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

Autor(es)

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

• Tipo de documento: Artigo Científico
• Fonte: JOURNAL OF SEPARATION SCIENCE; v. 46, n. 17, p. 13-pg., 2023-07-03.

Resumo

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)

• Processo FAPESP: 15/15462-5 - Emprego do grafeno como material sorvente em técnicas miniaturizadas de preparo de amostra.
• Beneficiário: Bruno Henrique Fumes
• Modalidade de apoio: Bolsas no Brasil - Doutorado
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• Beneficiário: Deyber Arley Vargas Medina
• Modalidade de apoio: Bolsas no Brasil - Pós-Doutorado
• Processo FAPESP: 17/02147-0 - Cromatografia líquida em uma gota e seu acoplamento com espectrometria de massas: estratégias instrumentais, desenvolvimento de materiais, automatização e aplicações analíticas
• Beneficiário: Fernando Mauro Lanças
• Modalidade de apoio: Auxílio à Pesquisa - Temático
• Processo FAPESP: 14/07347-9 - Desenvolvimento de novos materiais e dispositivos para técnicas miniaturizadas de preparo de amostras na área de segurança alimentar
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• Modalidade de apoio: Auxílio à Pesquisa - Regular
• Processo FAPESP: 19/26263-4 - Desenvolvimento de colunas capilares tubulares abertas para micro e nano cromatografia líquida acopladas a espectroscopia de massas sequencial
• Beneficiário: Natalia Gabrielly Pereira dos Santos
• Modalidade de apoio: Bolsas no Brasil - Doutorado Direto