Rapid determination of pharmaceuticals from multiple therapeutic classes in wastewater by solid-phase ex- traction and ultra-performance liquid chromatography tandem mass spectrometry

Chinese Science Bulletin (Impact Factor: 1.58). 07/2009; 54(24):4633-4643. DOI: 10.1007/s11434-009-0413-y


A new analytical method utilizing ultra-performance liquid chromatography (UPLC) tandem mass spectrometry (MS/MS) has been developed to determine 16 pharmaceuticals from 8 therapeutic classes in wastewater: bezafibrate, clofibric acid, carbamazepine, caffeine, chloramphenicol, diclofenac, gem-fibrozil, indomethacin, ketoprofen, mefenamic acid, metoprolol, nalidixic acid, N,N-diethyl-meta-tol-uamide, propranolol, sulpiride and trimethoprim. Key parameters of MS/MS, UPLC and solid phase extraction (SPE) were optimized. In general, recovery of target pharmaceuticals was over 70% for the wastewater effluent samples and 50% for the influent samples. The effects of matrix suppression, loss during the pretreatment as well as instrument variability were successfully corrected by two internal standards, and acceptable relative recovery was obtained. Target compounds were quantitatively ana-lyzed using multiple reaction monitoring (MRM) mode, and the detection limits ranged from 0.3 to 20 ng/L. A detailed study, matrix effect in effluent wastewater was also present. The method was applied to detecting pharmaceuticals in the wastewater from three wastewater treatment plants (WWTPs) in Bei-jing, China and the results demonstrated that most target compounds were detectable in both the in-fluent and effluent, with the mean concentrations ranging from 20.5 to 5775.6 ng/L and 4.6 to 418.6 ng/L, respectively. pharmaceuticals, solid phase extraction, tandem mass spectrometry, UPLC, wastewater

Download full-text


Available from: Jun Huang
  • Source
    • "Multiple reaction monitoring was applied for detection. The details of separations and mass spectrometer parameters for each compound are described in our previous study (Sui et al., 2009). "
    [Show abstract] [Hide abstract]
    ABSTRACT: This work investigates, for the first time, the occurrence and sources of 15 pharmaceuticals and personal care products (PPCPs) in surface water of Beijing, one of most densely populated cities in the world, in three sampling events representing different seasonal flow conditions. The detection frequencies of most PPCPs were in the range of 50-100%. The median concentrations of the selected PPCPs ranged from not detected to 4200ngL(-1) (caffeine). Generally, higher PPCP levels were observed in early spring, indicating both low flow condition and cold-water temperature might enhance their persistence. Source apportionment showed freshly discharged untreated sewage (67%) significantly contributed to the PPCP burden in the Beiyun River, which provides important information for environmental management.
    Full-text · Article · Oct 2014 · Chemosphere
  • Source
    [Show abstract] [Hide abstract]
    ABSTRACT: The occurrence and removal of 13 pharmaceuticals and 2 consumer products, including antibiotic, antilipidemic, anti-inflammatory, anti-hypertensive, anticonvulsant, stimulant, insect repellent and antipsychotic, were investigated in four wastewater treatment plants (WWTPs) of Beijing, China. The compounds were extracted from wastewater samples by solid-phase extraction (SPE) and analyzed by ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS). Most of the target compounds were detected, with the concentrations of 4.4 ng L(-1)-6.6 microg L(-1) and 2.2-320 ng L(-1) in the influents and secondary effluents, respectively. These concentrations were consistent with their consumptions in China, and much lower than those reported in the USA and Europe. Most compounds were hardly removed in the primary treatment, while their removal rates ranging from -12% to 100% were achieved during the secondary treatment. In the tertiary treatment, different processes showed discrepant performances. The target compounds could not be eliminated by sand filtration, but the ozonation and microfiltration/reverse osmosis (MF/RO) processes employed in two WWTPs were very effective to remove them, showing their main contributions to the removal of such micro-pollutants in wastewater treatment.
    Full-text · Article · Aug 2009 · Water Research
  • [Show abstract] [Hide abstract]
    ABSTRACT: Absorption spectra and refractive indices of benzimidazole molecules have been measured by terahertz time-domain spectroscopy (THz-TDS) in the room temperature and nitrogen conditions. We discussed the absorption spectra of thiabendazole and carbendazim in THz region. Meanwhile, density functional theory (DFT) with software package Gaussian 03 was employed for optimization and vibration analysis. The distinct absorption peaks of those molecules were caused by intermolecular hydrogen-bonding, molecular torsion or vibration modes, absorption of water molecules, etc. This result shows that the THz-TDS can be used for distinguishing between thiabendazole and carbendazim. As the absorption spectra are highly sensitive to the overall structure and configuration of the molecules, the THz-TDS procedure can provide a direct fingerprint of the molecular structure or conformational state of a compound.
    No preview · Article · May 2011
Show more