RU2530640C1 - Method for determination of apple puree weight fraction in pastille product by organic acids ratio - Google Patents

Abstract

FIELD: food industry.

SUBSTANCE: determination method envisages weighing of a 2.0-5.0 g sample of marshmallow. One places the sample in a 1,000 ml measuring flask, adds 100-200 cm³ of 10 mmol/l solution of benzoic acid with temperature equal to 60-70°C. Then the mass is thoroughly stirred in a 75-85°C water bath during 10-20 min until complete dissolution of the sample. The solution is filtered through a paper filter and diluted to the marked volume with benzoic acid solution having concentration equal to 10 mmol/l and centrifuged during 10-15 min at a rate of 2500-3000 rpm. Then clear solution if transferred into a vessel for performance of organic acids composition study by capillary electrophoresis method with indirect detecting using a buffer solution. The buffer solution consists of 8-12 mmol/l of benzoic acid, 8-10 mmol/l of diethylamine, 0.45-0.55 mmol/l of cetyl trimethyl ammonium bromide, 0.05-0.10 mmol/l of ethylenediaminotetraacetic acid. The solution pH is 5.0-5.7. The capillar length is 50-97 cm with the capillary effective length being 43-90 cm while the capillary external diameter is 50-75 mcm. The sample is introduced within the range of values of pressure multiplied by introduction time 200-1000 mbar×s. Detecting is performed by means of a diode matrix detector with the thermostat temperature equal to 21-28°C and voltage equal to 15-30 kV. Calculation of the malic acid and tartaric acid peaks height is performed at wave length amounting to 230 nm. Then the apple puree weight fraction is determined from a certain mathematical formula.

EFFECT: invention allows to determine weight fraction of apple puree in marshmallow and reduce the study performance time.

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Description

The invention relates to the field of food industry, in particular to the confectionery industry, and can be used to control the quality of marshmallows.

The closest analogue to the claimed method are GOST 6441-96 "Pastry. General specifications "and GOST R 53041-2008" Confectionery and semi-finished products of confectionery production. Terms and definitions ”, which establish the minimum mass fraction of fruit raw materials in pastel products - not less than 11%. However, the above regulatory documents do not indicate methods for determining the mass fraction of fruit raw materials in marshmallows.

In the proposed method, the mass fraction of applesauce in marshmallows is determined by the ratio of the complex of organic acids using the method of capillary electrophoresis.

The method of capillary electrophoresis is successfully used in the food industry to determine the quality and naturalness of wines (patents RU 2271000 C1, publ. 02.27.2006; RU 2156976 C2, publ. 27.09.2000).

The technical task of the invention is to determine the mass fraction of applesauce by the mass fraction of the complex of organic acids and reducing the time spent on research.

To achieve this goal, a method is proposed for determining the mass fraction of applesauce in a pasty product - marshmallows, which involves weighing 2.0-5.0 g of a marshmallow sample, placing the sample in a volumetric flask with a volume of 1000 ml, adding 100-200 cm ³ of a benzoic acid solution with a concentration 10 mmol / L and a temperature of 60-70 ° C, thoroughly stirring until the sample is dissolved for 10-20 minutes in a water bath at a temperature of 75-85 ° C, filtering the solution through a paper filter, adjusting the volume to the mark with a solution of benzoic acid with a concentration of 10 mmol l / l and centrifuged for 25-40 minutes at a speed of 3000-3500 rpm, after which the clear solution is transferred to a container for studying the composition of organic acids by capillary electrophoresis with indirect detection using a buffer solution of 8-12 mmol / l of benzoic acid, 8-10 mmol / l of diethanolamine, 0.45-0.55 mmol / l of cetyltrimethylammonium bromide, 0.05-0.10 mmol / l of ethylenediaminetetraacetic acid, at pH 5.0-5.7; the length of the capillary is 50-97 cm, the effective length of the capillary is 43-90 cm, the inner diameter of the capillary is 50-75 μm, the sample is introduced in the range of the product of pressure and the injection time from 200-1000 mbar × s, detection is carried out on a diode -matrix detector with a thermostat temperature of 21-28 ° C and a voltage of minus 15-30 kV; the calculation of the peak heights of malic and tartaric acids is carried out at a wavelength of 230 nm, after which the mass fraction of applesauce is determined by the formula:

where M is the mass fraction of applesauce in the product,%,

m is the mass of a sample of the product, g;

h ₁ - the sum of the heights of the peaks of malic and tartaric acids on the electrophoregram of a standard solution of organic acids with a mass fraction of each acid of 5 mg / l, in units transmission;

h ₂ - the sum of the heights of the peaks of malic and tartaric acids on the electrophoregram of the sample solution, in units transmission; if the product sample contains other fruit components, then the peak height of malic acid is calculated as the height of the peak of tartaric acid multiplied by a factor of 7.0 (according to reference data);

1.25 - coefficient taking into account the concentration of acids in a standard solution, sample dilution and the sum of mass fractions of malic and tartaric acids in applesauce, equal to 0.8% (according to reference data), g.

Reference data are taken from the reference book “Chemical composition of food products” / Ed. THEM. Skurikhina, M.N. Volgareva. VO Agropromizdat, 1987 .-- 360 p.

The technical result consists in the fact that the mass fraction of applesauce used for the production of confectionery products is proportional to the mass fraction of tartaric and malic organic acids in the product. When using other raw materials, the ratio of the mass fractions of tartaric and malic acids changes, the calculation is carried out as described above, and it becomes possible to determine the mass fraction of only apple puree used for the production of confectionery.

Example 1

A 2.5 g sample of marshmallow is weighed into a 1000 ml volumetric flask, 100 cm ^{3 of a} 10 mmol / L solution of benzoic acid is added at a temperature of 60 ° C, mixed thoroughly, dissolved for 15 minutes in a water bath at a temperature of 80 ° C. The solution is filtered through a paper filter, the solution volume is adjusted to the mark with a solution of benzoic acid with a concentration of 10 mmol / L. Then the solution is centrifuged for 30 minutes at a speed of 3000 rpm.

The clear solution is transferred to a container for studying the composition of organic acids by capillary electrophoresis with indirect detection.

The composition of the buffer solution: 11 mmol / L benzoic acid, 10 mmol / L diethanolamine, 0.45 mmol / L cetyltrimethylammonium bromide, 0.08 mmol / L ethylenediaminetetraacetic acid, pH 5.4.

Determination conditions: capillary length 65 cm, effective capillary length 58 cm, internal diameter of the capillary 75 μm, injection of a sample under a pressure of 600 mbar × s, diode array detector. Thermostat temperature 25 ° C. Voltage minus 25 kV.

The peak height of malic acid at a wavelength of 230 nm was 3.9 · 10 ^-4 units. transmission, tartaric acid 8.9 · 10 ^-4 units transmittance. An example of an electrophoregram of an extract of a marshmallow sample is shown in the graph.

The sum of the heights of the peaks of malic and tartaric acids h ₂ = 0.0013 units. transmittance. From the electrophoregram of the standard solution, we determine h ₁ = 0.0020 units. transmittance.

Mass fraction of applesauce in marshmallows is determined by the formula (1)

Claims (1)

A method for determining the mass fraction of applesauce in a pasty product - marshmallows, comprising weighing 2.0-5.0 g of a marshmallow sample, placing the sample in a 1000 ml volumetric flask, adding 100-200 cm ³ of a benzoic acid solution with a concentration of 10 mmol / l and temperature of 60-70 ° C, thoroughly mixing until the sample is dissolved for 10-20 minutes in a water bath at a temperature of 75-85 ° C, filtering the resulting solution through a paper filter, adjusting the volume to the mark with a solution of benzoic acid with a concentration of 10 mmol / l and subsequent centrifuged for 25-40 minutes at a speed of 3000-3500 rpm, after which the clear solution is transferred to a container for studying the composition of organic acids by capillary electrophoresis with indirect detection using a buffer solution of 8-12 mmol / l benzoic acid 8-10 mmol / L diethanolamine, 0.45-0.55 mmol / L cetyltrimethylammonium bromide, 0.05-0.10 mmol / L ethylenediaminetetraacetic acid, at pH 5.0-5.7; the length of the capillary is 50-97 cm, the effective length of the capillary is 43-90 cm, the inner diameter of the capillary is 50-75 μm, the sample is introduced in the range of the product of pressure and the injection time from 200-1000 mbar × s, detection is carried out on a diode -matrix detector with a thermostat temperature of 21-28 ° C and a voltage of minus 15-30 kV; the calculation of the peak heights of malic and tartaric acids is carried out at a wavelength of 230 nm, after which the mass fraction of applesauce is determined by the formula:

where M is the mass fraction of applesauce in the product,%,
m is the mass of a sample of the product, g;
h ₁ - the sum of the heights of the peaks of malic and tartaric acids on the electrophoregram of a standard solution of organic acids with a mass fraction of each acid of 5 mg / l, in units transmission;
h ₂ - the sum of the heights of the peaks of malic and tartaric acids on the electrophoregram of the sample solution, in units transmission; if the product sample contains other fruit components, then the height of the peak of malic acid is calculated as the height of the peak of tartaric acid, multiplied by a factor of 7.0 (according to reference data);
1.25 - coefficient taking into account the concentration of acids in a standard solution, sample dilution and the sum of mass fractions of malic and tartaric acids in applesauce, equal to 0.8% (according to reference data), g.