Microextraction by packed sorbent of N-nitrosamines from Losartan tablets using a high-throughput robot platform followed by liquid chromatography-tandem mass spectrometry

Author(s)

dos Santos, Natalia Gabrielly ; Medina, Deyber Arley Vargas ; Lancas, Fernando Mauro

• Document type: Journal article
• Source: JOURNAL OF SEPARATION SCIENCE; v. 46, n. 17, p. 13-pg., 2023-07-03.

Abstract

The development of a fast, cost-effective, and efficient microextraction by packed sorbent setup was achieved by combining affordable laboratory-repackable devices of microextraction with a high-throughput cartesian robot. This setup was evaluated for the development of an analytical method to determine N-nitrosamines in losartan tablets. N-nitrosamines pose a significant concern in the pharmaceutical market due to their carcinogenic risk, necessitating their control and quantification in pharmaceutical products. The parameters influencing the performance of this sample preparation for N-nitrosamines were investigated through both univariate and multivariate experiments. Microextractions were performed using just 5.0 mg of carboxylic acid-modified polystyrene divinylbenzene copolymer as the extraction phase. Under the optimized conditions, the automated setup enabled the simultaneous treatment of six samples in less than 20 min, providing reliable analytical confidence for the proposed application. The analytical performance of the automated high-throughput microextraction by the packed sorbent method was evaluated using a matrix-matching calibration. Quantification was performed using ultra-high-performance liquid chromatography-tandem mass spectrometry with chemical ionization at atmospheric pressure. The method exhibited limits of detection as low as 50 ng/g, good linearity, and satisfactory intra-day (1.38-18.76) and inter-day (2.66-20.08) precision. Additionally, the method showed accuracy ranging from 80% to 136% for these impurities in pharmaceutical formulations. (AU)

• FAPESP's process: 15/15462-5 - Employment of graphene as sorbent in miniaturized sample preparation techniques.
• Grantee: Bruno Henrique Fumes
• Support Opportunities: Scholarships in Brazil - Doctorate
• FAPESP's process: 19/22724-7 - Novel instrumental approaches for automated and miniaturized analytical methods for the detection of organic compounds by liquid chromatography coupled to mass spectrometry
• Grantee: Deyber Arley Vargas Medina
• Support Opportunities: Scholarships in Brazil - Post-Doctoral
• FAPESP's process: 17/02147-0 - Single drop chromatography and its coupling to mass spectrometry: instrumental strategies, development of materials, automation and analytical applications
• Grantee: Fernando Mauro Lanças
• Support Opportunities: Research Projects - Thematic Grants
• FAPESP's process: 14/07347-9 - Development of novel materials and devices for miniaturized sample preparation techniques in the area of food safety
• Grantee: Fernando Mauro Lanças
• Support Opportunities: Regular Research Grants
• FAPESP's process: 19/26263-4 - Development of open tubular capillary columns for micro and nano liquid chromatography coupled to sequential mass spectroscopy
• Grantee: Natalia Gabrielly Pereira dos Santos
• Support Opportunities: Scholarships in Brazil - Doctorate (Direct)