Flotation/ultrasound‐assisted microextraction followed by HPLC for determination of fat‐soluble vitamins in multivitamin pharmaceutical preparations

Abstract

Dissolved carbon dioxide flotation-emulsification microextraction technique coupled with high-performance liquid chromatography was developed for separation and determination of fat-soluble vitamins (A, D , E, and K ) in multivitamin pharmaceutical preparations. Dissolved carbon dioxide flotation was used to break up the emulsion of extraction solvent in water and to collect the extraction solvent on the surface of aqueous sample in narrowed capillary part of extraction cell. Carbon dioxide bubbles were generated in situ through the addition of 300 μL of concentrated hydrochloric acid into the alkaline sample solution at pH = 11.5 (1% w/v sodium carbonate), which was sonicated to intensify the carbon dioxide bubble generation. Several factors affecting the extraction process were optimized. Under the optimal conditions, the limits of detection were 0.11, 0.47, 0.20 and 0.35 μg/L for A, E, D , and K vitamins in water samples, respectively. The inter-day and intra-day precision of the proposed method were evaluated in terms of the relative standard deviation and were <10.5%.

Determination of Vitamins K1, K2 MK-4, MK-7, MK-9 and D3 in Pharmaceutical Products and Dietary Supplements by TLC-Densitometry

“…Thin-layer chromatography (TLC) has been applied for the determination of vitamin K 1 [34], K 2 MK-4, K 2 MK-7, and K 1 [35] and vitamin D 3 [36]. In the majority of the studies on vitamins K and D, high-performance liquid chromatography (HPLC) using different types of detection methods has been applied, including electrochemical [37], spectrophotometric, fluorimetric [38,39] or mass spectrometry/tandem mass spectrometry (LC-MS) [40][41][42]. Among the chromatographic methods, gas chromatography (GC) is lesser used in vitamin K and D analysis [43,44].…”

A concise review of quantification methods for determination of vitamin K in various biological matrices

“…Protein precipitation (PP), liquid-liquid extraction (LLE), and solid-phase extraction (SPE) are the three most common techniques used for vitamin K purification process in biological matrix to achieve efficient analyte recovery by reducing ion suppression and enhancement of analyte signal. Other approaches such as performing derivatization reactions (25)(26)(27)(28), emulsification mircroextraction (29), and sonication (30) have also been reported in sample preparations. PP is a rapid, generic and relative inexpensive sample preparation method.…”

“…Methadone component in pharmaceutical preparations was identified by a repeatable and reproducible HPLC-UV method. The total extraction time can be reduced to only 2 minutes by using dissolved carbon dioxide flotation after emulsification microextraction method (29).…”

Analysis of vitamin D metabolic markers by mass spectrometry: Recent progress regarding the “gold standard” method and integration into clinical practice

“…The aim of the study was to suggest an easy‐to‐perform method, that could be quickly established and readily transferred from one laboratory to another. Other alternative sample preparation methods for nonbiological samples such as pharmaceuticals, milk, yogurt, cereal, and so on are magnetic SPE (Hu et al, 2010; Jiao, Jiao, et al, 2016; Jiao, Zhang, et al, 2016; Momenbeik & Yazdani, 2015), SLE (Jenkinson et al, 2018), dispersive liquid–liquid microextraction (DLLME) (Kamankesh et al, 2017, 2018) and dissolved carbon dioxide flotation microextraction (Shahdousti & Aghamohammadi, 2018).…”