Determination of α-tocopherol in cereal grains by use of saponification coupled with ionic-liquid-based dispersive liquid–liquid microextraction before high-performance liquid chromatography-mass spectrometry

Abstract

A selective and low organic-solvent-consuming method of sample preparation combined with highperformance liquid chromatography-mass spectrometry detection is introduced for the analysis of atocopherol in cereal grains. The sample treatment involves initial saponification and preconcentration of the analyte performed by ionic-liquid-based dispersive liquid-liquid microextraction, with ethanol as disperser solvent and 1-octyl-3-methylimidazolium hexafluorophosphate as extraction solvent. The method offered excellent linearity over a range of 0.5-15 mg g À1 with a correlation coefficient of r > 0.998. Intra-day and inter-day repeatability, expressed as relative standard deviation were 3.4% and 5.9%, respectively. The quantitation limits and detection limits were 2.5 and 0.7 ng g À1 . Satisfactory recoveries ranging from 86.5% to 106.3% were obtained. The developed method was successfully applied to 12 cereal grain samples.

Salting-out assisted liquid–liquid extraction coupled with high-performance liquid chromatography for the determination of vitamin D3 in milk samples

“…Sample preparation process plays an important role in enhancing sensitivity and reducing matrix interference. The most common preparation technique is saponification [8,9], liquid-liquid extraction (LLE) [10], solid-phase extraction (SPE) [11][12][13][14] and derivatization [15]. Saponification is commonly the first step before LLE and SPE and is used to remove neutral lipids, especially triglycerides.…”

Vitamin E in foodstuff: Nutritional, analytical, and food technology aspects

“…Recently, several research groups have demonstrated that the drawbacks of using the traditional saponification method could be overcome by coupling saponification with dispersive liquid–liquid microextraction (DLLME) in lieu of traditional liquid–liquid extraction (LLE). DLLME is a new technique that is coupled with saponification to enhance reliability and extractability (Sadrykia et al., 2019; Xie et al., 2016). DLLME is a miniaturized form of LLE.…”

“…Xi et al found that IL-DLLME had several advantages over traditional extraction and DLLME. They reported that the significant reduction in the dosage of the sample and the volume of the saponification solution and the avoidance of washing, drying, and concentration steps via rotary evaporation made IL-DLLME faster and more straightforward than other methods; last but not least, IL-DLLME reduced the required quantity of the organic solvent from 200 ml of ethyl ether to 140 μl of 1-octyl-3-methylimidazolium hexafluorophosphate for one extraction (Xie et al, 2016).…”