Department of Analytical Chemistry, Faculty of Chemical Engineering and Technology, University of Zagreb, Marulićev trg 19, 10000, Zagreb, Croatia.
Anal Bioanal Chem. 2010 Oct;398(3):1185-94. doi: 10.1007/s00216-010-4004-1. Epub 2010 Jul 29.
An analytical method for multi-class pharmaceuticals determination in wastewater has been developed and validated. Target compounds were: sulfonamides (sulfadiazine, sulfaguanidine, sulfamethazine, sulfamethoxazole), fluoroquinolones (ciprofloxacin, enrofloxacin, norfloxacin), diaminopyrimidine (trimethoprim), anaesthetic (procaine), anthelmintic (praziquantel and febantel), and macrolide (roxithromycin). The method involves pre-concentration and clean-up by solid-phase extraction (SPE) using Strata-X extraction cartridges at pH 4.0. Target analytes were identified and quantitatively determined by liquid chromatography-tandem mass spectrometry using multiple reaction monitoring (MRM). Recoveries were higher than 50% with relative standard deviation (RSD) below 18.3% for three concentrations. Only for sulfaguanidine was low recovery obtained. Matrix effect was evaluated using matrix-matched standards. The method detection limit (MDL) was between 0.5 and 5 ng L(-1) in spiked water samples. The precision of the method, calculated as relative standard deviation, ranged from 0.5 to 2.0% and from 1.4 to 8.3 for intra-day and inter-day analysis, respectively. The described analytical method was used for determination of pharmaceuticals in effluent wastewaters from the pharmaceutical industry.
已经开发和验证了一种用于废水中多类药物分析的方法。目标化合物为：磺胺类药物（磺胺嘧啶、磺胺胍、磺胺甲恶唑、磺胺甲氧嘧啶）、氟喹诺酮类药物（环丙沙星、恩诺沙星、诺氟沙星）、二氨基嘧啶（甲氧苄啶）、麻醉剂（普鲁卡因）、驱虫药（吡喹酮和非班太尔）和大环内酯类（罗红霉素）。该方法采用 pH 4.0 的 Strata-X 萃取小柱进行固相萃取（SPE）进行预浓缩和净化。采用液相色谱-串联质谱法（MRM）进行多反应监测（MRM）进行目标分析物的鉴定和定量测定。对于三种浓度，回收率高于 50%，相对标准偏差（RSD）低于 18.3%。只有磺胺胍的回收率较低。采用基质匹配标准评估基质效应。在加标水样中的方法检测限（MDL）在 0.5 和 5 ng L(-1) 之间。该方法的精密度，以相对标准偏差表示，分别在日内和日间分析中为 0.5%至 2.0%和 1.4%至 8.3%。该分析方法已用于测定制药工业废水中的药物。
