On-Line Coupling of a Micro-Pressurized Liquid Extraction Method to Liquid Chromatography Via Solid-Phase Trapping
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2020-10-13
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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 seconds 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.
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Taylor, B. M., & Thurbide, K. B. (2020). On-Line Coupling of a Micro-Pressurized Liquid Extraction Method to Liquid Chromatography Via Solid-Phase Trapping. "Chromatographia". pp. 1-19. http://dx.doi.org/10.1007/s10337-020-03949-1