Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1316, Issue -, Pages 8-14Publisher
ELSEVIER
DOI: 10.1016/j.chroma.2013.09.034
Keywords
Membrane microextraction; Amino; Urea; Sorbents; Enrichment factors; Pharmaceuticals
Funding
- Singapore National Research Foundation
- National University of Singapore (NUS)
- NUS Graduate School of Integrative Sciences and Engineering
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Individual polar sorbents with surface-displayed amino groups (APS) and non-nucleophilic urea-groups (UPS), were prepared by chemical modification of granular silica gel with bifunctional silane coupling reagents. In this preliminary study, they were separately employed for micro-solid phase extraction (mu-SPE) of the quarternary salt of Amitriptyline (And), Carbamazepine (Cbz), Ketoprofen (Met) and Diclofenac (Dfn) from aqueous samples in conjunction with high performance liquid chromatography. The resulting enrichment factors for both APS and UPS are comparable and exceeded those of mu-SPE involving commercial C18-silica gel sorbents. The presence of highly polar, but non-basic and non-nucleophilic surfaces on UPS prompted the development of a UPS-based mu-SPE method. Good linear correlation was found over a concentration range of 0-50 mu g L-1 with limits of detection ranging from 0.66 to 2.36 mu g L-1). Limits of quantification between 1.61 and 7.88 mu g L-1 were obtained. HPLC analyses indicated that relative recoveries of 123% for Ami, 65.6% for Cbz, 71.2% for Ket and 66.5% for Dfn were obtained during mu-SPE of spiked (10 mu g L-1) environmental water samples with percentage relative standard deviations (%RSD) of between 2.1% and 12.6%. (C) 2013 Elsevier B.V. All rights reserved.
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