Development of selective comprehensive two-dimensional liquid chromatography with parallel first-dimension sampling and second-dimension separation—application to the quantitative analysis of furanocoumarins in apiaceous vegetables
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Various implementations of two-dimensional high-performance liquid chromatography are increasingly being developed and applied to the analysis of complex materials, including those encountered in the analysis of foods, beverages, and nutraceuticals. Previously, we introduced the concept of selective comprehensive two-dimensional liquid chromatography (sLC × LC) as a hybrid between the more conventional, but extreme opposite sampling modes of heartcutting (LC–LC) and fully comprehensive (LC × LC) 2D separation. The sLC × LC approach breaks the link between first dimension (1D) sampling time and second dimension (2D) analysis time that is faced in LC × LC and allows very rapid (as low as 1 s) sampling of highly efficient 1D separations, while at the same time allowing efficient 2D separations on the timescale of tens of seconds. In this paper, we improve upon our previous sLC × LC work by demonstrating the ability to perform the processes of 1D sampling and 2D separation in parallel. This significantly improves the flexibility of the technique and allows targeted analysis of analytes that elute close together in time in the 1D separation. To demonstrate the value of this added capability, we have developed a sLC × LC method using multi-wavelength ultraviolet absorbance detection for the quantitative analysis of six target furanocoumarin compounds in extracts of celery, parsley, and parsnips. We show that 2D separations of 1D effluent containing the target compounds of interest reveal the presence of unanticipated interferent peaks that would otherwise compromise the quantitative accuracy of the method. We also demonstrate the application of the chemometric method iterative key set factor analysis with alternating least-squares to sLC × LC to mathematically resolve target compounds that are only slightly separated chromatographically but not sufficiently resolved for accurate quantitation.
KeywordsLiquid chromatography Two-dimensional Furanocoumarin Chemometrics Selective comprehensive Targeted analysis
All of the HPLC columns used in this work were generous gifts from their respective manufacturers. The flow selector valves were generous gifts of Cadence Fluidics, LLC. DRS, EDL, and DCH were supported by a Faculty Startup Award from the Camille and Henry Dreyfus Foundation. EDL was also supported by a research scholarship from the Howard Hughes Medical Institute. RCA was supported by an Altria Fellowship from VCU, and the work of SCR and RCA was supported by NSF grant CHE-0911330. SPT was supported by NCI grant 5K07CA128952-03. We would also like to acknowledge Jae Kyeom Kim, Scott Simpkins, Noemia Strapazzon, and Lindsay Young for providing vegetable samples.
- 3.Karger BL, Snyder LR, Horvath C (1973) An introduction to separation science. Wiley, New YorkGoogle Scholar
- 14.Dugo P, Mondello L, Cacciola F, Donato P (2011) In: Mondello L (ed) Comprehensive two-dimensional liquid chromatography combined with mass spectrometry. Wiley, New YorkGoogle Scholar
- 16.Dugo P, Mondello L, Cacciola F, Donato P (2011) In: Mondello L (ed) Comprehensive two-dimensional liquid chromatography applications. Wiley, New YorkGoogle Scholar
- 22.Eeltink S, Dolman S, Ursem M, Swart R, McLeod F, Schoenmakers PJ (2009) Maximizing the peak production rate in off-line comprehensive two-dimensional liquid chromatography with mass spectrometry design. LC-GC Eur 22:404–406, 408–410, 412–413Google Scholar
- 27.Carr PW, Davis JM, Rutan SC, Stoll DR (2012) In: Grushka E, Grinberg N (eds) Principles of online comprehensive multidimensional liquid chromatography. CRC Press, Boca RatonGoogle Scholar
- 33.Paine MF, Widmer WW, Hart HL, Pusek SN, Beavers KL, Criss AB, Brown SS, Thomas BF, Watkins PB (2006) A furanocoumarin-free grapefruit juice establishes furanocoumarins as the mediators of the grapefruit juice-felodipine interaction. Am J Clin Nutr 83:1097–1105Google Scholar
- 34.Guo L, Yamazoe Y (2004) Inhibition of cytochrome P450 by fruanocumarins in grapefruit juice and herbal medicines. Acta Pharmacol Sin 25:129-136Google Scholar
- 57.Vivó-Truyols G, van der Wal S, Schoenmakers PJ (2010) Comprehensive study on the optimization of online two-dimensional liquid chromatographic systems considering losses in theoretical peak capacity in first- and second-dimensions: a pareto-optimality approach. Anal Chem 82:8525–8536CrossRefGoogle Scholar