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Anal Bioanal Chem ; 411(6): 1219-1228, 2019 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-30617392

RESUMEN

A fully automated method for the determination of lovastatin in dietary supplements containing red yeast rice has been developed. It uses a sequential injection analysis system combined with solid-phase extraction applying highly selective molecularly imprinted polymer sorbent. A miniaturized column for on-line extraction was prepared by packing 4.5 mg of the sorbent in a 5.0 × 2.5-mm-i.d. cartridge, which was used in the flow manifold. Sequential injection analysis manifold enabled all steps of lovastatin extraction and continuous spectrophotometric detection at 240 nm. A limit of detection of 60 µg g-1, a limit of quantitation of 200 µg g-1, and a linear calibration range of 200-2000 µg g-1 were achieved. Intra-day and inter-day precision values (RSD) were ≤ 6.7% and ≤ 4.9%, respectively, and method recovery values of spiked red yeast rice extracts at 200, 1000, and 2000 µg g-1 concentration levels were 82.9, 95.2, and 87.7%. Our method was used for determination of lovastatin lactone in four dietary supplements containing red yeast rice as a natural source of lovastatin, also known as monacolin K. The extracted samples were subsequently analyzed by the reference UHPLC-MS/MS method. Statistical comparison of results (F test, t test, α = 0.05) obtained by both methods did not reveal significant difference. A substantial advantage of the new automated approach is high sample throughput thanks to the analysis time of 7.5 min, miniaturization via down-scaling the extraction column, and smaller sample and solvent consumption, as well as reduced generation of waste. Graphical abstract ᅟ.


Asunto(s)
Anticolesterolemiantes/análisis , Productos Biológicos/análisis , Suplementos Dietéticos/análisis , Lovastatina/análisis , Impresión Molecular/métodos , Extracción en Fase Sólida/métodos , Cromatografía Líquida de Alta Presión/instrumentación , Cromatografía Líquida de Alta Presión/métodos , Diseño de Equipo , Análisis de Inyección de Flujo/instrumentación , Análisis de Inyección de Flujo/métodos , Límite de Detección , Impresión Molecular/instrumentación , Polímeros/química , Extracción en Fase Sólida/instrumentación , Espectrofotometría Ultravioleta/instrumentación , Espectrofotometría Ultravioleta/métodos , Espectrometría de Masas en Tándem/instrumentación , Espectrometría de Masas en Tándem/métodos
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