Tandem HILIC‐RP liquid chromatography for increased polarity coverage in food analysis

Comprehensive non‐targeted analysis of food products normally requires two complementary chromatographic runs to achieve maximum compound coverage. In this study, we present a sensitive tandem‐LC method, which combines RP and HILIC separation in a single run. The setup consists of a C18 trap column and two subsequently coupled analytical columns (HILIC and C18) which are operated in parallel. First, hydrophobic compounds are retained on the RP trap column while rather hydrophilic compounds are directly transferred onto a HILIC phase. Next, the pre‐fractionated sample composition is analyzed by HILIC or RP chromatography, respectively. The presented setup allows individual and independent gradient elution as well as interfacing with mass spectrometry. The performance of the method has been proven by means of food relevant standards and analysis of complex food samples (e.g. red wine, meat extract). The simple and robust setup provides high flexibility in the selection of column combinations and does not require sophisticated instrumental setups or software. The method significantly increases the covered polarity range compared to classical one‐dimensional chromatography. Our results indicate that tandem LC is a valuable and universal tool in the non‐targeted screening of various types of complex food samples.

[1]  I. Ferrer,et al.  Liquid chromatography/quadrupole-time-of-flight mass spectrometry with metabolic profiling of human urine as a tool for environmental analysis of dextromethorphan. , 2012, Journal of chromatography. A.

[2]  B. McCarry,et al.  Tandem LC columns for the simultaneous retention of polar and nonpolar molecules in comprehensive metabolomics analysis. , 2013, Journal of separation science.

[3]  B. Hammock,et al.  Mass spectrometry-based metabolomics. , 2007, Mass spectrometry reviews.

[4]  I. Losito,et al.  Hydrophilic interaction and reversed phase mixed-mode liquid chromatography coupled to high resolution tandem mass spectrometry for polar lipids analysis. , 2016, Journal of chromatography. A.

[5]  G. Rainer,et al.  Analysis of multiple quaternary ammonium compounds in the brain using tandem capillary column separation and high resolution mass spectrometric detection. , 2012, Journal of chromatography. A.

[6]  Jairus Bowne,et al.  A tandem liquid chromatography–mass spectrometry (LC–MS) method for profiling small molecules in complex samples , 2015, Metabolomics.

[7]  Philippe Schmitt-Kopplin,et al.  The chemodiversity of wines can reveal a metabologeography expression of cooperage oak wood , 2009, Proceedings of the National Academy of Sciences.

[8]  K. Burgess,et al.  Recent advances in liquid and gas chromatography methodology for extending coverage of the metabolome. , 2017, Current opinion in biotechnology.

[9]  A. Gómez-Caballero,et al.  Untargeted metabolomic analysis using liquid chromatography quadrupole time-of-flight mass spectrometry for non-volatile profiling of wines. , 2015, Analytica chimica acta.

[10]  M. González-Sanjosé,et al.  Various applications of liquid chromatography-mass spectrometry to the analysis of phenolic compounds. , 1999, Journal of chromatography. A.

[11]  Serially coupling hydrophobic interaction and reversed-phase chromatography with simultaneous gradients provides greater coverage of the metabolome , 2015, Metabolomics.

[12]  M. Witting,et al.  Integrating analytical resolutions in non-targeted wine metabolomics , 2015 .

[13]  P. Sandra,et al.  Serial coupling of reversed-phase and hydrophilic interaction liquid chromatography to broaden the elution window for the analysis of pharmaceutical compounds. , 2008, Journal of chromatography. A.

[14]  I. Wilson,et al.  LC-MS-based methodology for global metabolite profiling in metabonomics/metabolomics , 2008 .

[15]  R. Kostiainen,et al.  Effect of eluent on the ionization efficiency of flavonoids by ion spray, atmospheric pressure chemical ionization, and atmospheric pressure photoionization mass spectrometry. , 2001, Journal of mass spectrometry : JMS.

[16]  P. Schmitt‐Kopplin,et al.  Liquid chromatography-mass spectrometry in metabolomics research: mass analyzers in ultra high pressure liquid chromatography coupling. , 2013, Journal of chromatography. A.

[17]  Thomas Letzel,et al.  Serial coupling of reversed-phase and zwitterionic hydrophilic interaction LC/MS for the analysis of polar and nonpolar phenols in wine. , 2013, Journal of separation science.

[18]  Richard A Dixon,et al.  Phytochemistry meets genome analysis, and beyond. , 2003, Phytochemistry.

[19]  A. Atanassov,et al.  Wine Metabolite Profiling: Possible Application in Winemaking and Grapevine Breading in Bulgaria , 2009 .

[20]  Xin Lu,et al.  Novel, fully automatic hydrophilic interaction/reversed-phase column-switching high-performance liquid chromatographic system for the complementary analysis of polar and apolar compounds in complex samples. , 2008, Journal of chromatography. A.

[21]  P. Schmitt‐Kopplin,et al.  A grape and wine chemodiversity comparison of different appellations in Burgundy: vintage vs terroir effects. , 2014, Food chemistry.

[22]  J. R. Torres-Lapasió,et al.  Stationary phase modulation in liquid chromatography through the serial coupling of columns: A review. , 2016, Analytica chimica acta.