最普遍的化合物，浓度高达42.06微克/升（μgL⁻¹），而其他化合物在较少的样品中以较低浓度（高达15.99微克/升）被检测到。
