Sequential design of experiments approach for the multiproduct analysis of cholesterol-lowering drugs by ultra-high-performance supercritical fluid chromatography

Autor(es)

Santana, Igor Miranda ^[1] ; Jardim, Isabel Cristina Sales Fontes ^[1] ; Breitkreitz, Marcia Cristina ^[1]

Afiliação do(s) autor(es)

^[1] Univ Estadual Campinas, Inst Chem, Dept Analyt Chem, Campinas, SP - Brazil

• Tipo de documento: Artigo Científico
• Fonte: JOURNAL OF SEPARATION SCIENCE; OCT 2020.
• Citações Web of Science: 0

Resumo

A multiproduct approach toward method development is presented for a fast and reliable analysis of the eight most important cholesterol-lowering drugs via ultra-high-performance supercritical fluid chromatography. A two-step approach based on design of experiments was applied: (1) selection of the stationary phase, organic modifier, and diluent in the mobile phase through a multilevel categorical design and (2) optimization of the elution strength by varying the pressure, temperature, and gradient using a central composite design. Finally, the flow rate was adjusted. The first design selected UPC(2)Torus 1-AA as the column, ethanol:water as the organic modifier, and acetonitrile:ethanol 3:2 v/v as the diluent. The results led to a pressure, column temperature, and gradient elution of 14.83 MPa, 42 degrees C, and 5-15.5% of ethanol:water in CO2, respectively. The flow rate was set at 1.8 mL/min, providing a total analysis time of 4 min. This multiproduct method was validated and applied to 11 different commercial products available in the Brazilian market, and it was found to be accurate, withr> 0.990, recoveries between 95 and 105%, and precision not higher than 5.4%. Therefore, this method was shown to be a greener alternative for the analysis of these pharmaceuticals. (AU)

• Processo FAPESP: 16/05636-9 - Desenvolvimento de métodos analíticos inovadores para analitos de interesse farmacêutico empregando cromatografia com fluído supercrítico de ultra alta eficiência (UHPSFC) em associação com ferramentas quimiométricas
• Beneficiário: Márcia Cristina Breitkreitz
• Modalidade de apoio: Auxílio à Pesquisa - Regular