METHOD FOR DETERMINING THE QUALITATIVE AND QUANTITATIVE CONTENT OF MONOCHLOROPROPANEDIOLS, GLYCIDOL IN VEGETABLE OILS Russian patent published in 2025 - IPC G01N30/06 

FIELD: fat-and-oil industry.

SUBSTANCE: invention relates to the oil and fat industry, in particular to methods for quantitative and qualitative determination of the content of monochloropropane diols (MCPD) and glycidol and esters thereof in lipid-containing food matrices, and can be used for determination of 2-monochloropropanediol, 3-monochloropropanediol, glycidol in liquid and solid vegetable oils. Method for determining the qualitative and quantitative composition of monochloropropane diols, glycidol in vegetable oil involves preparation of reference samples of the determined compounds, with subsequent analysis of reference samples by gas chromatography with a mass detector, building, based on the obtained data, a calibration curve and a regression equation for each component being determined. Preparation of the test sample, analysis of the test sample, calculation of the content of the analytes in the test sample is carried out according to a predetermined equation describing a calibration line constructed in coordinates of the ratio of the areas of peaks of the reference components to the values of the areas of the peaks of the internal standard and ratio of weight of added reference components to weight of added internal standard. Quantitative content of the analysed components in the oil sample is calculated using the formula: X=[(Ax/Ais)-b]×IS×1/a×1/W, where X is concentration of analyte in test sample, mg/kg; Ax is the area of the peak of the quantitative ion of the analyte; Ais is internal standard ion peak area; a is the tangent of the inclination angle of the calibration curve; b is the point of intersection of the calibration curve with the Y axis; IS is the amount of the internal standard introduced into the test sample, mcg; W is the weight of the analysed sample, g. Preparation of reference samples and the test sample is carried out by mixing the reference samples and the test sample, respectively, with a solvent, followed by derivatisation with 2.5 % solution of phenyl-boric acid and adding an internal standard, represented by hexachlorobenzene with concentration of 3.0 mcg/ml, extraction of phenyl-boron-derivatives of defined components with hexane, concentration in a stream of nitrogen at temperature 40 °C. Analysis is carried out on a gas chromatograph while detecting components with a mass-spectrometer detector in SIM mode, including for hexachlorobenzene ions.

EFFECT: wider range of methods of determining MCPD and glycidol, which enable simultaneous determination in vegetable oil: 3-MCPD, 2-MCPD and glycidol while maintaining high accuracy and implementation of said method.

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