Abstract
The increasing use of pharmaceuticals, their presence in the aquatic environment, and the associated toxic effects, have raised concerns in recent years. In this work, a new multi-residue analytical method was developed and validated for the determination of 10 pharmaceuticals in wastewaters using online solid-phase extraction (online SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The compounds included in the method were antineoplastics (cabazitaxel, docetaxel, doxorubicin, etoposide, irinotecan, methotrexate, paclitaxel, and topotecan), renin inhibitors (aliskiren), and antidepressants (maprotiline). The method was developed through several experiments on four online SPE cartridges, three reversed phase chromatography columns, and four combinations of mobile phase components. Under optimal conditions, very low limits of detection (LODs) of 1.30 to 10.6 ng L−1 were obtained. The method was repeatable, with relative standard deviations (RSD, %) for intraday and interday precisions ranged from 1.6 to 7.8 and from 3.3 to 13.2, respectively. Recovery values ranged from 78.4 to 111.4%, indicating the reproducibility of the method. Matrix effects were mainly presented as signal suppression, with topotecan and doxorubicin being the two most affected compounds (31.0% signal suppression). The proposed method was successfully applied to hospital effluents, detecting methotrexate (4.7–9.3 ng L−1) and maprotiline (11.2–23.1 ng L−1). Due to the shorter overall run time of 15 min, including sample preparation, and reduced sample volume (0.9 mL), this on-line SPE-LC-MS/MS method was extremely convenient and efficient in comparison to the classical off-line SPE method. The proposed method was also highly sensitive and can be used for ultratrace quantification of the studied pharmaceuticals in wastewaters, providing useful data for effective environmental monitoring.
Highlights
Several studies have evaluated the occurrence, effects, and risks of pharmaceutical compounds in the environment [1,2,3,4], with most of those studies concluding that pharmaceuticals can compromise water quality
Based on the considerations discussed above, we developed and validated an online solid-phase extraction (SPE)-LC-MS/MS method for the determination of ten pharmaceutical compounds in wastewaters
The method was optimized by fine-tuning several critical parameters that were directly related to the extraction, chromatographic and mass spectrometric behaviors of the target drugs
Summary
Several studies have evaluated the occurrence, effects, and risks of pharmaceutical compounds in the environment [1,2,3,4], with most of those studies concluding that pharmaceuticals can compromise water quality. Pharmaceuticals are commonly found in aquatic compartments at very low concentrations ranging from ultratrace (ng L−1) to trace (μg L−1) levels, which are currently regarded as potential hazard for a variety of living organisms, including humans [6,7]. The removal efficiency of pharmaceuticals greatly varies among different wastewater treatment systems, and a significant amount of the parent drugs and their transformation products may pass through and enter the aquatic environment [4,9,10,11] and wetlands [12]. Pharmaceuticals with larger consumption rates have been commonly detected in wastewater, surface water, and even in drinking water [13]. Thanks to the advancements in analytical instruments and the significant improvement in sensitivity of analytical methods, ultratrace analysis of a large group of pharmaceutical compounds in various aquatic matrices is becoming a common practice
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