General Standardization Trends and Prospects for Objective Evaluation of Organoleptic properties of Beer and Beer Beverages

Lyudmila Tretyak^1*, Maksim Rebezov^2,3,4, Nadezhda Kenijz⁵, Mars Khayrullin⁶,
Maria Babaeva⁶, Svetlana Zhukovskaya⁶, Evgeny Ponomarev⁶, Andrey Goncharov⁶,
Valentina Gagauz¹

¹Orenburg State University, Orenburg, Russian Federation.

²V.M. Gorbatov Federal Research Center for Food Systems of Russian Academy of Sciences,

Moscow, Russian Federation.

³Prokhorov General Physics Institute of the Russian Academy of Science, Moscow, Russian Federation.

⁴Russian State Agrarian Correspondence University, Balashikha, Russian Federation.

⁵Kuban State Agrarian University, Krasnodar, Russian Federation.

⁶K.G. Razumovsky Moscow State University of Technologies and Management

(The First Cossack University), Moscow, Russian Federation.

*Corresponding Author E-mail: tretyak_ln@inbox.ru

ABSTRACT:

This article describes general trends and problems of standardization of alcohol products. It specifies the requirements for standardization of fermentation by-products (FPB) in comparison with strong alcoholic beverages. The work focuses on the lack of standards for the content of fermentation by-products in beer and beer beverages, limiting the development of methods for their quantitative determination. The necessity of objective estimation of organoleptic properties of beer and beer drinks on the basis of determination of the ratio of actual concentration of fermentation by-products with concentrations determining the "recognition threshold" of the main taste-defining substances of the component composition of the finished product has been justified. The results of approbation of standardized chromatographic methods of assessment of toxicity and authenticity of strong drinks in terms of determining the actual content of the main components of fermentation by-products in beer and beer beverages are presented. Perspectives of application of individual author's methods are outlined. The application of dose estimation of taste and aromatic bouquet of ready beverage on the basis of gas chromatographic method of analysis is substantiated.

KEYWORDS: Assessment of Taste and Aroma, Beer, Organoleptic Analysis, Taste and Aroma.

INTRODUCTION:

Beer, as a fermentation product, is characterized by the formation of many different properties of chemicals and compounds, which causes a complex multi-component composition of the finished beverage. Along with wine, beer belongs to the alcoholic beverages with the most complex chemical composition. More than 2000 compounds have been revealed in the composition of beer and beer drinks based on separate sources^1-9. Consumer properties of beer, including its biological value and organoleptic characteristics, are largely determined by the ratio of basic and minor compounds of the component composition of the finished drink. The main components of the taste composition of beer are considered to be the main components of liquorice oil (1-propanol, 2-propanol, isobutyl alcohol, 1-butanol, isoamyl alcohol, etc.), acetaldehyde, certain volatile acids, esters, as well as vicinal diketones (acetoin and diacetyl).

In brewing technology, these chemicals are classified as fermentation by-products (FPBs). Fermentation by-products in beer along with ethanol (the main fermentation product) determine not only the taste and aroma but also the toxic properties of the finished product. It is known that isoamyl alcohol, ethyl acetate and isoamyl acetate represent the main components of beer flavour exceeding 10% of all volatile substances of the finished drink^10,11. Despite the prevalence of higher alcohols and esters, the spectrum of substances forming the bouquet of the finished beer is much wider and contains, in addition to the above mentioned, organic acids and sulfur compounds. Recent studies show a special significance among fermentation by-products of vicinal dicytons, the content of which determines the taste of beer. Diacetyl (2.3 buttandium) is considered to be the bouquet-forming substances of the fresh beer and their concentrations determine the aroma of the beer at the fermentation stage. According to the data of the All-Russian Scientific Research Institute of Brewing, Non-Alcoholic and Wine Industry (a branch of the V.M. Gorbatov Federal Research Center for Food Systems of the Russian Academy of Sciences), the content of diacetyl in Russian beer varieties ranges from 0.1 to 0.3 mg/dm³. From classical fermentation technology it is known that "the approximate value of the content of total diacetyl (vicinal dicyketones and its predecessors) in mature beer should not exceed 0.1 mg/L"^12,13 at the threshold value of taste perception, equal to 0.10-0.15 mg/L.

The purpose of this article is to identify general trends in the standardization of the composition and content of microtoxic impurities in alcoholic beverages and to indicate the prospects for objective assessment of organoleptic properties of beer and beer beverages using instrumental methods for quantitative determination of the actual content of fermentation by-products in finished products.

MATERIALS AND METHODS:

For the analysis of the general tendencies of standardization of alcoholic beverages the methods of directed and systematic search of the information, and also methods of the problem-thematic analysis are used. For experimental determination of chemical compounds that form a component composition of fermentation by-products, the standardized gas chromatographic methods have been adapted: GOST 32039-2013 "Vodka and ethyl alcohol from food raw materials. Gas chromatographic method of authentication", GOST 30536-2013 "Vodka and ethyl alcohol from food raw materials. Gas chromatographic express method for determination of toxic impurities content". The experimental studies were conducted in accredited laboratories of Orenburg. The proposals on development of the method of objective complex estimation of flavor-aromatic properties are based on the system approach and author's methods of determination of the content of particular substances of fermentation by-products composition, protected by patents for inventions^10,11.

RESULTS AND DISCUSSION:

In special studies^13,14, there were prepared suggestions on the quantitative estimation of the taste and aroma of separate substances in the general taste and aroma bouquet of a particular beer. The ratio of the real (actually detected) concentration to the concentration allowing to "recognize" this substance is accepted as a dose of flavor-aromatic substance. The proposed parameter has a mathematical certainty and allows to give an objective organoleptic assessment of the finished product. Its application assumes the knowledge of concentrations, allowing to "recognize" the character of feeling. In the State Standard GOST ISO 5492-2014 "Organoleptic analysis. Dictionary" there is no definition of "recognition threshold concentration".

Comparing the two GOST ISO 5492-2014 standardized terms "recognition threshold ("identification threshold")" and "detection threshold", we conclude that an objective assessment can be made when comparing the actual concentration with the recognition threshold - determining "the minimum physical intensity of the stimulus, at which every time this intensity will occur, the tester will assign the same descriptor to this stimulus" (i.e., the uncertainty of organoleptic evaluation will be eliminated). The concentration of this substance that allows to "recognize" the nature of the sensation has been suggested in the dose approach developed in special studies^15,16 and improved later¹⁷ by the authors of this article to be taken as "unit of taste". In the context of the above reasons, the taste dosage of any substance that may affect the taste and flavour of the prepared beer should be determined:

Taste Dose of the Substance = (Actual concentration of the substance, mg/L)/(Taste recognition threshold concentration, mg/L)

At present there are no objective (instrumentally defined) norms for the content of fermentation by-products in finished beer and beer drinks and as a result there are no standardized methods of their control. The author's criteria for assessing beer aromatic substances are known, for example, according to Miedaner^12,17. However, these criteria cannot be classified as objective, since the "threshold value of taste perception of a substance (mg/L)", which is the basis for evaluation, depends on the individual physiological abilities of the taster. It is known that "taste perception" is very different among experts, and therefore cannot be standardized (cannot serve as a measure of sensitivity, as is common for metrological characteristics of measuring instruments). The given method does not allow to estimate objectively "threshold value of taste perception of substance", possessing as a value of mathematical uncertainty. Therefore, the results of such assessments by Miedaner are limited to a verbal description of the flavours being sensed. A similar approach is used to develop the "Wheel of Tastes and Flavours" known in brewing. The authors of this article develop the direction of quantitative evaluation of beer taste and aroma, which was justified by Morten Mailgaard¹⁸.

However, the previously proposed quantitative evaluation should be reduced to the new requirements, both in terms of methodology (to classify beer as a "taste good") and in terms of taste descriptors^19,20. Unlike beer in strong alcoholic beverages, the content of toxic impurities is regulated. For example, GOST 12712-2013 "Vodka and special vodka. General Technical Specifications" specifies restrictions on the content of impurities in the finished drink depending on the strength of the finished drink and the quality of the alcohol. The content of toxic micro impurities regulated by GOST 12712 (item 5.1.3, table 2 - Physico-chemical indicators) for special vodkas and vodkas made of rectified ethyl alcohol from food raw materials of various degrees of purification ("Highest purification", "Extra", "Lux" and "Alpha") are different. The difference in actual concentrations of toxic micro impurities determines not only the taste and aromatic properties (organoleptics), but also has a significant impact on the toxicity of finished drinks. Taking into account the multicomponent composition of beer, it should be noted that individual by-products of fermentation have a more significant contribution (in comparison with ethanol) to the total toxicity of the finished beverage (in terms of 100 g of ethanol). Special studies^{13,14,21,22,23} on the evaluation of the potential toxicity of the elements forming the same type groups of chemical compounds allowed us to identify the criterion representatives (most typical for each chemical group) having the maximum contribution to the total toxicity. According to the method of estimation of "threshold doses" value we have got a variation range of ready beverage toxic substances. Arranging the substances in descending order of toxicity, we can demonstrate their contribution to the toxicity of the finished beer: ethyl acetate (esters); isoamyl alcohol (higher alcohols); acetaldehyde (aldehydes); caprylic acid (saturated fatty acids). Much attention is focused on finding methods of objective control of substances responsible for the taste and aroma of finished beer. In conditions of normative uncertainty (absence of standardized methods for determining the content of higher alcohols and esters as the basis for the component composition of fermentation by-products in beer), proposals¹³ have been developed to adapt the standardized gas chromatographic method (technique) as applied to beer analysis. The method was based on GOST R 51698-2000 "Vodka and ethyl alcohol from food raw materials. Gas chromatographic express method for determination of the content of toxic impurities" (GOST was cancelled from 15 February 2015). We determined the actual content of individual components of fermentation by-products on the basis of an accredited laboratory in beer samples of the most demanded varieties. However, straight transfer of vodka and cognac quality criteria, as substantiated in the article¹³, is not applicable for beer quality assessment.

The problem of falsification of alcoholic beverages has been acute for the market in recent years. ROSKACHESTVO, as a rule, acting on behalf of the Government of Russia, during multistage studies of the quality of light pasteurized beer on the Russian market has repeatedly emphasized the lack of objective methods of control (source information is taken from the portal of the independent non-profit organization "ROSKACHESTVO": https://rskrf.ru/news/podvedeny-itogi-issledovaniya-piva/). This has a special relation to the quality of beer beverages: "...the results of studies show that the existing classification of beer beverages misleads consumers about their composition and properties. Due to the lack of clear identification features, it contributes to the so-called legal falsification". The lack of methods to control the implementation of mandatory requirements is an evidence of the industry problem. Therefore, authoritative members of the commission "ROSKACHESTVO" put anonymous samples for taste, color and flavor points, resorting to verbal rather than instrumental assessment. However, the increase in the number of dangerous (toxic) and counterfeit strong alcoholic beverages (primarily vodka), as well as the increased capacity of chromatography, have contributed to the development and standardization of identification methods applicable to the assessment of the authenticity of alcoholic products. We used the fact that these methods are based on standardized gas chromatographic research methods: GOST 32039-2013 "Vodka and ethyl alcohol from food raw materials. Gas chromatographic method of authentication" and GOST 30536-2013 "Ethyl vodka and ethyl alcohol from food raw materials. Gas chromatographic express method for determination of toxic impurities content".

In the vodka conformity assessment practice, GOST 32039-2013 is the most used, as this interstate standard regulates the determination of concentrations for a wider component composition of strong alcoholic beverages. Therefore, on the basis of an accredited testing laboratory we have analyzed the brands of beer and beer beverages that are most in demand among consumers. General information about the tested beer and beer beverages samples is presented in Table 1. Some results on the content of fermentation by-products and complex organoleptic evaluation on the example of the most demanded beer samples were presented by the authors earlier²⁴. The published article summarizes the data on concentrations of microtoxic impurities not only in beer, but also in beer drinks, which are popular among young people at present. The analysis of the actual content of microtoxic impurities determining the taste and aromatic properties of finished products is presented in comparison with strong drinks (Table 2). The summarized literature data on the concentrations of fermentation by-products found in domestic and foreign samples of top and bottom fermentation beer (systematized in the framework of the special study author's developments) are given in monograph¹³. The results of own researches obtained on the basis of accredited testing laboratories "Center of Hygiene and Epidemiology in the Orenburg region" and "Federal Scientific Center of Biological Systems and Agrotechnologies of the Russian Academy of Sciences" are published in^25,26.

Table 1: Basic information on the studied brands of beer and beer beverages.

Brand of beer and beer beverages	Type of beer (beer drink)	Producer (city), regulatory document for the quality of the finished product (if available)	Volume fraction of alcohol, %	Extractivity, %,	Retail price (volume of consumer packaging 500 ml), in Russian rubles ₽ (rate 1$ =64,8₽).
1. "Martens" beer.	Light, pasteurized, filtered.	Belgium	12.2	21.0	99.00
2. Beer "Ohota krepkoye."	Light, pasteurized	United Breweries Heineken (Yekaterinburg).	8.1	12.0	39.90
3. "Amsterdam Navigator" beer.	Light, pasteurized	Moscow - Efes Brewery TU 9184-050-48354931-2012	8.0	14.2	54.90
4. Beer "Lowenbrau Original."	Light, pasteurized	SAN InBev" (Saransk, Yalga settlement)	5.4	12.0	49.90
5. SPATEN Miinchen Beer	Light, pasteurized	Spaten Franziskaner Brau GmbH	5.2	11.8	94.90
6. Baltika №3 Classic Beer.	Light, pasteurized	Baltika Breweries TU 9184-201-01824944-2008	4.8	12.0	43.90
7. Beer drink "Essa" with the taste and aroma of pineapple and grapefruit.	Light, pasteurized	Moscow - Ephesus Brewery TU 9184-046-48354931-2012	6.5	16.8	49.90
8. Seth and Reillys Garage Hard beer drink Super Lemon.	Pasteurized	Baltika Breweries TU 9184-207-01824944-2014	4.6	14.9	54.90
9 Beer drink "Velikopopovitsky Kozel Dark"	Dark, pasteurized.	Moscow-Efes Brewery TU 9184-048-48354931-2012	3.7	9.6	47.99

Note: Samples of beer and beer drinks purchased in Orenburg were analysed. At the time of the study, their actual shelf life did not exceed one month from the date of production (it is known that in beer after 1-1.5 months of storage secondary and tertiary chemical compounds are formed when fermentation by-products interact).

Table 2: Regulated and real (actual) content of microtoxic impurities in alcoholic drinks of different strength (summarized data of authors' own research).

Indicator	Vodka, 1 dm³ of anhydrous alcohol, mg		Cognacs, mg/100 cm³of anhydrous alcohol		Beer ****** (mg/dm³)**	Beer drinks (mg/dm3)
Indicator	Indicators for "Extra" alcohol vodka, regulated by GOST R 51355-99*	Real**	Regulated by GOST R 51618-2000***	Real**	Content in the tested samples
Strength (volume fraction of ethyl alcohol), %	40.0-45.0	38.0-40.0	Not less 40.0	38.0-42.0	4.8 – 12.2	3.7-6.5
Mass concentration of aldehydes (aldehydes in conversion to acetic aldehyde)	4.0	2.13-2.14	5.0-50.0	14.2-23.4	1.35-26.93	3.58-7.36
Mass concentration of fusel oil (higher alcohols) 1 dm³ of anhydrous alcohol	5.0	0.37-0.4	170.0-500.0	483.1-535.0	41.36- 167.13	83.36-264.34
Mass concentration of complex esters (average esters in conversion to acetic-ethyl ether)	10.0	0.5-0.6	50.0-270.0	67.0-74.0	123.84-309.60	86.19-248.01
Volume fraction of methyl alcohol, %	0.02	0.00036	1.0+0.05 g/L	0.281 mg	0.0003-0.0006	0.0002-0.0004

Notes:

* - GOST R 51355-99 "Vodka and vodka special. General technical specifications" (cancelled since June 28, 2013, GOST 12712-2013 "Vodka and vodka special. General technical specifications": entered into force from 15.02.2015);

** - The actual content of fermentation by-products in randomly selected samples of vodka and cognacs was determined in the Federal State Budgetary Institution "Center of Hygiene and Epidemiology in the Orenburg region" by standardized methods. Detailed description and peculiarities of the methods application are given in [3];

*** - GOST R 51618-2000 has now been updated to GOST R 51618-2009;

**** - real content of fermentation by-products in the samples of the most demanded brands of beer and beer drinks (characteristics of samples are given in Table 1). Research results of the Test Center of FSBNU "Federal Research Center of Biological Systems and Agro-technologies of the Russian Academy of Sciences" are presented. A gas chromatograph "Crystal-2000M" with PID detector is used as the main equipment. The study is based on gas chromatographic method of evaluating the authenticity of strong drinks (GOST 32039-2013).

Fig. 1: Doses of taste of the main substances that carry taste and aroma demanded in the Orenburg beer drinks market (own research)

The development and implementation of GOST 57893-2017 can be considered a major breakthrough in the standardization of methods for assessing the component composition and content of fermentation by-products. However, the full application of this method in brewing practice requires its validation. Probably for this reason, in the available literature we have not found the results of practical research on the composition and concentration of fermentation by-products in beer using this method. It is necessary to highlight the technological problems of reducing beer toxicity. In brewing, there are no methods of purifying semi-products and finished beer from components of fermentation by-products with increased toxicity. The conducted analysis has shown that all variety of methods of beer purification consists in washing beer with carbon dioxide (carbon dioxide); electrophysical methods of beer purification: by influence of electromagnetic fields of high (HF) and ultra-high (UHF) frequencies by infrared, ultra-violet radiation and ultrasound (all listed methods have not received wide circulation). In addition, the effect of carbon dioxide and the effect of electrophysical treatment on the composition of fermentation by-products of finished beer has not been studied extensively enough. It is well known that carbon dioxide in sufficient quantities has a beneficial effect on the taste of beer, giving a pleasant refreshing taste.

In contrast, various materials and methods of purification are widely used for vodka production technologies: low-cost absorbers-activated carbon, soda, potassium permanganate (manganese). Besides, biological (using milk, bread from rye or mixed flour) and chemical (using alkalis with the subsequent fraction distillation) methods of purification are widespread. Frosting and gluing as alternative methods of vodka purification have recently become widespread. In the beer production process, the content of toxic impurities, consisting mainly of fermentation byproducts, is not only not regulated, but they are also considered to be taste stimulating, without taking into account the dual role: simultaneous exposure to taste and toxicity. This is due to the specificity of individual fermentation by-products not only to form the taste and aroma of beer, but also to characterize, along with ethyl alcohol, the toxicity of the finished beverage^18,19,20. We link the special interest in the content of fermentation by-products in beer with their dual role: many of them belong to substances of 2nd and 3rd hazard classes. Taking into account the simultaneous contribution of the components of fermentation by-products to the toxicity and organoleptics of the brewed beer, the authors of this article propose the methodology of complex assessment of taste and aromatic properties of beer on the basis of chromatographic determination of concentration of volatile fermentation by-products^16,17, patent-protected spectrophotometric express method for determination of diacetyl¹⁰, as well as a method for estimation of organoleptic parameters of beer quality by determining the concentration of acetoin, which can change the taste of ready beer¹¹. In addition, safety requirements on the principles of HACCP, perspective and inexpensive technological methods of beer production with specified flavor-aromatic properties and reduced toxicological characteristics^29,30,31. The necessity of metrological evaluation of methods (techniques) allowing not only to identify brewing products, but also to objectively determine organoleptic properties of beer and beer drinks, becomes an actual task of standardization in the field of metrological support of alcoholic beverages.

CONCLUSION:

Taking into account modern trends in the development of society and, in particular, a fundamental change in the system of nutrition, both at the level of diets and at the component level, the widespread presence of falsified products, the issues of quality analysis of beer and beer beverages are becoming relevant and require timely consideration. It is necessary to agree with the opinion of the representatives of ROSSPIRTPROM JSC that in order to detect falsified alcoholic beverages more advanced methods of testing and measurement are required. Due to the mentioned features of individual components of fermentation by-products, their content in the finished beer should be limited. Lack of standardized methods (techniques) for quantitative determination of the content of fermentation by-products in beer restrains the appointment of standards limiting their content in the finished product. For this reason, valid methods of quantitative determination (evaluation) of actual concentrations of various toxic substances - flavour and aroma carriers of finished beer and beer drinks - should be developed and tested in practice. The results given in the article confirm the possibility of application of chromatographic methods for determination of concentrations of volatile components of fermentation by-products not only in beer, but also in beer drinks. The practical testing of chromatographic method allows to confirm that the prospects of objective evaluation of taste and aroma are connected with metrological possibilities of chromatographic analysis. A significant barrier in restricting access to the domestic market for falsified beverages must be the relevant normative documents of both international (ISO) and interstate (GOST) and national (GOST R) levels. They must regulate not only the composition and organoleptic characteristics of beverages, but also the main parameters specific to the beverage. In order to standardise, approbation and metrological evaluation of author's methods of photometric determination of acetoin and diacetyl content in the finished beer are required.

ACKNOWLEDGEMENT:

We thank EJA – Professional Translation Services, Indonesia for editing the manuscript.

CONFLICT OF INTEREST:

The listed authors declare no conflict of interest in any capacity, including competing or financial.

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Received on 27.05.2020 Modified on 20.07.2021

Research J. Pharm.and Tech 2022; 15(3):1323-1329.

DOI: 10.52711/0974-360X.2022.00221