Dr. Robert  Channon  Md image

Dr. Robert Channon Md

2525 S Michigan Ave B-390
Chicago IL 60616
312 676-6691
Medical School: Other - Unknown
Accepts Medicare: No
Participates In eRX: No
Participates In PQRS: No
Participates In EHR: No
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NPI: 1568445146
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Electrochemical flow injection analysis of hydrazine in an excess of an active pharmaceutical ingredient: achieving pharmaceutical detection limits electrochemically. - Analytical chemistry
The quantification of genotoxic impurities (GIs) such as hydrazine (HZ) is of critical importance in the pharmaceutical industry in order to uphold drug safety. HZ is a particularly intractable GI and its detection represents a significant technical challenge. Here, we present, for the first time, the use of electrochemical analysis to achieve the required detection limits by the pharmaceutical industry for the detection of HZ in the presence of a large excess of a common active pharmaceutical ingredient (API), acetaminophen (ACM) which itself is redox active, typical of many APIs. A flow injection analysis approach with electrochemical detection (FIA-EC) is utilized, in conjunction with a coplanar boron doped diamond (BDD) microband electrode, insulated in an insulating diamond platform for durability and integrated into a two piece flow cell. In order to separate the electrochemical signature for HZ such that it is not obscured by that of the ACM (present in excess), the BDD electrode is functionalized with Pt nanoparticles (NPs) to significantly shift the half wave potential for HZ oxidation to less positive potentials. Microstereolithography was used to fabricate flow cells with defined hydrodynamics which minimize dispersion of the analyte and optimize detection sensitivity. Importantly, the Pt NPs were shown to be stable under flow, and a limit of detection of 64.5 nM or 0.274 ppm for HZ with respect to the ACM, present in excess, was achieved. This represents the first electrochemical approach which surpasses the required detection limits set by the pharmaceutical industry for HZ detection in the presence of an API and paves the wave for online analysis and application to other GI and API systems.
Examination of the factors affecting the electrochemical performance of oxygen-terminated polycrystalline boron-doped diamond electrodes. - Analytical chemistry
In order to produce polycrystalline oxygen-terminated boron-doped diamond (BDD) electrodes suitable for electroanalysis (i.e., widest solvent window, lowest capacitive currents, stable and reproducible current responses, and capable of demonstrating fast electron transfer) for outer sphere redox couples, the following factors must be considered. The material must contain enough boron that the electrode shows metal-like conductivity; electrical measurements demonstrate that this is achieved at [B] > 10(20) B atoms cm(-3). Even though BDD contains a lower density of states than a metal, it is not necessary to use extreme doping levels to achieve fast heterogeneous electron transfer (HET). An average [B] ~ 3 × 10(20) B atoms cm(-3) was found to be optimal; increasing [B] results in higher capacitive values and increases the likelihood of nondiamond carbon (NDC) incorporation. Hydrogen-termination causes a semiconducting BDD electrode to behave metal-like due to the additional surface conductivity hydrogen termination brings. Thus, unless [B] of the material is known, the electrical properties of the electrode may be incorrectly interpreted. Note, this layer (formed on a lapped electrode) is electrochemically unstable, an effect which is exacerbated at increased potentials. It is essential during growth that NDC is minimized as it acts to increase capacitive currents and decrease the solvent window. We found complete removal of NDC after growth using aggressive acid cleans, acid cycling, and diamond polishing impossible. Although hydrogen termination can mask the NDC signature in the solvent window and lower capacitive currents, this is not a practical procedure for improving sensitivity in electroanalysis. Finally, alumina polishing of lapped, NDC free, freestanding, BDD electrodes was found to be an effective way to produce well-defined, stable, and reproducible surfaces, which support fast (reversible) HET for Fe(CN)6(4-) electrolysis, the first time this has been reported at an oxygen-terminated surface.

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