Sequential design of experiments approach for the multiproduct analysis of cholesterol-lowering drugs by ultra-high-performance supercritical fluid chromatography.
J Sep Sci
; 43(22): 4234-4242, 2020 Nov.
Article
em En
| MEDLINE
| ID: mdl-32951322
ABSTRACT
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 UPC2 Torus 1-AA as the column, ethanolwater as the organic modifier, and acetonitrileethanol 32 v/v as the diluent. The results led to a pressure, column temperature, and gradient elution of 14.83 MPa, 42°C, and 5-15.5% of ethanolwater 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, with r > 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.
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Texto completo:
1
Coleções:
01-internacional
Base de dados:
MEDLINE
Assunto principal:
Colesterol
Idioma:
En
Revista:
J Sep Sci
Ano de publicação:
2020
Tipo de documento:
Article
País de afiliação:
Brasil
País de publicação:
ALEMANHA
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ALEMANIA
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DE
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DEUSTCHLAND
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GERMANY