Microwave-assisted solvent extraction of solid matrices and subsequent detection of pharmaceuticals and personal care products (PPCPs) using gas chromatography-mass spectrometry

Concentrations of pharmaceuticals and personal care products (PPCPs) in natural solids remain largely unknown. Contributing to this, is a lack of methods permitting the simultaneous detection of the diverse, low-level contaminants present in these complex matrices. We have developed a microwave-assisted solvent extraction (MASE)-based method targeting seven diverse PPCPs (caffeine, 17 beta-estradiol, ibuprofen, ketoprofen, musk ketone, naproxen, and triclosan) and a molecular marker for fecal waste (epicoprostanol). The method consisted of optimizing the following variables: derivatization of the polar target analytes, silica gel open column clean-up, and gas chromatographic-mass spectrometric (GC-MS) analysis of sample extracts for analysis and detection of the compounds noted above. Testing of the method on spiked soil allowed for 89.6 +/- 2.89% recovery of three target compounds and 25.0 +/- 1.93% recovery of five of the compounds. Although the latter recoveries were low, the precision across all recoveries was high, suggesting good reproducibility in application of the method. Furthermore, we suspect that matrix effects are likely responsible for the lower recoveries. Techniques with the exclusive incorporation of organic solvents were found inapplicable in the study of a pharmaceutical salt, diphenhydramine HCl. Application of the developed method to sediment collected directly downstream of the effluent pipe of a wastewater treatment plant allowed detection of ibuprofen, naproxen, ketoprofen, and epicoprostanol, at ng-mu g per gram dry weight concentrations. The observation of acidic pharmaceuticals, previously believed to exhibit insignificant sorption to solid matrices, in the tested sediment samples, coupled with application of biosolids for agricultural purposes, demonstrates the need for expanded investigation of PPCP contamination of natural solid matrices. (c) 2007 Elsevier B.V. All rights reserved.