UHPLC-PDA Assay for Simultaneous Determination of Vitamin D₃and Menaquinone-7 in Pharmaceutical Solid Dosage Formulation

Abstract

A newly developed method based on ultrahigh performance liquid chromatography (UHPLC) was optimized for the simultaneous determination of vitamin D3 and menaquinone-7 (MK-7) in tablet formulation in the present study. UHPLC separation of vitamin D3 and MK-7 was performed with ACE Excel 2 C18-PFP column (2 μm, 2.1 × 100 mm) at 0.6 mL min−1 flow rate, whereas the mobile phase consisted of methanol/water (19 : 1, v/v, phase A) and isopropyl alcohol (99.9%, phase B) containing 0.5% triethylamine. Isocratic separation of both the analytes was performed at 40°C by pumping the mobile phases A and B in the ratio of 50 : 50 (v/v, pH, 6.0). Both analytes were detected at a wavelength of 265 nm and the injection volume was 1.0 μL. The overall runtime per sample was 4.5 min with retention time of 1.26 and 3.64 min for vitamin D3 and MK-7, respectively. The calibration curve was linear from 5.0 to 100 μg mL−1 for vitamin D3 and MK-7 with a coefficient of determination (R2) ≥ 0.9981, while repeatability and reproducibility (expressed as relative standard deviation) were lower than 1.46 and 2.21%, respectively. The proposed HPLC method was demonstrated to be simple and rapid for the determination of vitamin D3 and MK-7 in tablets.

An Approach to Investigate Content-Related Quality of Nutraceuticals Used by Slovenian Consumers: A Case Study with Folate and Vitamin D Supplements

“…This can be a major technological challenge for many manufacturers [23]. Quality control is also crucial for both production and shelf life; however, the laboratory quantification of certain constituents can be challenging [24][25][26][27][28]. The bioavailability of ingredients used in food supplements and their interactions also need to be considered, but this area is commonly overlooked and very challenging to regulate [29].…”

Electrochemical Determination of Vitamin D3 in Pharmaceutical Products by Using Boron Doped Diamond Electrode

“…Due to the worldwide use of vitamin D 3 through fortified foods, or various forms of dietetic supplements, the demand for its analysis has increased dramatically, and higher requirements have been placed on its analytical techniques. Numerous analytical methods have been reported for determination of vitamin D 3 , and the majority of these reports are based on chromatographic methods , while immunoassays, capillary electrophoresis and various sensor methods are used as well, but to a much lesser extent. Even though chromatographic methods are providing accurate results, they usually require complicated sample pretreatment step, robust instrumentation, expertise in handling the instruments and long analysis time, which makes them unsuitable for routine analysis.…”

A green ultra‐fast liquid chromatographic method for quantification of curcumin in extract of Curcuma longa L. followed by confirmation via spectroscopic techniques

“…The resultant parameters of the linear regression including the standard deviation (SD) of the response based upon the slope and intercept determined the detection (LOD) and quantitation (LOQ) limits. The LOD and LOQ were defined as 3.3 σ/S and 10 σ/S, respectively [29][30][31][32][33][34] where, σ is standard deviation and S is slope of regression line.…”