On-Line Coupling of a Micro-Pressurized Liquid Extraction Method to Liquid Chromatography Via Solid-Phase Trapping
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ORIGINAL
On‑Line Coupling of a Micro‑Pressurized Liquid Extraction Method to Liquid Chromatography Via Solid‑Phase Trapping Bradley M. Taylor1 · Kevin B. Thurbide1 Received: 14 July 2020 / Revised: 25 August 2020 / Accepted: 28 August 2020 © Springer-Verlag GmbH Germany, part of Springer Nature 2020
Abstract A novel method is introduced which employs fast on-line micro-pressurized liquid extraction (µPLE) directly interfaced with HPLC via a solid-phase extraction (SPE) trap. The technique utilizes rapid heating to remove analytes from 5–10 mg samples in typically 20 s using only about 200 µL of solvent. The resulting extract is then internally transferred to an SPE trap, where the analyte is absorbed/concentrated and then later completely desorbed/injected to an HPLC for chromatographic analysis. Test extractions of caffeine from Ottawa sand show that analyte in the 200 µL µPLE extract can be quantitatively trapped by SPE (100 ± 4%; n = 3), whereas even moderately larger extract volumes (e.g., 1 mL), still well below those normally used in conventional PLE, led to poor recoveries and precision (1.0 ± 0.5% recovery; n = 3). As a result, it was found that the on-line µPLE-SPE system could provide near 400-fold analyte enrichment factors that enhanced the analysis of samples with low analyte levels. For instance, application of the method showed that it can facilitate the analysis of impurities in pharmaceutical tablets and pesticide residues in fruit flesh. The on-line µPLE-SPE system also provided relatively rapid quantitative results in this regard. For example, the technique, respectively, recovered 95 ± 3% (n = 5) and 99 ± 3% (n = 4) of a phenoxypropionic acid herbicide from strawberry and apple samples and was about 10–30 times faster than a conventional ultrasonic extraction method. The findings indicate that on-line µPLE-SPE can facilitate coupling to HPLC and provide very rapid sample preparation/preconcentration using little solvent. Graphic abstract
On-line μPLE API SPE trap
Impurities
HPLC
Keywords Micro · On-line analysis · HPLC · Solid-phase trapping · Pressurized liquid extraction
Introduction Submitted for publication as an original research paper in: Chromatographia. * Kevin B. Thurbide [email protected] 1
Department of Chemistry, University of Calgary, Calgary, AB T2N 1N4, Canada
Modern analytical sample preparation is as an important area that is increasingly guided by principles which produce samples for analysis with minimal time and waste involved [1, 2]. Currently in this regard, one of the most effective methods developed for solid samples is pressurized liquid
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extraction (PLE). PLE essentially uses a heated pressurized solvent to assist in disrupting analyte-matrix interactions while increasing mass transfer rates to yield an overall improved extraction performance [3]. For example, PLE typically requires only 10–15 min of extraction time and 10–25 mL of solvent per sample [4, 5]. Nonetheless, since even these favourable metrics can still potentially
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