Generic SFC-MS methodology for the quality control of vitamin D3 oily formulations

• Published in: Journal of pharmaceutical and biomedical analysis Vol. 209; p. 114492
• Main Authors: Jambo, Hugues, Dispas, Amandine, Hubert, Cédric, Lecomte, Frédéric, Ziemons, Éric, Hubert, Philippe
• Format: Journal Article Web Resource
• Language: English
• Published: Elsevier B.V 05.02.2022; Elsevier
• Subjects: Food supplements; Human health sciences; Medicines; Pharmacie, pharmacologie & toxicologie; Pharmacy, pharmacology & toxicology; Quality control; Routine analysis; Sciences de la santé humaine; SFC-MS; Vitamin D3; SFC-MS; Vitamin D3; Routine analysis; Medicines; Food supplements; Quality control
• ISSN: 0731-7085; 1873-264X; 1873-264X
• DOI: 10.1016/j.jpba.2021.114492

•Use of SFC in routine analysis for the QC of medicines and food supplements.•“Dilute-and-shoot” approach as preparation technique for complex samples in SFC.•Matrix effect was monitored and compared between different types of oily matrices.•Implementation of a control strategy based on a three-level SST.•Differences in manufacturing and QC suggested between medicines and food supplements. Vitamin D3 is a key micronutrient whose intakes are inadequate for most populations worldwide. Supplementation with medicines or food supplements is commonly prescribed to correct this imbalance and the quality of these products must be ensured. In this context, a generic methodology for the assay of vitamin D3 in oily formulations is proposed using supercritical fluid chromatography coupled to mass spectrometry (SFC-MS). It is in line with green analytical chemistry principles and combines the use of i) a fast and robust analytical method (4.0 min analysis time) ii) an easy sample preparation compatible with high throughput analysis (“dilute-and-shoot” approach) and iii) a relevant control strategy. Seventeen products from multiple manufacturers and encompassing a large content range were evaluated in this study. They were classified in four groups to streamline their processing considering the use of a matrix-matched calibration procedure. Matrix effect was thoroughly studied and was found to be low (99–106%), stable intra/inter-series and comparable between the different groups and types of matrices. The implemented control strategy was based on a three-level system suitability tests (SST). Level 1 SST: resolution of the critical pair that was above 1.5 for all analysis series. Level 2 SST: evaluation of the adequacy of the calibration for a QC sample in terms of recovery that was between 97% and 104% with a variability between 1% and 2%. Level 3 SST: method trueness that was between 95% and 102%. Sample analysis highlighted differences in types of products and dosage forms. This is the first study to propose a complete strategy for the quality control of vitamin D3 oily formulations and should prove useful in QC laboratories.