University of Liège (ULiège), CIRM, Laboratory of Pharmaceutical Analytical Chemistry, Liège, Belgium.
University of Liège (ULiège), CIRM, Laboratory of Pharmaceutical Analytical Chemistry, Liège, Belgium; University of Liège (ULiège), CIRM, Laboratory for the Analysis of Medicines, Liège, Belgium.
J Pharm Biomed Anal. 2022 Feb 5;209:114492. doi: 10.1016/j.jpba.2021.114492. Epub 2021 Nov 25.
Vitamin D 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 D 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 D oily formulations and should prove useful in QC laboratories.
维生素 D 是一种关键的微量营养素，其摄入量在世界范围内大多数人群中都不足。通常会开药物或食品补充剂来补充以纠正这种不平衡，必须确保这些产品的质量。在这种情况下，提出了一种使用超临界流体色谱法结合质谱法（SFC-MS）测定油制剂中维生素 D 的通用方法。它符合绿色分析化学的原则，结合了以下方法：i）快速而稳健的分析方法（4.0 分钟分析时间），ii）与高通量分析兼容的简单样品制备（“稀释和进样”方法），以及 iii）相关的控制策略。在这项研究中，评估了来自多个制造商的 17 种产品，涵盖了很大的含量范围。为了简化处理过程，考虑使用基质匹配校准程序，将它们分为四组进行分类。彻底研究了基质效应，发现其很低（99-106％），在同一系列和不同组之间具有稳定性，并且在不同类型的基质之间具有可比性。所实施的控制策略基于三级系统适用性测试（SST）。一级 SST：所有分析系列的关键对的分辨率均高于 1.5。二级 SST：根据 QC 样品的回收率评估校准的充分性，回收率在 97％至 104％之间，变异性在 1％至 2％之间。三级 SST：方法准确度在 95％至 102％之间。样品分析突出了产品类型和剂型之间的差异。这是第一项提出完整的维生素 D 油制剂质量控制策略的研究，应该对 QC 实验室有用。
