AWWA WQTC64030

The objective of this work was to investigate the presence of some pharmaceuticals and personal care products (PPCP) in an effluent of ahospital corresponding to a population of approximately 100,000 inhabitants. Compoundsbelonging to different therapeutical classes have been considered such as anti-inflammatories(ibuprofen, naproxen, diclofenac), tranquilizers (diazepam), anti-epileptics (carbamazepine) andb-blockers.The soluble content of the fragrances, anti-inflammatories, carbamazepine and diazepam wasdetermined after solid-phase extraction (SPE) of 500 ml samples using 60 mg OASIS HLBcartridges (Waters, Milford, MA, USA). Meclofenamic acid and dihydrocarbamazepine wereadded to the samples as surrogate standards. All compounds were quantitatively eluted fromthe cartridge using 3ml of ethyl acetate. This extract was then divided into two fractions: one ofthem was used for the direct determination of the soluble content of carbamazepine, diazepamand fragrances; the second one was employed for the determination of the anti-inflammatoryspecies. In this case compounds were silylated previously to their gas chromatographicseparation according to a previously published method. In both cases, GC/MS was used todetermine the concentration of the investigated compounds in the SPE extract. In the cases ofgalaxolide and tonalide, complementary methodology was used to determine the overall amountpresent in samples containing solids: the total load. A previously developed method based onan SPME (Solid Phase Micro Extraction) technique using PDMS/DVB fiber was used for thispurpose. The whole sample, including the soluble fraction and the solid particles, wasthermostatized and magnetically stirred during the extraction process. The SPME fiber wasexposed to the headspace over the sample. After the sampling time (30 min), the fiber wasdesorbed into the GC injector and GC-MS analysis was performed.Antibiotics, X-ray contrast media and estrogens were analyzed in Barcelona by the group of Dr.D. Barcel¿¿. For the first two groups, analyses were carried out by LC electrospray tandem MSafter an enrichment step using an SPE method and elution with methanol Estrogens wereanalyzed by GC (ion trap) MS/MS after an enrichment step using an SPE method, elution withacetone and derivatization with MSTFA/DTE/TMSI for 1 h at 60 8C. Values given for the different samples of the STP considered inthis work correspond to the mean value of two aliquots of each composite sample.HPLC¿¿¿MS was applied using a Hewlett-Packard (now Agilent Technologies, Palo Alto, CA,USA) Series 1100 HPLC/MSD system. An ammonium formate/formic acid buffer (10 mM, pH3.7) aqueous phase and acetonitrile were used to produce a multi-step binary elution gradient. The flow rate was 0.200 mL/min, and all flow was directed to the mass spectrometer.Separations were made using a Metasil Basic 3 µm, 150mm ¿¿ 2.0 mm, C18 analytical columncoupled to either a Metasil Basic Safeguard (MetaChem Technologies), 3 _m, 2.0mm guardcolumn, or NewGuard RP-18, 7 µm, 15mm ¿¿ 3.2mm guard column (Perkin-Elmer). Includes 26 references, tables.

Product Details

Edition:

Vol. - No.

Published:

11/01/2006

Number of Pages:

6

File Size:

1 file , 330 KB