Simultaneous Determination of Vitamins D3 (Calcitriol, Cholecalciferol) and K2 (Menaquinone-4 and Menaquinone-7) in Dietary Supplements by UHPLC.

The content and composition of dietary supplements is of great interest due to their increasing consumption and variety of available brand offered in the market. Accurate determination of vitamins is important for the improvement of dietary supplement quality and nutrition assessments. In this regard, the simultaneous determination of vitamin D3 (calcitriol-CT and cholecalciferol-CHL) and K2 (menaquinone-4-MK-4 and menaquinone-7-MK-7) in dietary supplements was developed by using ultra-high-pressure liquid chromatography (UHPLC). The overall runtime per sample was above 35 min, with the retention times of 2.40, 6.59, 7.06, and 32.6 min for vitamin D3 (CT and CHL) and vitamin K2 (MK-4 and MK-7), respectively. The limits of detection and limits of quantification for the target nutritional compounds ranged between 0.04-0.05 µg/mL, respectively. The validation results indicated that the method had reasonable linearity (R2 ≥ 0.9990), good recovery (>82%), satisfactory intra-day precision (≤1.9%) and inter-day precision (≤3.5%), and high selectivity and specificity. The validated UHPLC method was demonstrated to be precise, accurate, and robust for the simultaneous determination of vitamins D3 (CT and CHL) and K2 (MK-4 and MK-7) in dietary supplements.

Optimization of High-Pressure Extraction Process of Antioxidant Compounds from Feteasca regala Leaves Using Response Surface Methodology.

Circular economy principles are based on the use of by-products from one operation as the raw materials in another. The aim of this work is to obtain extracts with high antioxidant capacity and resveratrol content for the superior capitalization of the biomass of Feteasca regala leaves obtained during vineyard horticultural operations in spring. In order to obtain a high-quality extract at an industrial level, an optimal extraction process is needed. Central composite design (CCD) was used for the experiment design, which contained three independent variables: the ratio of extraction solvent to solid matter, temperature (°C) and time (minutes). The evaluation of extracts was done by measuring the total antioxidant capacity of the extracts using photo-chemiluminescent techniques, and the resveratrol content using liquid chromatography. Process optimization was done using response surface methodology (RSM). Minitab software version 17.0 was used for the design of experiments and data analysis. Regression analysis showed that the model predicts 87.5% of the variation for resveratrol and 96% for total antioxidant capacity (TAC). The temperature had the biggest influence on the extraction yield. The optimal operational conditions for the extraction method applied had the following conditions: ratio e/m 2.92; 43.23 °C and 55.4 min. A maximum value of 34,623 µg ascorbic acid equivalent (AAE) /mL total antioxidant capacity and 182.4 µg/mL resveratrol content were obtained when the optimal extraction parameters where used. The values obtained in experiments proved that by using RSM an accurate model can be obtained for extraction of Feteasca regala leaves.