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Vitamin D3: Preconcentration and Determination in Cereal Samples Using Ultrasonic-Assisted Extraction and Microextraction Method

Kamankesh, Marzieh, Mohammadi, Abdorreza, Mollahosseini, Afsaneh, Jazaeri, Sahar, Shahdoostkhany, Mehrnoosh
Cereal chemistry 2017 v.94 no.3 pp. 532-538
breads, cholecalciferol, detection limit, high performance liquid chromatography, liquid-phase microextraction, potassium hydroxide, response surface methodology, statistical analysis, wheat flour
This research is the first analytical method to isolate and determine cholecalciferol (vitamin D₃) in cereal samples. Ultrasonic-assisted extraction followed by dispersive liquid-liquid microextraction as a fast, reliable, and highly sensitive method was employed for the preconcentration step. High-performance liquid chromatography allowed an efficient and considerably faster analysis. Alcoholic KOH solution was employed for accomplishing the fast and easy release of vitamin D₃ from the wheat flour and bread matrix. Effective factors in the microextraction process were investigated and optimized with response surface methodology based on a central composite design. Under the best conditions, the calibration curves showed high levels of linearity (R² > 0.999) for vitamin D₃ in the range of 2–500 ng/g. The relative standard deviation for the seven analyses was 6.2%. The relative recoveries of vitamin D₃ in spiked wheat flour and bread samples were 87–98%. The limit of detection and limit of quantitation were 0.7 and 2.1 ng/g, respectively. The method compared favorably with other methods for vitamin D₃ analysis of various foods.