Analytical Research Forum 2022 - Book of abstracts

Rapid separation of tetracaine and oxymetazoline in pharmaceuticals via liquid chromatography with electrochemical detection at a boron-doped diamond electrode Huda Alghamdi, Majidah Alsaeedi, Phyllis E. Hayes, and Jeremy D. Glennon Innovative Chromatography Group, Irish Separation Science Cluster (ISSC), Ireland 113220126@umail.ucc.ie Tetracaine hydrochloride (TCH) is a nasal anesthetic that is used to perform dental restorative procedures and an ocular anesthetic for topical instillation into the conjunctiva. Oxymetazoline hydrochloride (OZH) is a nasal decongestant which relieves a stuffy nose. When it is included in nasal solutions that also contain TCH it narrows blood vessels, resulting in the enhanced efficacy and action duration of TCH. However, a moderate to acute overdosage of OZH and TCH can lead to mydriasis, nausea, cyanosis, tachycardia, cardiovascular failure, disorientation, seizures, and even death. TCH and OZH have also been found to act as micropollutants in natural waters, with long-term effects on living systems. Liquid chromatography (LC) has been mainly utilized for the determination of either TCH or OZH; however, there is a need for rapid and efficient methods for simultaneous analysis in pharmaceutical Preparations and aqueous samples. This study investigates the use of a liquid chromatography (LC) equipped with electrochemical detection (ECD) for the simultaneous determination of TCH and OZH by utilizing the fast separation of core-shell silica particles coupled with the boron-doped diamond (BDD) electrodes sensitivity. Rapid reversed-phase (RP) separation was achieved within 45 sec using a core- shell column, by adjusting the ratio of organic solvent, mobile phase pH, detection potential and mobile phase flow rate. Sensitivity was compared using ultraviolet (UV) detection at 280 nm, and ECD at + 1.3 V with detection limits of 40 and 70 nM for TCH and OZH, respectively. The proposed method was utilized successfully in the analysis of pharmaceutical Preparations, where the estimated levels of TCH and OZH in these Preparations are in agreement with the specified values outlined by the manufacturers. References 1. J. Capetillo, M. Drum, A. Reader, S. Fowler, J. Nusstein, M. Beck, Anesthetic efficacy of intranasal 3% tetracaine plus 0.05% oxymetazoline (Kovanaze) in maxillary teeth, J. Endod. 45(3) (2019) 257-262. 2. P.N. Kulkarni, A.M. Dodake-Supekar, A.S. Nipte, C.K. Jadhav, C.H. Gill, Analytical method development and validation for anti asthamatic drug oxymetazoline hydrochloride in nasal spray formulations by rp-hplc, J. Drug Deliv. Ther. 9(4-A) (2019) 505-510. 3. J.O. Abdulsattar, H. Hadi, S. Richardson, A. Iles, N. Pamme, Detection of doxycycline hyclate and oxymetazoline hydrochloride in pharmaceutical preparations via spectrophotometry and microfluidic paper-based analytical device (μPADs), Anal. Chim. Acta 1136 (2020) 196-204.

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