Validation and application of an analytical method for the determination of selected acidic pharmaceuticals and estrogenic hormones in wastewater and sludge

ABSTRACT

This study was undertaken to develop an extraction method for seven acidic pharmaceuticals and five steroidal estrogens from wastewater, treated wastewater and sludge samples. The temperature and time of sample derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide was optimized. Our results show that pretreatment combined with solid phase extraction (SPE) for wastewater samples (using an ENVI-C18 cartridge) and liquid-solid extraction combined with SPE (using an HLB cartridge) for sludge samples increased the analytical efficiency for acidic pharmaceuticals and estrogenic hormones using gas chromatography-mass spectrometry (GC-MS). The derivatization conditions were optimized at 40°C for 2 h. In addition, the derivatized samples were stable at ambient temperature. The new method was validated and applied to the analysis of real wastewater and discharged sludge samples from a local wastewater treatment plant. Except for 17α-ethinylestradiol, all acidic pharmaceuticals and estrogens were detected in the influent, effluent and discharged sludge samples. The concentrations of these compounds were particularly high in the discharged sludge samples.

KEYWORDS:

• Solid phase extraction
• derivatization
• gas chromatography-mass spectrometry
• wastewater treatment plant

Funding

This work was supported by Specialized Research Fund for the Doctoral Program of Higher Education (No. 20120071120033), the Natural Science Foundation of Shanghai (No. 12ZR1440900), the National Natural Science Foundation of China (No. 51108149, 41130206, 51308127), the Open Topic of State Key Laboratory of Pollution Control and Resource Reuse (No. PCRRF11014) and Anhui Provincial Natural Science Foundation (No. 11040606Q32).