A multi-residue analysis method was developed for the determination of penicillins in wastewater of WWTP, surface water and groundwater in Spain. The procedure involves a solid phase extraction (SPE) and the subsequent analysis by liquid chromatography coupled to tandem mass spectrometry detection (LC-QqQ-MS/MS). The SPE processes were optimized by test of cartridges, sample pH and elution solvents. ENV+ cartridge was chosen for the extraction of penicillins from different environmental samples. The best conditions for the extraction efficiency of the targets were observed at sample pH 6, by eluting solvents of methanol and acetonitrile respectively. The method has been validated by calibration curve, corresponding regression coefficient, limit of quantification and recoveries. The results showed that the recoveries of more than 90% were presented in all the compounds, except AMOX and AMPI, which had special amino-group in the molecular structure different with others. The matrix effect was also considered in the experiment and it was concluded that different matrix effect could be found between three kinds of waters, and the low retention of AMOX and AMPI on the cartridges was attributed to the matrices interference. The real sample detection showed that the penicillins degraded fast and only AMOX appeared in the studied environmental samples. The results of toxicology test on two compounds (AMOX and AMPI) showed that bacteria V. fischeri was proved to be relatively insensitive to both targets. The decreasing order of toxicity in three environmental waters for AMOX and AMPI was: wastewater > groundwater > surface water.

In this work, an n-octadecylamine functionalized mesoporous carbon nanocomposite (ODA-MPC) was synthesized, and its novel application was demonstrated by utilizing it as a sorbent in matrix solid-phase dispersion (MSPD) of nine pesticide residues identified by gas chromatography-mass spectrometer. Here, the protection of the sorbent by the mesoporous fiber membrane enabled it to process complex aqueous matrices and made it advantageous to be used in MSPD. The results confirmed the excellent ability of ODA-MPC to remove matrix interferences and reduce matrix effects compared to the traditional solid phase extraction. In particular, the recoveries were 85.0–95.8% (n = 3) with relative standard deviations less than 5%. Additionally, nine pesticide residues in vegetables and fruit were satisfactorily extracted and detected.