  Citation: Allen, R.C. Haloperoxidase-Catalyzed Luminol Luminescence. Antioxidants 2022, 11, 518. https://doi.org/10.3390/ antiox11030518 Academic Editor: Ernst Malle Received: 27 January 2022 Accepted: 4 March 2022 Published: 8 March 2022 Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in published maps and institutional affil- iations. Copyright: © 2022 by the author. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https:// creativecommons.org/licenses/by/ 4.0/). antioxidants Article Haloperoxidase-Catalyzed Luminol Luminescence Robert C. Allen Department of Pathology, Creighton University, Omaha, NE 68178, USA; robertallen@creighton.edu; Tel.: +1-402-350-3193 Abstract: Common peroxidase action and haloperoxidase action are quantifiable as light emission from dioxygenation of luminol (5-amino-2,3-dihydrophthalazine-1,4-dione). The velocity of enzyme action is dependent on the concentration of reactants. Thus, the reaction order of each participant reactant in luminol luminescence was determined. Horseradish peroxidase (HRP)-catalyzed luminol luminescence is first order for hydrogen peroxide (H 2 O 2 ), but myeloperoxidase (MPO) and eosinophil peroxidase (EPO) are second order for H 2 O 2 . For MPO, reaction is first order for chloride (Cl - ) or bromide (Br - ). For EPO, reaction is first order for Br - . HRP action has no halide requirement. For MPO and EPO, reaction is first order for luminol, but for HRP, reaction is greater than first order for luminol. Haloperoxidase-catalyzed luminol luminescence requires acidity, but HRP action requires alkalinity. Unlike the radical mechanism of common peroxidase, haloperoxidases (XPO) catalyze non-radical oxidation of halide to hypohalite. That reaction is second order for H 2 O 2 is consistent with the non-enzymatic reaction of hypohalite with a second H 2 O 2 to produce singlet molecular oxygen ( 1 O 2 *) for luminol dioxygenation. Alternatively, luminol dehydrogenation by hypohalite followed by reaction with H 2 O 2 yields dioxygenation consistent with the same reaction order. Haloperoxidase action, Cl - , and Br - are specifically quantifiable as luminol luminescence in an acidic milieu. Keywords: haloperoxidase; myeloperoxidase; eosinophil peroxidase; horseradish peroxidase; halide oxidation; singlet molecular oxygen; luminol luminescence; chemiluminescence; reaction order; kinetic analysis 1. Introduction Myeloperoxidase (MPO) enzymatic action produces light emission or chemilumi- nescence. Such luminescence is native, i.e., no chemiluminigenic substrate is needed, requires H 2 O 2 , halide, and acidic pH [1,2], and correlates with the requirements for MPO microbe killing described by Klebanoff [3]. Both luminescence and microbicidal action are hydrogen peroxide (H 2 O 2 ), chloride (Cl - ), and acid-dependent. Light emission implies haloperoxidase-catalyzed combustive oxygenation. MPO catalyzes H 2 O 2 oxidization of halide to hypohalite, e.g., Cl - oxidation to hypochlorite (OCl - ). The non-enzymatic reac- tion of hypohalite with a second H 2 O 2 produces electronically excited singlet molecular oxygen ( 1 O 2 *) [46]. Both H 2 O 2 and OCl - are singlet multiplicity reactants necessitating a single multiplicity product [7,8]. The relaxation of 1 O 2 * to its triplet ground state ( 3 O 2 ) requires intersystem crossing, and as such, 1 O 2 * has about a microsecond lifetime [9,10]. This lifetime is sufficient for reactivity, but such reaction is restricted to within a radius of about 0.3 microns (micrometer) of its nascence. Spin conservation and frontier orbital considerations restrict the direct reaction of ground-state triplet multiplicity oxygen ( 3 O 2 ) with singlet multiplicity biomolecules. Thus, combustion is not spontaneous, and the large exergonicity that would result from such action is unrealized. Spin and frontier orbital considerations do not limit 1 O 2 * reaction with biomolecules. The electrophilic reactivity of 1 O 2 * drives oxygenation of organic molecules, and a fraction of the reaction products will have electronically excited singlet multiplicity carbonyl functions that relax by emitting photons in the visible spectrum. Antioxidants 2022, 11, 518. https://doi.org/10.3390/antiox11030518 https://www.mdpi.com/journal/antioxidants