“Chemical Characterization of Nutraceuticals:
Speciation by Liquid Chromatography Mass
Spectrometry”

Mass
spectrometry (MS) is a very useful analytical technique because it provides
structural information at the atomic and molecular level. It has also
become a useful tool for biological analysis such as protein and DNA. For
example, in a genomic study MS determines the abundance and identities of
nucleobases present in a DNA sample. The use of particle beam glow discharge
mass spectrometry (PB-GDMS) in our laboratory allows easier spectral
analysis because it produces both atomic and molecular information in the same
spectra. The particle beam glow discharge (PB-GD) source de-couples the
vaporization and ionization steps leading to much simpler spectra.
In
this lab the a HPLC is coupled to a particle beam interface, which removes
solvent vapor and lighter elements (e.g. He) through a series of
nebulization and momentum separation steps and is then introduced into the
GD/MS for subsequent detection. The use of low-pressure plasma such as the
glow discharge (GD) provided good speciation analysis in mass spectrometry with
not spectral interferences from the atmosphere. Research in the laboratory with
the PB-GDMS system will include the analysis of liquid samples for metal
speciation in nutraceutical products, speciation of metal-containing compounds
(e.g. selenoproteins and selenoaminoacids) as well as introduction of a new
source hollow cathode discharge geometry for the PB-GDMS.
“Metals Analysis
of Botanical Products in Various Matrices Using a Single Microwave Digestion
and Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) Method”,
Joaudimir Castro, Julia C. Spraul and R. Kenneth Marcus, Analytical Methods, 2009,
1, 188–194.
“On-line Separation and Identification of Inorganic
and Organic Arsenic Species in Ethanolic Kelp and Bladderwrack Extracts Through
Liquid Chromatography/Particle Beam-Electron Ionization Mass Spectrometry (LC/PB-EIMS)”,
M.V.B. Krishna, J. Castro, T.M. Brewer, and
R.K. Marcus, J. Anal. At. Spectrom. 2009, 24(2), 199-208.
“Liquid
Chromatography Particle Beam/Mass Spectrometry Analysis of Botanical Products Using
both Electron Impact and Glow Discharge Ionization Sources”, J. Castro,
M.V.B. Krishna, and R.K. Marcus, American Laboratory News Edition, February
2008, 40 (4), 8.
“Analysis and Characterization of Botanical
Products. Speciation by particle beam mass spectrometry.” Joaudimir Castro and R. Kenneth Marcus,
G.I.T. Laboratory Journal, 2007, 11 (3-4), 58-59.
“Online Mercury Speciation through
Liquid Chromatography with Particle Beam/Electron Ionization Mass Spectrometry
Detection”, M. V.
Balarama Krishna, Joaudimir Castro, Tim M. Brewer, and R. Kenneth Marcus, J.
Anal. At. Spectrom., 2007, 22, 283-291.
“Electron Impact and Glow Discharge
Ionization LC/MS Analysis of Green Tea Tincture”, Jacob Venzie, Joaudimir Castro, M. V.
Balarama Krishna, and R. Kenneth Marcus, Analytical and Bioanalytical
Chemistry, 2007, 387, 321-333.
“Particle
Beam Sample Introduction into Glow Discharge Plasmas for Speciation Analysis”, Tim M. Brewer, Joaudimir Castro, and
R. Kenneth Marcus, Spectrochimica Acta B Review, 2006, 61, 134-149.
“A
greener approach to aspirin synthesis using microwave irradiation”, David Sanabria, Marilyn Garcia,
Joaudimir Castro, Johanna Fajardo,
Book Chapters
“Ion source geometries
and mass analyzers in glow discharge mass spectrometry”, Joaudimir Castro, C.
Derrick Quarles Jr. and R. Kenneth Marcus, accepted for publication in The
Encyclopedia of Mass Spectrometry-Elemental and Isotope Mass Spectrometry.
“Glow Discharge Mass
Spectrometry”, C. Derrick Quarles Jr., Joaudimir Castro and R. Kenneth
Marcus, accepted for publication in The Encyclopedia of Spectroscopy and
Spectrometry.
Oral
Presentations
“Speciation of Botanical Extracts
by HPLC-Particle Beam/Glow Discharge Mass Spectrometry”, R. Kenneth Marcus, Joaudimir Castro, and Carolyn E.
Quarles, presented at the 2010 Winter Conference on Plasma Spectrochemistry,
Fort Myers, FL, January 4-9, 2010.
“Liquid
Chromatography Particle Beam Mass Spectrometry (LC-PB/MS): An Analytical Tool
for the Characterization of Botanical Products”, Joaudimir Castro, and R. Kenneth Marcus, presented at
the 61st Southeastern Regional Meeting of the American Chemical
Society, San Juan, PR, October 21-24, 2009.
“Lead speciation in botanical extracts
via liquid chromatography particle beam mass spectrometry”, Joaudimir Castro and R. Kenneth
Marcus, presented at the 2009 International Symposium on Metallomics,
Cincinnati, OH, June 7-10, 2009.
“Evaluation of a Liquid
Chromatography-Particle Beam/Mass Spectrometry (LC-PB/MS) System for the
Comprehensive Speciation of Arsenic and Selenium Species in Biological Fluids”,
Joaudimir Castro and R. Kenneth Marcus, presented at the
2009 Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy,
Chicago, IL, March 8-12, 2009.
“Comprehensive Speciation of Botanical
Products”, R.
Kenneth Marcus and
Joaudimir Castro, presented at the 2009 Pittsburgh Conference on Analytical
Chemistry and Applied Spectroscopy, Chicago, IL, March 8-12, 2009.
“Development of a Hollow Cathode
Geometry for Particle Beam Glow Discharge Mass Spectrometry” J. Castro, M.V.B. Krishna and
R.K. Marcus, presented at the 2008 Federation of Analytical Chemistry and Spectroscopy
Conference, Reno, NV, September 28 – October 2, 2008.
“Validation of a High Performance Liquid
Chromatography Particle Beam Mass Spectrometry (LC-PB/MS) with Electron Impact
and Glow Discharge Ionization Sources for Botanical Extracts”, Joaudimir Castro, M.V. Balarama
Krishna and R. Kenneth Marcus, presented at the 2008 Pittsburgh Conference on
Analytical Chemistry and Applied Spectroscopy, New Orleans, LA, March 2-7,
2008.
“Comprehensive Selenium Speciation
Analysis of Selenium-Enriched Samples through Liquid Chromatography-Particle
Beam/Mass Spectrometry (LC-PB/MS)”,
J. Castro, G. Ojeda, M.V.B. Krishna, and R.K. Marcus, presented at the
2008 Pittsburgh Conference on Analytical Chemistry and Applied Spectroscopy,
New Orleans, LA, March 2-7, 2008.
“Comprehensive Selenium Speciation
through Liquid Chromatography Particle Beam Mass Spectrometry (LC-PB/MS) via
Electron Impact and Glow Discharge Ionization”, Joaudimir Castro, Geovannie
Ojeda,
“Comprehensive Speciation of Botanical
Extracts HPLC-Particle Beam/Glow Discharge Mass Spectrometry”, R.K. Marcus, M.V.B. Krishna and J. Castro,
presented at the 2008 Winter Conference Plasma Spectrometry, Temecula, CA,
January 6-12, 2008.
“Chemical Characterization of Botanical
Products”, Joaudimir
Castro, Timothy M. Brewer,
“Comprehensive Speciation in the
Characterization of Botanical Extracts and Nutraceuticals”, R. Kenneth Marcus, Timothy M. Brewer, Joaudimir Castro,
and
“High Performance Liquid Chromatography
Particle Beam/Mass Spectrometry (HPLC-PB/MS) Analysis of Nutraceuticals Using
Electron Impact and Glow Discharge Ionization Sources”, Joaudimir Castro, M. V. Balarama
Krishna, John R. Choiniere,
“Chromatographic and Mass Spectral
Techniques for the Analysis of Caffeic Acid Derivatives in Echinacea purpurea
Extract”, Joaudimir
Castro, M. V. Balarama Krishna, John R. Choiniere and R. Kenneth Marcus,
presented at the 2007 Pittsburgh Conference on Analytical Chemistry and Applied
Spectroscopy, Chicago, IL, February 25-March 2, 2007.
“Heavy Metal Analysis in Botanical
Extracts using Microwave Digestion and an Inductive Coupled Plasma Atomic
Emission Spectrometry (ICP-AES) Method”, Joaudimir Castro, Julia E. Cooper and R. Kenneth
Marcus, presented at the 2007 Pittsburgh Conference on Analytical Chemistry and
Applied Spectroscopy, Chicago, IL, February 25-March 2, 2007.
“Comprehensive Speciation using Particle
Beam Methods: Biological, Food, and Environmental Chemistries”, R. Kenneth Marcus, Timothy M. Brewer, Joaudimir Castro,
and
“New Separation and Detection Schemes
for Metal Speciation of Botanical Products”, R. Kenneth Marcus, Tim M. Brewer, Joaudimir Castro
and
“High Performance Liquid
Chromatography-Particle Beam/Glow Discharge-Mass Spectrometry (HPLC-PB/GDMS)
Analysis of Green Tea Extract”, Joaudimir Castro, Jacob L. Venzie,
“Capillary-Channeled Polymer (C-CPTM)
Fibers as a Stationary Phase for High Performance Liquid Chromatography (HPLC)
Separation of Nutraceuticals”, Joaudimir
Castro, Jacob L.
Venzie, R. Kenneth Marcus, presented at the 2006 Pittsburgh Conference on
Analytical Chemistry and Applied Spectroscopy, Orlando, FL, March 12 - 17,
2006.
“Nutraceutical/Botanical
Products: Challenges for Producers, Regulators, and (Mostly) Analytical
Chemists”, R.
Kenneth Marcus, Jacob L. Venzie, Joaudimir Castro, Timothy M. Brewer, and
M.V. Balarama Krishna, presented at the 2006 Pittsburgh Conference on
Analytical Chemistry and Applied Spectroscopy, Orlando, FL, March 12 - 17,
2006.
“Nutraceutical/Botanical
Products: Challenges for Producers, Regulators, and (Mostly) Analytical
Chemists”, R.
Kenneth Marcus, Jacob L. Venzie, Joaudimir Castro, Timothy M. Brewer, and
M.V. Balarama Krishna, presented at the 2006 Winter Conference on Plasma
Spectrochemistry, Tucson, AZ. January 8-13, 2006.
Posters
“Evaluation of Biological Fluids via Liquid
Chromatography Particle Beam Mass Spectrometry (LC-PB/MS)”, Joaudimir
Castro, Carolyn E. Quarles, and R. Kenneth Marcus, presented at the 2010
Winter Conference on Plasma Spectrochemistry, Fort Myers, FL, January 4-9, 2010.
“Isoflavone Composition Analysis via Liquid
Chromatography-Particle Beam/Mass Spectrometry (LC-PB/MS)”, Carolyn
E. Quarles, Joaudimir
Castro, Kristina Chumanov and R. Kenneth Marcus, presented at the 2010 Winter
Conference on Plasma Spectrochemistry, Fort Myers, FL, January 4-9, 2010.
“Determination of Caffeine and Catechin
Species in Green Tea Extracts by Liquid Chromatography-Particle Beam Mass
Spectrometry”, Joaudimir
Castro, Tara Pregibon, and R. Kenneth Marcus, presented at the 2009
SEAGEP Student Conference, Charleston, SC., May 19-21, 2009.
“Validation of Green Tea Extracts by
Liquid Chromatography-Particle Beam/Electron Ionization Mass Spectrometry
(LC-PB/EIMS)”,Tara
Pregibon, Joaudimir
Castro, and R. Kenneth Marcus, presented at the 2009 Pittsburgh Conference on
Analytical Chemistry and Applied Spectroscopy, Chicago, IL, March 8-12, 2009.
“Chemical Characterization of Botanical
Products by Liquid Chromatography Particle Beam/Mass Spectrometry (LC-PB/MS)”, J. Castro, M.V.B. Krishna, and R.K. Marcus,
presented at the 2008 SEAGEP Student Conference, Gainesville, FL, May 12-14,
2008.
“Comprehensive speciation analysis of selenium in
garlic through liquid chromatography-particle beam/electron impact mass
spectrometry”, G. Ojeda Torres, J. Castro, M.V.B. Krishna, and R.K.
Marcus, presented at the 235th ACS National Meeting, New Orleans, LA, United
States, April 6-10, 2008.
“Liquid Chromatography Particle Beam/Mass Spectrometry
(HPLC-PB/MS) Analysis of Nutraceuticals Using Electron Impact and Glow
Discharge Ionization Sources”,
Joaudimir Castro, M. V. Balarama Krishna, John R. Choiniere,
“High Performance Liquid
Chromatography-Particle Beam/Glow Discharge-Mass Spectrometry (HPLC-PB/GDMS)
Analysis of Green Tea Extract”,
J. Castro, J. L. Venzie, M.V.B. Krishna and R. K. Marcus, presented at
the 2006 CAEFF Student Retreat, Charleston, SC. August 18-20, 2006.
“High Performance Liquid
Chromatography-Particle Beam/Glow Discharge-Mass Spectrometry (HPLC-PB/GDMS)
Analysis of Green Tea Extract”, J.
Castro, J. L. Venzie,
M.V.B. Krishna and R. K. Marcus, presented at the 2006 SEAGEP Student
Conference, Clemson, SC. April 17-19, 2006.
“High Performance Liquid
Chromatography-Particle Beam/Glow Discharge-Mass Spectrometry (HPLC-PB/GDMS)
Analysis of Green Tea Extract”,
J. Castro, J.L. Venzie, M.V.B. Krishna and R.K. Marcus, presented at the
2006 Winter Conference on Plasma Spectrochemistry, Tucson, AZ. January
8-13, 2006.
“Development
and Use of an Inductively Coupled Plasma Atomic Emission Spectrometry Method
for Analysis of Heavy Metals in Commercial Botanical Supplements”, Julia E. Cooper, Joaudimir Castro,
and R. Kenneth Marcus, presented at the 2006 Winter Conference on Plasma
Spectrochemistry,
“Community Interaction Student-Affiliates Project:
The magic of chemistry and something else”, Barbra M. Ramirez, Joaudimir Castro, and Ingrid
Montes, presented at the 227th ACS National Meeting, Anaheim, CA, United
States, March 28-April 1, 2004.
E-mail:
jcastro@clemson.edu
Phone:
864-656-0996
Fax:
864-656-0567
Joy Castro
Clemson University
Department of Chemistry
219 Hunter Laboratories