METHOD OF QUANTITATIVE DETERMINATION OF N-DIPHENYLNITROSAMINE IN MEAT SAMPLES OF FOOD PRODUCTION BY METHOD OF CHROMATOGRAPHY-MASS-SPECTROMETRY

FIELD: food industry.SUBSTANCE: method of quantitative determination of N-diphenylnitrosamine in meat samples of food production by the method of chromatography-mass spectrometry is characterized by the fact that sample preparation is carried out. 10 ml of potassium methylate are added to 5 g of a meat sample. Potassium methylate is preliminary obtained by means of mixing potassium hydroxide with methanol at the weight ratio of 1:4.9, respectively. The mixture of the sample with potassium methylate is further heated at the temperature of 60-70°C for 2 hours. Then it is mixed with 10 ml of hexane and subjected to centrifugation for 20 minutes at 4500 rpm. Thereinafter, the lower layer is separated and water is added thereto with vigorous stirring to the volume of 45 ml. The mixture is left for holding at the temperature of 5-7°C for 12 hours and then centrifuged again for 20 minutes at 4500 rpm. The aqueous layer separated during the centrifugation is subjected to solid phase extraction (SPE) on a SPE apparatus containing a carbon cartridge in which the SPE device cartridge is first flushed with methylene chloride, and ethyl acetate is passed through it with a delay of 30 seconds. Then it is flushed with water. Thereinafter, the previously obtained aqueous layer is charged. The cartridge is dried for 20 minutes. The elution of the aqueous layer from the cartridge with methylene chloride is carried out. Thereinafter, the resulting eluants are analyzed by chromatography-mass spectrometry, and the amount of N-diphenylnitrosamine in the meat sample is determined, using a calibration curve in the selective ion monitoring mode.EFFECT: method allows to quickly and accurately determine N-diphenylnitrosamine in meat products.2 cl, 1 dwg, 4 tbl, 1 ex Изобретение относится к области пищевой промышленности и предназначено для определения N-дифенилнитрозамина в мясной продукции. Способ количественного определения N-дифенилнитрозамина в мясных пробах пищевой продукции методом хромато-масс-спектрометрии характеризуюется тем, что осуществляют пробоподготовку. К 5 г мясной пробы добавляют 10 мл метилата калия. Метилат калия получают предварительно путем смешивания гидроокиси калия с метанолом в массовом соотношении 1:4,9 соответственно. Производят последующий нагрев смеси пробы с метилатом калия при температуре 60-70°С в течение 2 ч. Затем смешивают ее с 10 мл гексана и подвергают центрифугированию в течение 20 мин при 4500 об/мин. Далее отделяют нижний слой и добавляют в н