The conditions and parameters of chromatography were selected for the quantitative determination of propionic acid and its salts in bakery products using high-performance liquid chromatography. Validation studies of the developed measurement technique confirmed its suitability for determining the content of propionic acid and its salts in bakery products in the range from 200 to 3000 mg/kg. It was shown that in 25% of the samples of smallpiece bakery products, lamb products and donuts we examined, an excess of the maximum permissible level of propionic acid and its salts was found

Baranovskaya Yu.

Gripinich A.

Roslik V.

Yegorova Z.

English

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The scientific heritage No 121 (2023) 39 PHYSICS AND MATHEMATICS  DETERMINATION OF PROPIONIC ACID AND ITS SALTS IN BAKERY PRODUCTS  Yegorova Z., Belarusian State Technological University, Associate Professor, Faculty of Technology of Organic Substances, Ph.D. Gripinich A., Belarusian State Technological University, graduate of the Faculty of Technology of Organic Substances Baranovskaya Yu., Scientific and Practical Center of the National Academy of Sciences of Belarus for Food, chemical engineer of the 2nd category in the Chromatographic Research Sector Roslik V. Scientific and Practical Center of the National Academy of Sciences of Belarus for Food, Head of the Sector of Chromatographic Research   Abstract The conditions and parameters of chromatography were selected for the quantitative determination of propi-onic acid and its salts in bakery products using high-performance liquid chromatography. Validation studies of the developed measurement technique confirmed its suitability for determining the content of propionic acid and its salts in bakery products in the range from 200 to 3000 mg/kg. It was shown that in 25% of the samples of small-piece bakery products, lamb products and donuts we examined, an excess of the maximum permissible level of propionic acid and its salts was found. Keywords: bakery products, propionic acid, salts of propionic acid, high-performance liquid chromatog-raphy, validation of measurement method.  Introduction. A flexible and at the same time sta-ble technological process for the production of high-quality bakery products is impossible without the tar-geted use of microingredients - food additives, baking improvers and other components [3]. These ingredients include: ascorbic acid E300, calcium peroxide E930, azodicarbonamide E927a, calcium sulfate E516, cal-cium lactate E327, sorbitol E420, calcium propionate E282, etc. [4]. Our analysis of scientific and technical literature indicated that a serious problem is microbio-logical spoilage of bakery products, to combat which propionic acid and its salts are used [5]. Propionic acid E280 is a monobasic saturated car-boxylic acid (CH3CH2COOH) – a colorless, caustic liquid with a pungent odor. A natural source of propi-onic acid is the waste products of bacteria of the genus Propionibacterium. Industrial production of E280 is carried out using chemical synthesis. It has been estab-lished that propionic acid does not have toxic, muta-genic or carcinogenic properties, and it does not have a cumulative effect. However, the possibilities of using propionic acid in the food industry are limited due to changes in the taste of the finished product under its in-fluence. Therefore, propionates are usually used in food production - E281, E282 and E283. Salts of propionic acid (sodium propionate E281 (CH3CH2COONa), cal-cium propionate E282 (Ca(C2H5COO)2) and potassium propionate E283 (CH3CH2COOK)) are crystalline white powders with a pungent odor, highly soluble in water. Of all the salts of propionic acid, the preservative E282 is most often used in the food industry to prevent the growth of unwanted microflora. The preservative is used in the production of bakery and flour confection-ery products, cheeses and cheese products, and is also included in cosmetics and medicines.  Propionic acid and its salts in food products can be identified using the IR spectrum, thin-layer or paper chromatography, and quantified using high-perfor-mance liquid chromatography. Currently, our country uses two standard methods for determining propionic acid in food products using high-performance liquid chromatography. In dairy products - according to GOST 31504 [2], in complex food additives - accord-ing to GOST R 70224 [1]. The main difference between these methods is the use of different chemical compositions and quantities of mobile phases. Considering the above, it was of interest to determine the possibility of adapting these methods for the determination of propionic acid and its salts in bakery products. Aim. Determining the possibility of using the high-performance liquid chromatography method for the quantitative determination of propionic acid and its salts in bakery products. Materials and methods. The objects of the study were samples of bakery products (4 samples of buns, 2 samples of tortillas and 1 sample each of bagels and do-nuts), the recipe of which contains propionic acid and its salts (Table 1).    40 The scientific heritage No 121 (2023) Table 1 Characteristics of research objects  Item No. Research object Compound 1 2 3 1 Wheat tortilla «Mutlukal» with spinach Wheat flour, vegetable oil, salt, sugar, spinach powder and spice mixture E422, raising agents E500, E450, emulsifier E471, preservatives E202, E282, acidity regulators E296, E330 2 Bakery products «Rulets» with poppy seeds Wheat flour, drinking water, Vienna poppy filling, sunflower oil, water, mono- and diglycerides of fatty acids, citric acid, beta-carotene, sugar, pressed baker's yeast, complex food additive Orindsted pro 45, iodized table salt, baking mixture for increasing volume «XXL», flavoring E1422 3 Breakfast buns Wheat flour, drinking water, white sugar, refined deodorized sunflower oil, fiber, pressed baker's yeast, K-SOFT baking mixture, complex food additive Grinstead pro 45, iodized table salt, E1422 flavoring 4 Buns «For hot dog» Wheat flour, drinking water, white sugar, solid margarine, pressed baker's yeast, wheat fiber, dry milk product, iodized table rock salt, complex food additive bak-ery improver «Universal Super», complex food additive Grindsted Pro 45 5 Donuts «Berlin-skie» with «Boiled condensed milk» Wheat flour, milk containing a product with a milk fat substitute «Premium», melange, special-purpose cooking fat «SolPro», cooking fat «Frying», antioxi-dants (E320, E321), hard margarine brand MT 82%, mixture for the production of bakery products «Hefikonk», white sugar, pressed baker's yeast, iodized table salt, complex food additive «Flora Super», baking mixture for increasing volume «XXL» 6 Bagels «Barskie» «Vanilla» Wheat flour, drinking water, sugar, margarine, compressed baker's yeast, dry milk product, baking improver «Universal Super», iodized table rock salt, cal-cium propionate (preservative E282), food flavoring «Vanillin» 7 Hamburger bun Wheat flour, drinking water, white sugar, solid margarine, pressed baker's yeast, peeled sesame seeds (99.90%), wheat fiber, dry milk product, iodized table rock salt, baking improver «Universal Super», complex food additive GRINDSTED PRO 45 8 Wheat tortilla «Mutlukal» with tomato Wheat flour, vegetable oil, salt, sugar, tomato powder and spice mixture 1.8% (onion powder, garlic powder, lemon zest powder, basil powder, dill powder, red sweet pepper, cumin, coriander, thyme, turmeric), E422 , raising agents E500, E450, emulsifier E471, preservatives E202, E282, acidity regulators E296, E330  The subject of the study was propionic acid and its salts. To determine propionic acid and its salts, a method was used that is based on the extraction of pro-pionic acid and its salts from the analyzed sample, their quantitative determination using HPLC using a reverse-phase column and a spectrophotometric detector. The essence of the method we adapted was as follows. (10.000±0.001) g of the analyzed product was trans-ferred into a volumetric flask with a capacity of 100 cm3. 100 cm3 of extraction solution was added to the flask, kept in an ultrasonic bath for 10 minutes, then 5 cm3 of Carrese I and Carrese II solutions were added to precipitate interfering substances, mixed thoroughly and 5 cm3 of acetonitrile was added. The contents of the flask were brought to the mark with double-distilled water, mixed thoroughly and filtered through a folded paper filter. 1 cm3 of the filtrate was transferred to a 10 cm3 volumetric flask, the volume of the contents in the flask was adjusted to the mark with the mobile phase for HPLC. The resulting solution, after filtering through a membrane filter, was used for chromatographic anal-ysis. Using the Chem Station software, the signals of propionic acid and its salts were identified in the result-ing chromatograms based on the detection wavelength and the coincidence of retention times in the calibration solutions. Using the signal areas, the mass concentra-tion of the identified propionic acid and its salts was calculated. To ensure that the methodology we adapted is accurate, linear, reproducible and correct, we vali-dated it using a generally accepted method.  Results and discussion. The results of the valida-tion of the methodology for measuring the content of propionic acid and its salts in bakery products are pre-sented in Table 2. Table 2 Results of validation of the methodology for measuring the content of propionic acid and its salts in bakery prod-ucts Parameter and units of measurement Numerical value  Repeatability limit r, % 14 Relative error limits ±δ, %, P=0,95 23 Reproducibility limit R, % 14 Measuring range, mg/kg 200–3000  The scientific heritage No 121 (2023) 41 As a result of the validation of the measurement technique, the following analytical characteristics were determined and confirmed by calculations: linearity, re-peatability, intermediate precision, uncertainty, which met the standards. The results of studies of the content of propionic acid in the study objects are presented in Table 3. Table 3 Results of determining the content of propionic acid and its salts in the research objects Item No. Sample name Propionic acid con-tent, mg/kg 1 Breakfast buns 1814,09 2 Buns «For hot dog» 2119,76 3 Hamburger bun 1252,76 4 Bakery products «Rulets» with poppy seeds 1567,41 5 Wheat tortilla «Mutlukal» with tomato 248,78 6 Wheat tortilla «Mutlukal» with spinach 2482,09 7 Bagels «Barskie» «Vanilla» 618,64 8 Donuts «Berlinskie» with «Boiled condensed milk» 250,91 Bread with reduced energy value, butter pastries and flour confectionery products, pita, packaged (TR CU 029/2012) [6] No more than 2 g/kg  As can be seen from the data presented, the con-tent of propionic acid in the study objects varied widely: from 250 to 2500 mg/kg. Also, the research re-sults indicate that two samples of bakery products (wheat tortilla “Mutlukal” with spinach and a bun «For a hot dog») do not comply with national legislation in terms of the indicator «Mass fraction of preservatives» (Table 2). It should be noted that samples of buns, ba-gels and donuts produced by Belarusian enterprises had a shelf life of no more than 20 days, samples of tortillas were foreign-made with a shelf life of 9 months. Thus, it is confirmed that the effectiveness of preservatives depends on the microbiological quality of the original recipe components and the degree of compliance with technological regimes and sanitary and hygienic pro-duction conditions. Conclusions. Based on the results of the research, the following conclusions can be drawn. Propionic acid and its salts are most often used as a preservative in baked goods made from wheat flour. Validation studies of the method for measuring the content of propionic acid and its salts in bakery products confirmed its suit-ability in the range from 200 to 3000 mg/kg with a rel-ative error of ±23%. In 25% of the samples of small-piece bakeries, lamb products and donuts we examined, we found that the maximum permissible level of propi-onic acid and its salts was exceeded by 6.0% and 24.1%. The high-performance liquid chromatography method we adapted for determining the content of pro-pionic acid and its salts can be used to control these pre-servatives in baked goods, as well as in low-moisture products (bagels) and donuts.   References 1. Food additives. Method for determining propi-onate ions in complex food additives GOST 70224-2022. – Enter. 01/01/2023. – Minsk: Interstate Council for Standardization, Metrology and Certification: Bela-rusian State Institute of Standardization and Certifica-tion, 2022. – 12 p. 2. Milk and dairy products. Determination of the content of preservatives and dyes by high-performance liquid chromatography GOST 31504-2012. – Enter. 07/01/2013. – Minsk: Interstate Council for Standardi-zation, Metrology and Certification: Belarusian State Institute of Standardization and Certification, 2012. – 15 p. 3. Mugaleva, A.E. Analysis of the assortment and assessment of the quality of bread and bakery products sold on the consumer market / A.E. Mugaleva. – Bel-gorod: BelSU, 2017. – 95 p. 4. Nutritional supplements. Types, properties and safety of food additives [Electronic resource] / Modern production and technology. – Moscow, 2023 – Access mode: https://itexn.com/9345_pishhevye-dobavki-vidy-svojstva-i-bezopasnost-pishhe-vyh-do-bavok.html. – Access date: – 04/26/2023. 5. Nutritional supplements. Calcium propionate [Electronic resource] / Prime chemicals group. – Mos-cow, 2020. – Access mode: https://prodobavki.com-/dobavki/E282.html?page=all. – Access date: 04/20/2023. 6. Safety requirements for food additives, flavor-ings and technological aids: TR CU 029/2012. – Adopted by decision of the Council of the Eurasian Economic Commission of July 20, 2012 No. 58. – Minsk: Gosstandart: RUE «Belarusian State Institute of Standardization and Certification», 2012. – 308 p.   

DETERMINATION OF PROPIONIC ACID AND ITS SALTS IN BAKERY PRODUCTS

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DETERMINATION OF PROPIONIC ACID AND ITS SALTS IN BAKERY PRODUCTS

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