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Title: Beyond the wall: High-throughput quantification of plant soluble and cell-wall bound phenolics by liquid chromatography tandem mass spectrometry

Journal Article · · Journal of Chromatography
 [1];  [2];  [3];  [4]; ORCiD logo [1]
  1. Univ. of North Texas, Denton, TX (United States)
  2. NaPro Research, LLC, Washington, DC (United States)
  3. Benson Hill Biosystems, St. Louis, MO (United States)
  4. Michigan State Univ., East Lansing, MI (United States)

Plants accumulate several thousand of phenolic compounds, including lignins and flavonoids, which are mainly synthesized through the phenylpropanoid pathway, and play important roles in plant growth and adaptation. A novel high-throughput ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method was established to quantify the levels of 19 flavonoids and 15 other phenolic compounds, including acids, aldehydes, and alcohols. The chromatographic separation was performed in 10 minutes, allowing for the resolution of isomers such as 3-, 4-, and 5-chlorogenic acids, 4-hydroxybenzoic and salicylic acids, isoorientin and orientin, and luteolin and kaempferol. The linearity range for each compound was found to be in the low fmol to the high pmol. Furthermore, this UHPLC-MS/MS approach was shown to be very sensitive with limits of detection between 1.5 attomoles to 300 fmoles, and limits of quantification between 5 attomoles to 1,000 fmoles. Extracts from maize seedlings were used to assess the robustness of the method in terms of recovery efficiency, matrix effect, and accuracy. The biological matrix did not suppress the signal for 32 out of the 34 metabolites under investigation. Additionally, the majority of the analytes were recovered from the biological samples with an efficiency above 75 %. All flavonoids and other phenolic compounds had an intra- and inter-day accuracy within a ± 20 % range, except for coniferyl alcohol and vanillic acid. Finally, the quantification of flavonoids, free and cell wall-bound phenolics in seedlings from two maize lines with contrasting phenolic content was successfully achieved using this methodology.

Research Organization:
Univ. of North Texas, Denton, TX (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Biological and Environmental Research (BER)
Grant/Contract Number:
SC0016490
OSTI ID:
1658576
Journal Information:
Journal of Chromatography, Vol. 1589; ISSN 0021-9673
Publisher:
ElsevierCopyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 28 works
Citation information provided by
Web of Science

References (37)

Evolution and current status of research in phenolic compounds journal November 2007
Antioxidant properties of phenolic compounds journal April 1997
Metabolic Engineering of the Phenylpropanoid and Its Primary, Precursor Pathway to Enhance the Flavor of Fruits and the Aroma of Flowers journal November 2015
Metabolic Engineering of the Phenylpropanoid Pathway Enhances the Antioxidant Capacity of Saussurea involucrata journal August 2013
Techniques for Analysis of Plant Phenolic Compounds journal February 2013
Synthesis, isolation, identification and characterization of new process-related impurity in isoproterenol hydrochloride by HPLC, LC/ESI-MS and NMR journal December 2017
Determination of Free and Total Phenolic Acids in Plant-Derived Foods by HPLC with Diode-Array Detection journal May 2002
Simultaneous Quantification of Flavonoids and Phenolic Acids in Plant Materials by a Newly Developed Isocratic High-Performance Liquid Chromatography Approach journal October 2010
Methods for Determining Cell Wall-Bound Phenolics in Maize Stem Tissues journal January 2018
Polyphenolic composition and antioxidant activity of açai (Euterpe oleracea Mart.) from Colombia journal February 2017
A new ultrahigh performance liquid chromatography with diode array detection coupled to electrospray ionization and quadrupole time-of-flight mass spectrometry analytical strategy for fast analysis and improved characterization of phenolic compounds in apple products journal November 2013
Fast Detection of Phenolic Compounds in Extracts of Easter Pears (Pyrus communis) from the Atacama Desert by Ultrahigh-Performance Liquid Chromatography and Mass Spectrometry (UHPLC–Q/Orbitrap/MS/MS) journal January 2016
An Optimized Method for Analysis of Phenolic Compounds in Buds, Leaves, and Fruits of Black Currant (Ribes nigrum L.) journal October 2012
An UPLC-MS/MS Method for the Simultaneous Identification and Quantitation of Cell Wall Phenolics in Brassica napus Seeds journal February 2013
Targeted Metabolomics of the Phenylpropanoid Pathway in Arabidopsis thaliana using Reversed Phase Liquid Chromatography Coupled with Tandem Mass Spectrometry : Measuring Lignin Precursors by LC-MS journal February 2017
Flavone-rich maize: an opportunity to improve the nutritional value of an important commodity crop journal September 2014
A Novel Reduplicate Strategy for Tracing Hemostatic Compounds from Heating Products of the Flavonoid Extract in Platycladi cacumen by Spectrum-Effect Relationships and Column Chromatography journal September 2015
Determination of the phenolic composition from Brazilian tropical fruits by UHPLC–MS/MS journal August 2015
Qualitative and Quantitative Analysis of Phenolic Acids, Flavonoids and Iridoid Glycosides in Yinhua Kanggan Tablet by UPLC-QqQ-MS/MS journal July 2015
Quantitative determination of plant phenolics in Urtica dioica extracts by high-performance liquid chromatography coupled with tandem mass spectrometric detection journal January 2014
Simultaneous detection of flavonoids and phenolic acids in Herba Lysimachiae and Herba Desmodii Styracifolii using liquid chromatography tandem mass spectrometry journal May 2013
Quantifying the Labeling and the Levels of Plant Cell Wall Precursors Using Ion Chromatography Tandem Mass Spectrometry journal May 2010
Targeted Metabolomics of Physaria fendleri, an Industrial Crop Producing Hydroxy Fatty Acids journal February 2014
High-throughput quantification of the levels and labeling abundance of free amino acids by liquid chromatography tandem mass spectrometry journal March 2017
Using MetaboAnalyst 3.0 for Comprehensive Metabolomics Data Analysis journal September 2016
A critical review of methods for characterisation of polyphenolic compounds in fruits and vegetables journal June 2011
Mass spectrometric behavior of phenolic acids standards and their analysis in the plant samples with LC/ESI/MS system journal September 2014
Hierarchical Scheme for LC-MS n Identification of Chlorogenic Acids journal May 2003
LC-DAD/ESI-MS/MS study of phenolic compounds in ash (Fraxinus excelsior L. and F. americana L.) heartwood. Effect of toasting intensity at cooperage: LC-DAD/ESI-MS/MS of ash wood phenolic compounds journal July 2012
Characterization of Flavonoid Glycosides from Fenugreek (Trigonella foenum-graecum) Crude Seeds by HPLC–DAD–ESI/MS Analysis journal November 2014
Structure elucidation of glycosphingolipids and gangliosides using high-performance tandem mass spectrometry journal March 1988
Determination of flavone, flavonol, and flavanone aglycones by negative ion liquid chromatography electrospray ion trap mass spectrometry journal June 2001
Characterization of flavone and flavonol aglycones by collision-induced dissociation tandem mass spectrometry journal August 1997
Characterization of 3-methoxyflavones using fast-atom bombardment and collision-induced dissociation tandem mass spectrometry journal October 1999
Signal suppression/enhancement in high-performance liquid chromatography tandem mass spectrometry journal June 2010
Determination of Flavonoids and Phenolics and Their Distribution in Almonds journal July 2006
Insoluble-Bound Phenolics in Food journal September 2016

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