Chapter

# Cider Vinegar Production

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## Abstract

Cider vinegar or apple cider vinegar is the vinegar produced by the acetous fermentation of apple cider, according to the Codex Alimentarius. In other words, the primal raw material is apple juice or concentrated apple juice that undergoes alcoholic fermentation, and after that, the produced cider is subjected to a fermentation with acetic acid bacteria, for the final production of the vinegar. Cider vinegar is consumed and produced in several countries around the world, mainly in the United States of America, the United Kingdom, and Switzerland.

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A GC-FID method for major volatile analysis in cider and wine was validated under the requirements of the ISO/ IEC 17025 regulation using a split mode injection. This method presented a good linearity (R²>0.999, Cm>99%), a wide range of calibration, the maximum random errors for repeatability and intermediate precision were 5% and 8%, respectively, and the maximum limit of quantifi cation and limit of detection were 14.1 mg l-1 and 4.6 mg l-1, respectively. Trueness, expressed as recovery (%), was successfully validated by means of two different methods, standard addition (92-110%) and comparison against reference materials (93-115%). Expanded uncertainty estimated at 95% confi dence level ranged between 11% for methanol and 7% for allyl alcohol. The validated method was successfully applied for the analysis of major volatiles in ciders and wines, and to detect yeast and lactic acid bacteria spoilage.
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A chromatographic method for the separation of volatile compounds in Asturian cider apple juices has been developed. For this separation purpose, a monocationic imidazolium-based ionic liquid bearing a reactive terminal iodine atom was synthesized by a quaternization-anion exchange chemical sequence. Next, the gas chromatography (GC) stationary phase was prepared by covalently linking the imidazolium monolith to the reactive silanol groups of the inner capillary wall at 70 °C. This coated GC column exhibited good thermal stability (290 °C), as well as good efficiency (2000 plates/m) in the separation of volatile compounds from Asturian apple cider juices, and was characterized using the Abraham solvation parameter model. The intra-day and inter-day precision of the chromatographic method was evaluated, obtaining relative standard deviations from 3.7 to 12.9% and from 7.4 to 18.0%, respectively. Furthermore, recoveries from 82.5 to 122% were achieved. Open image in new windowGraphical AbstractCovalent bonding of an ionic liquid to inner column wall led to a great improvement of the separation efficiencies of stationary phases in gas chromatography
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Ice cider is a high value specialty product that was developed in Quebec, Canada. It is typically very sweet and has an intense apple taste due to specific production practices. Other fruit wines can be produced at a lower cost, and there is a need for ice cider authentication methods. An experiment was conducted to determine the uniqueness of ice cider in terms of physico-chemistry. Simple laboratory procedures were considered in addition to infrared and fluorescence spectroscopy. One hundred bottles with vintages from 2001 to 2015 were collected. Besides, 11 comparable apple wines (CAW) were selected, including quiet, fortified, aperitif and fire ciders. In addition, 36 ‘laboratory wines’ (LW) were prepared by mixing various juices, ethanol and sugars. A linear discriminant analysis with variable selection was performed to classify products as ice cider or not. Input variables were results from laboratory test or scores from principal component analysis of spectra. Ninety four percent of ice ciders and 45% of CAW were correctly identified by simple laboratory tests but the method was not specific as 6 LWs were confused with ice cider. Infrared spectroscopy or fluorescence at 280, 330, 415 and 460 nm excitation wavelengths allowed for correct classification of 95% of samples and all LW. Infrared was poor at distinguishing CAW (45% correct classification) while fluorescence was better (73% correct classification). Measuring intrinsic fluorescence represents an opportunity for a simple and low cost for the authentication of ice cider.
Article
Varietal base ciders were produced from three varieties of dessert apples (‘Pink Lady®’, ‘Royal Gala’ and ‘Red Delicious’) at pre-commercial, commercial and post-commercial harvest timings. Rapid analytical methods were used to categorise the base ciders, and data analysed using principal component analysis (PCA). The titratable acidity of apple must was significantly higher for the pre-commercial harvest fruit for both the ‘Royal Gala’ and ‘Red Delicious’ varieties. The base cider phenolic content was highest in the pre-commercial harvest fruit for all varieties. ‘Red Delicious’ had the highest total phenolics as determined by spectral analysis and supported by the classification provided by the PCA analysis. The spectral fingerprints of the ciders showed two main peaks at approximately 280 nm and 320 nm indicating phenolic concentrations. Studies analysing characteristics of dessert apple varieties with relevance for cider production will allow for informed decision making for both apple producers and cider makers.
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Optimization of a multivariate calibration process has been undertaken for a Visible-Near Infrared (400-1100 nm) sensor system, applied in the monitoring of the fermentation process of the cider produced in the Basque Country (Spain). The main parameters that were monitored included alcoholic proof, L-lactic acid content, glucose+fructose and acetic acid content. The Multivariate calibration was carried out using a combination of different variable selection techniques and the most suitable pre-processing strategies were selected based on the spectra characteristics obtained by the sensor system. The variable selection techniques studied in this work include Martens Uncertainty test, interval Partial Least Square Regression (iPLS) and Genetic Algorithm (GA). This procedure arises from the need to improve the calibration models prediction ability for cider monitoring.
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The aim of this study was to identify the main amino acids responsible for the production of esters in ciders. The experiments were carried out in apple must and synthetic must. The amino acids were analysed by high-performance liquid chromatography and the volatile compounds by gas chromatography. Aspartate, asparagine and glutamate positively influenced the production of esters in the cider models and were used in the experiments with mixtures. The response surface generated by the proposed model yielded two regions that maximized the production of esters. In addition, the combination of aspartate and glutamate predicted a higher production. The optimal suggested concentrations were 43.4% of aspartate and 56.6% of glutamate for 120mg/L of total nitrogen. The apple must supplemented with these two amino acids resulted in four times more esters than in the same cider without supplementation, demonstrating the effectiveness of the proposed model.
Article
Multiple binary mixtures of different kinds of vinegars have been analyzed through UV-Vis absorption. Two types of mathematical models (multiple linear regression (MLR) and artificial neural network (ANN)) have been employed to identify and quantify the components of such blends. Six different vinegars were used to prepare these mixtures, each one with a particular botanical origin: white wine, red wine, apple cider, apple, molasses, and rice. The best results have been attained with the ANN based models, offering mean estimation error values averages of 1% (v/v) and mean correlation coefficients (R2) over 0.99. This model is adequate to perform the estimation and achieve an accurate and reliable tool. Nevertheless, although the MLR models provide worse results (0.88 in terms of R2 and 5% v/v error), they can be used depending on the application and required accuracy.
Article
Unfiltered vinegar samples collected from three oxidation cycles of the submerged industrial production of each, red wine and organic apple cider vinegars, were sampled in a Slovene vinegar producing company. The samples were systematically collected from the beginning to the end of an oxidation cycle and used for culture-independent microbial analyses carried out by denaturing high pressure liquid chromatography (DHPLC) and Illumina MiSeq sequencing of 16S rRNA gene variable regions. Both approaches showed a very homogeneous bacterial structure during wine vinegar production but more heterogeneous during organic apple cider vinegar production. In all wine vinegar samples Komagataeibacter oboediens (formerly Gluconacetobacter oboediens) was a predominating species. In apple cider vinegar the acetic acid and lactic acid bacteria were two major groups of bacteria. The acetic acid bacterial consortium was composed of Acetobacter and Komagataeibacter with the Komagataeibacter genus outcompeting the Acetobacter in all apple cider vinegar samples at the end of oxidation cycle. Among the lactic acid bacterial consortium two dominating genera were identified, Lactobacillus and Oenococcus, with Oenococcus prevailing with increasing concentration of acetic acid in vinegars. Unexpectedly, a minor genus of the acetic acid bacterial consortium in organic apple cider vinegar was Gluconobacter, suggesting a possible development of the Gluconobacter population with a tolerance against ethanol and acetic acid. Among the accompanying bacteria of the wine vinegar, the genus Rhodococcus was detected, but it decreased substantially by the end of oxidation cycles.
Article
Voltammograms recorded on the glassy carbon electrode (GCE) may be a chemical fingerprints of food samples, enabled distinguishing the origin of the considered products. In this work the objects of the study was 5 Polish ciders of various brands. For each sample 10 scans were recorded by DPV in the potential range between -0.2 and 1.0 V in Britton-Robinson buffer at pH 2.0. The signals preprocessing realized by baseline correction with 4-th degree polynomial and normalization (in 0 to 1 interval), performed to reduce problems with insufficient signal's repeatability associated with mechanical renovation of the electrode surface before each measurement. The PLS-DA classification models were built using the training set and then validated using the samples absent in the learning process. The final multi-class model with optimized complexity enables classification of the ciders with 100% sensitivity and specificity, with the exception of one cider, where specificity was 95% (for validation set).
Article
The identification of vinegars produced from six different raw materials (red wine, white wine, cider, apple, molasses, and rice) in blends has been accomplished through their UV-Vis spectra and different mathematical models: partial least squares discriminant analysis (PLS-DA) and artificial neural networks (ANNs). The registered spectra were mathematically treated following a linear (PLS-DA) approach and a non-linear one (ANN) based on multilayer perceptron models with different training functions. The average correct classification rate of a series of comparable internal validations was around 55% and 90%, for the PLS-DA and the ANN models respectively, which heavily favors the non-linear approach. Therefore, an accurate chemometric tool with the ability to detect specific vinegars in mixtures in an inexpensive and straightforward fashion has been designed and optimized.
Article
This research was conducted to evaluate the impact of co-fermentation with Saccharomyces cerevisiae and Williopsis saturnus var. mrakii on the volatile profile of cider. Cider co-fermentation was carried out by co-inoculating S. cerevisiae and W. saturnus var. mrakii at a ratio of 1:100. Changes in yeast cell population, total soluble solid content (degrees Brix [°Bx]), and pH were monitored. Volatiles were analysed using headspace solid-phase microextraction/gas chromatography–mass spectrometry/flame ionization detector (HS-SPME/GC-MS-FID). A diverse group of volatiles, including fatty acids, alcohols, aldehydes, esters and ketones, were identified, among which alcohols and esters were the predominant compounds. Although most of these compounds showed similar dynamics of change, the final concentrations of some volatiles differed significantly between single-culture and co-culture fermentations. Volatiles that were indigenous to apple juice decreased during fermentation, while production of isoamyl acetate, 2-phenylethyl acetate, ethyl acetate, ethyl decanoate, ethyl dodecanoate and ethyl octanoate varied significantly among the monocultures and co-culture. Co-fermentation by S. cerevisiae and W. saturnus resulted in a more complex volatile profile, which could impact on the aromatic characteristics of cider, thus representing a novel way to modulate flavour.
Article
This study was conducted to examine the influence of the following apple juice treatments on different parameters of cidermaking process: sulphiting (50 mg/L of total S02), clarification with pectolytic enzymes (Ultrazym 100 G, 3g/hL), and bentonite fining (lOOg/hL). The different treatments slowed down alcoholic fermentation, the greatest effect being found for the combination of the three treatments. With respect to malolactic fermentation, must sulphiting, with or without the other two treatments, delayed this process, which took place after alcoholic fermentation. The low levels of lactic acid bacteria during this period can explain this delay. The only treatment that had any significant influence on volatile acidity was sulphiting, either on its own or in combination with the other treatments. Thus lower acetic acid levels were detected in ciders treated with SO2.
Chapter
The word vinegar has been in use in the English language since the 14th century, when it arrived in the British Isles from the French vinaigre, a word that simply means ‘sour wine’, and that came in turn from the Latin vinum acre, ‘sour wine’ or, more commonly, vinum acetum, ‘wine vinegar’.
Chapter
Apple vinegar or cider vinegar (CV) is made with apple juice or concentrated apple juice (CAJ) through a double fermentation: alcoholic and acetic. Cider vinegar is extensively used in several countries including Austria, the UK, the USA and Switzerland (Ebner, 1982; Lea, 1988).
Article
The aim of this study was to evaluate the potential of integrated membrane processes for the clarification and the concentration of apple juice, taking into account the impact on the product quality. The fresh apple juice, with a total soluble solids (TSS) content of about 12°Brix was previously clarified by combined application of fining agents (gelatin and bentonite) and ultrafiltration (UF) through 10 kDa or 100 kDa molecular weight cut-off (MWCO) membranes on laboratory scale. The clarified juice was then concentrated by osmotic distillation (OD), membrane distillation (MD), coupled operation of OD and MD or by conventional thermal evaporation up to 65°Brix. The effect of different clarification and concentration processes on formation of 5-hydroxymethylfurfural (HMF), retention of bioactive compounds (phenolic compounds, organic acids, glucose, fructose and sucrose) and their efficiency in preserving natural color and aroma (trans-2-hexenal, the most relevant compound in apple juice aroma) were evaluated in order to maintain a high quality product. The new membrane-based concentration techniques were very efficient since the product characteristics were very similar to that of the initial apple juice especially regarding the retention of bright natural color and pleasant aroma, which are significantly lost during thermal evaporation. Furthermore, among all the concentration treatments applied, only thermally evaporated samples resulted formation of HMF. Phenolic compounds, organic acids and sugars were very stable against all concentration processes, including thermal evaporation. Coupled operation of OD and MD reduced trans-2-hexenal losses drastically tending towards that of the initial juice and hence can be proposed as the most promising alternative to conventional thermal evaporation technique.
Article
This paper studies the clarification of vinegars (white, rosé and red) by cross-flow microfiltration on an industrial scale. The reduction in turbidity for the three kinds of vinegars was notable: for filtered vinegars it was less than 0.5 NTU. The reduction of total solids in suspension was complete. These results show the utility of using microfiltration to simultaneously clarify and cold sterilise vinegar. The effect of microfiltration on colour and polyphenol content was acceptable. The colour reduction, expressed as a decrease in modified colour intensity, was practically negligible for white vinegars, 11% for rosé vinegar and 37% for red vinegar. The reduction in polyphenol content was less than 15% in all vinegars, and was largest for red vinegar, followed by rosé and finally white vinegar. The polyphenolic profile of the filtered vinegars is quite similar to that of the initial vinegar. The reduction in benzoic and hydroxycinnamic acids identified was less than 10% for all vinegars. However, the reduction in procyanidin B2 was total for rosé and red vinegars.
Article
Wine vinegar is produced in most Mediterranean countries and extensively used as a condiment, acidifying and food preserving agent. Traditional production requires maturation in wood for many years to obtain a high acetic degree and the resulting product is relatively expensive. New technologies are being designed to overcome this difficulty with the objective of producing vinegars with a similar quality and at the same time less expensive. These methods of production involve the use of submerged bacterial culture and a continuous aeration system. Recent research is focussed in improving yield and quality of the final product.
Association of Manufacturers and Formulators of Enzyme Products
AMFEP. 2018. Association of Manufacturers and Formulators of Enzyme Products (https:// amfep.org).
Chemistry and Technology of Soft Drinks and Fruit Juices, Third Edition
• P R Ashurst
Ashurst, P.R. (Ed.). 2016. Chemistry and Technology of Soft Drinks and Fruit Juices, Third Edition. Oxford: John Wiley & Sons, Ltd. B&P. 2018. B&P Engineering (www.engineering-bp.com).
• Bucher
Bucher. 2018. Bucher Unipektin AG, Switzerland (www.bucherunipektin.com).