Optimization and validation of a fast Supercritical Fluid Chromatography method for the quantitative determination of vitamin D3 and its related impurities.
SFC; Green analytical Chemistry; vitamin D3; method validation; accuracy profile; Design space
Abstract :
[en] In the uprising context of green analytical chemistry, Supercritical Fluid Chromatography (SFC) is often suggested as an alternative to Normal Phase Liquid Chromatography. Indeed, SFC provides fast, efficient and green separations. In this report, the quantitative performances of SFC were challenged on a real-life case study: the Quality Control (QC) of vitamin D3. A rapid and green SFC method was optimized thanks to the Design of Experiments–Design Space (DoE–DS) methodology. It provided robust and high quality separation of the compounds within a 2 min timeframe, using a gradient of ethanol as co-solvent of the carbon dioxide. The analytical method was fully validated according to the total error approach, demon- strating the compliance of the method to the specifications of U.S. Pharmacopeia (USP: 97.0–103.0%) and European Pharmacopeia (EP: 97.0–102.0%) for an interval of [50–150%] of the target concentration. In order to allow quantification of impurities using vitamin D3 as an external standard in SFC-UV, correction factors were determined and verified during method validation. Thus, accurate quantification of impu- rities was demonstrated at the specified levels (0.1 and 1.0% of the main compound) for a 70.0–130.0% dosing range. This work demonstrates the validity of an SFC method for the QC of vitamin D3 raw material and its application to real samples. Therefore, it supports the switch to a greener and faster separative technique as an alternative to NPLC in the pharmaceutical industry.
Research Center/Unit :
CIRM - Centre Interdisciplinaire de Recherche sur le Médicament - ULiège
Disciplines :
Pharmacy, pharmacology & toxicology Chemistry
Author, co-author :
Andri, Bertyl ; Université de Liège > Département de pharmacie > Chimie analytique
Lebrun, Pierre ; Université de Liège > Département de pharmacie > Chimie analytique
Dispas, Amandine ; Université de Liège > Département de pharmacie > Chimie analytique
Klinkenberg, Régis; Galephar research center M/F
Streel, Bruno; Galephar research center M/F
Ziemons, Eric ; Université de Liège > Département de pharmacie > Département de pharmacie
Hubert, Philippe ; Université de Liège > Département de pharmacie > Chimie analytique
Language :
English
Title :
Optimization and validation of a fast Supercritical Fluid Chromatography method for the quantitative determination of vitamin D3 and its related impurities.
Publication date :
2017
Journal title :
Journal of Chromatography. A
ISSN :
0021-9673
eISSN :
1873-3778
Publisher :
Elsevier Science, Amsterdam, Netherlands
Special issue title :
Selected paper from 31st International Symposium on Chromatography (ISC2016), 28 August - 1 September 2016, Cork, Ireland.
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