Optimization of two methods for the analysis of hydrogen peroxide: High performance liquid chromatography with fluorescence detection and high performance liquid chromatography with electrochemical detection in direct current mode

Two complementary methods were optimized for the separation and detection of trace levels of hydrogen peroxide. The first method utilized reversed-phase high-performance liquid chromatography with fluorescence detection (HPLC–FD). With this approach, hydrogen peroxide was detected based upon its par...

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Published in:	Journal of Chromatography A Vol. 1217; no. 48; pp. 7564 - 7572
Main Authors:	Tarvin, Megan, McCord, Bruce, Mount, Kelly, Sherlach, Katy, Miller, Mark L.
Format:	Journal Article
Language:	English
Published:	Amsterdam Elsevier B.V 26-11-2010 Amsterdam; New York: Elsevier Elsevier
Subjects:	Analytical chemistry Chemistry Chromatographic methods and physical methods associated with chromatography Chromatography, High Pressure Liquid - instrumentation Chromatography, High Pressure Liquid - methods Electrochemical detection Electrochemistry Exact sciences and technology Fluorescence Fluorescence detection HPLC Hydrogen peroxide Hydrogen Peroxide - analysis Other chromatographic methods Hydrogen peroxide Electrochemical detection HPLC Fluorescence detection Trace analysis Fluorescence detector Chemical analysis HPLC chromatography Explosions Derivatization Optimization Postcolumn Electrochemical detector Reversed phase chromatography Hemin Residue Metalloporphyrin Quantitative analysis
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Abstract	Two complementary methods were optimized for the separation and detection of trace levels of hydrogen peroxide. The first method utilized reversed-phase high-performance liquid chromatography with fluorescence detection (HPLC–FD). With this approach, hydrogen peroxide was detected based upon its participation in the hemin-catalyzed oxidation of p-hydroxyphenylacetic acid to yield the fluorescent dimer. The second method utilized high performance liquid chromatography with electrochemical detection (HPLC–ED). With this approach, hydrogen peroxide was detected based upon its oxidation at a gold working electrode at an applied potential of 400 mV vs. hydrogen reference electrode (Pd/H 2). Both methods were linear across the range of 15–300 μM, and the electrochemical method was linear across a wider range of 7.4–15,000 μM. The limit of detection for hydrogen peroxide was 6 μM by HPLC/FD, and 0.6 μM by HPLC/ED. A series of organic peroxides and inorganic ions were evaluated for their potential to interfere with the detection of hydrogen peroxide. Studies investigating the recovery of hydrogen peroxide with three different extraction protocols were also performed. Post-blast debris from the detonation of a mixture of concentrated hydrogen peroxide with nitromethane was analyzed on both systems. Hydrogen peroxide residues were successfully detected on this post-blast debris.
AbstractList	Two complementary methods were optimized for the separation and detection of trace levels of hydrogen peroxide. The first method utilized reversed-phase high-performance liquid chromatography with fluorescence detection (HPLC-FD). With this approach, hydrogen peroxide was detected based upon its participation in the hemin-catalyzed oxidation of p-hydroxyphenylacetic acid to yield the fluorescent dimer. The second method utilized high performance liquid chromatography with electrochemical detection (HPLC-ED). With this approach, hydrogen peroxide was detected based upon its oxidation at a gold working electrode at an applied potential of 400mV vs. hydrogen reference electrode (Pd/H₂). Both methods were linear across the range of 15-300μM, and the electrochemical method was linear across a wider range of 7.4-15,000μM. The limit of detection for hydrogen peroxide was 6μM by HPLC/FD, and 0.6μM by HPLC/ED. A series of organic peroxides and inorganic ions were evaluated for their potential to interfere with the detection of hydrogen peroxide. Studies investigating the recovery of hydrogen peroxide with three different extraction protocols were also performed. Post-blast debris from the detonation of a mixture of concentrated hydrogen peroxide with nitromethane was analyzed on both systems. Hydrogen peroxide residues were successfully detected on this post-blast debris. Two complementary methods were optimized for the separation and detection of trace levels of hydrogen peroxide. The first method utilized reversed-phase high-performance liquid chromatography with fluorescence detection (HPLC-FD). With this approach, hydrogen peroxide was detected based upon its participation in the hemin-catalyzed oxidation of p-hydroxyphenylacetic acid to yield the fluorescent dimer. The second method utilized high performance liquid chromatography with electrochemical detection (HPLC-ED). With this approach, hydrogen peroxide was detected based upon its oxidation at a gold working electrode at an applied potential of 400 mV vs. hydrogen reference electrode (Pd/H(2)). Both methods were linear across the range of 15-300 μM, and the electrochemical method was linear across a wider range of 7.4-15,000 μM. The limit of detection for hydrogen peroxide was 6 μM by HPLC/FD, and 0.6 μM by HPLC/ED. A series of organic peroxides and inorganic ions were evaluated for their potential to interfere with the detection of hydrogen peroxide. Studies investigating the recovery of hydrogen peroxide with three different extraction protocols were also performed. Post-blast debris from the detonation of a mixture of concentrated hydrogen peroxide with nitromethane was analyzed on both systems. Hydrogen peroxide residues were successfully detected on this post-blast debris. Two complementary methods were optimized for the separation and detection of trace levels of hydrogen peroxide. The first method utilized reversed-phase high-performance liquid chromatography with fluorescence detection (HPLC–FD). With this approach, hydrogen peroxide was detected based upon its participation in the hemin-catalyzed oxidation of p-hydroxyphenylacetic acid to yield the fluorescent dimer. The second method utilized high performance liquid chromatography with electrochemical detection (HPLC–ED). With this approach, hydrogen peroxide was detected based upon its oxidation at a gold working electrode at an applied potential of 400 mV vs. hydrogen reference electrode (Pd/H 2). Both methods were linear across the range of 15–300 μM, and the electrochemical method was linear across a wider range of 7.4–15,000 μM. The limit of detection for hydrogen peroxide was 6 μM by HPLC/FD, and 0.6 μM by HPLC/ED. A series of organic peroxides and inorganic ions were evaluated for their potential to interfere with the detection of hydrogen peroxide. Studies investigating the recovery of hydrogen peroxide with three different extraction protocols were also performed. Post-blast debris from the detonation of a mixture of concentrated hydrogen peroxide with nitromethane was analyzed on both systems. Hydrogen peroxide residues were successfully detected on this post-blast debris.
Author	Sherlach, Katy Mount, Kelly Miller, Mark L. McCord, Bruce Tarvin, Megan
Author_xml	– sequence: 1 givenname: Megan surname: Tarvin fullname: Tarvin, Megan organization: CFSRU, Visiting Scientist Program, Federal Bureau of Investigation Laboratory, Quantico, VA, USA – sequence: 2 givenname: Bruce surname: McCord fullname: McCord, Bruce organization: Department of Chemistry, Florida International University, Miami, FL, USA – sequence: 3 givenname: Kelly surname: Mount fullname: Mount, Kelly organization: EU, Federal Bureau of Investigation Laboratory, Quantico, VA, USA – sequence: 4 givenname: Katy surname: Sherlach fullname: Sherlach, Katy organization: CFSRU, Federal Bureau of Investigation Laboratory, Quantico, VA, USA – sequence: 5 givenname: Mark L. surname: Miller fullname: Miller, Mark L. email: Mark.L.Miller@IC.FBI.GOV organization: CFSRU, Federal Bureau of Investigation Laboratory, Quantico, VA, USA
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Keywords	Hydrogen peroxide Electrochemical detection HPLC Fluorescence detection Trace analysis Fluorescence detector Chemical analysis HPLC chromatography Explosions Derivatization Optimization Postcolumn Electrochemical detector Reversed phase chromatography Hemin Residue Metalloporphyrin Quantitative analysis
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Snippet	Two complementary methods were optimized for the separation and detection of trace levels of hydrogen peroxide. The first method utilized reversed-phase...
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SubjectTerms	Analytical chemistry Chemistry Chromatographic methods and physical methods associated with chromatography Chromatography, High Pressure Liquid - instrumentation Chromatography, High Pressure Liquid - methods Electrochemical detection Electrochemistry Exact sciences and technology Fluorescence Fluorescence detection HPLC Hydrogen peroxide Hydrogen Peroxide - analysis Other chromatographic methods
Title	Optimization of two methods for the analysis of hydrogen peroxide: High performance liquid chromatography with fluorescence detection and high performance liquid chromatography with electrochemical detection in direct current mode
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