ISSN print edition: 0366-6352 ISSN electronic edition: 1336-9075 Registr. No.: MK SR 9/7 Published monthly

Analytical validation of a microwave-assisted ICP-MS method for the quantification of elemental impurities in doxycycline hyclate tablets

Tirth V. Shah, Sneha R. Sagar, Sujal Shah, Anirban Roy Chowdhury, Tushar Mehta, and Dilip G. Maheshwari

Department of Quality Assurance, L.J. Institute of Pharmacy, L J University, Ahmedabad, India

E-mail: dgmaheshwari@gmail.com

Received: 14 May 2023  Accepted: 23 February 2024

Abstract:

Elemental impurities are generated in pharmaceuticals at various stages of the manufacturing process and storage. The presence of elemental impurities in pharmaceuticals may lead to severe health complications. In this work, the presence of elemental impurities was determined in doxycycline hyclate tablets using microwave-assisted sample preparation. Concentrated nitric acid (70%) and hydrofluoric acid (47–51%) were used for the preparation of sample solution. Spike recovery experiments were performed using a matrix to detect class 1 (As, Cd, Hg, and Pb) and class 2A (Co, V and Ni) elements in a single analysis. The developed ICP-MS method was validated using different analytical parameters, i.e. specificity, linearity, precision (system precision and method precision), accuracy, limit of detection (LOD) and limit of quantitation (LOQ). All the experimental results demonstrated that the developed ICP-MS method is suitable for the simple and sensitive analysis of trace elements in doxycycline hyclate tablets.

Graphical abstract

Keywords: ICP-MS; Doxycycline hyclate tablets; Elemental impurities; Microwave-assisted digestion; Method validation

Full paper is available at www.springerlink.com.

DOI: 10.1007/s11696-024-03385-7

Chemical Papers 78 (8) 4661–4669 (2024)