A Simple Method for the Simultaneous Determination of Pharmaceuticals and Personal Care Products in River Sediment by Ultrasound-Assisted Extraction Followed by Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry.

Abstract

A simple method was developed using ultrasound-assisted extraction (UAE) combined with solid-phase microextraction (SPME) coupled with gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of eight different pharmaceuticals and personal care products (PPCPs) (ibuprofen, 2-benzyl-4-chlorophenol, naproxen, triclosan, ketoprofen, diclofenac, bisphenol A and estrone) in river sediment. UAE conditions were optimized involving extraction variables such as extraction solvent, extraction time, sample amount, extraction temperature, pH and salt addition. A 100 mg of sediment was extracted by optimized UAE process using 7 mL deionized water (pH 3) + 1% methanol as solvent, room temperature and 1 min extraction at 70% of amplitude. A 5 mL of supernatant was subsequently extracted by SPME; the extracted analytes were derivatized on fiber in head-space mode with N-methyl-N-(tertbutyldimethylsilyl) trifluoroacetamide and then analyzed by GC-MS. The developed method was evaluated by testing: precision (CV < 8%), linearity (R > 0.98), recoveries (56-108%), limits of detection (<0.25 ng/g) and quantitation (<0.8 ng/g). Finally, the method was successfully applied to sediment samples collected from Tula River, Hidalgo, Mexico (one of the most polluted river) in which naproxen and triclosan were identified at ng/g concentration levels. Quantitative results were compared with Tula River water samples, showing PPCPs distribution rate between water and sediment. The method is robust, simple and environmentally friendly, and provides straightforward analyses of these trace organic pollutants in sediment samples.