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FOOD AND NUTRITIONAL ANALYSIS / Coffee, Cocoa, and Tea

Table 7 The content of D-isocitric acid and citric acid/D-isocitric acid ratio in different fruit juices Fruit juice
D-isocitric

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Applications: Food. Radiochemical Methods: Food and Environmental Applications.

acid content (mg l 1)

Citric acid/D-isocitric acid ratio 80130 5090 170260 120140 80200 15150

Further Reading
Gilbert J and Anklam E (2002) Validation of analytical methods for determining mycotoxins in foodstuffs. Trends in Analytical Chemistry 21: 468486. Heftmann E (ed.) (2000) Chromatography and Electrophoresis in Food Analysis. Amsterdam: Elsevier. Loureiro V and Querol A (1999) The prevalence and control of spoilage yeast in foods and beverages. Trends in Food Science & Technology 10: 356365. Mello LD and Kubota LT (2002) Review of the use of biosensors as analytical tools in the food and drink industries. Food Chemistry 77: 237256. Nollet LML (2000) Food Analysis by HPLC. New York: Marcel Dekker. Sancho T, Gimenez-Jurado G, Malfeito-Ferreira M, and Loureiro V (2000) Zymological indicators: A new concept applied to the detection of potential spoilage yeast species associated with fruit pulps and concentrates. Food Microbiology 17: 613624. Schaller E, Bosset JO, and Escher F (1998) Electronic noses and their application to food. Lebensmittel-Wissenschaft und-Technologie 31: 305316. Wetzel DLB and Charalambous G (eds.) (1999) Instrumental Methods in Food and Beverage Analysis. Amsterdam: Elsevier.

Orange Grapefruit Lemon Mandarin Raspberries Apricot

65200 140350 240420 7090 60220 70200

concentrations can be found in various fruits (Table 7). The determination of D-isocitric acid is important especially in the evaluation of citrus juices. Simple falsication of orange concentrate or juice by addition of sugars, citric acid, and water can be detected from the citric acid/D-isocitric acid ratio, which is usually lower than 130 in authentic orange juice.
See also: Carbohydrates: Sugars Chromatographic Methods. Fluorescence: Food Applications. Immunoassays, Applications: Food. Ion-Selective Electrodes: Food Applications. Mass Spectrometry: Food Applications. Nuclear Magnetic Resonance Spectroscopy

Coffee, Cocoa, and Tea


S Y Tse, Wyeth-Ayerst Research, Princeton, NJ, USA
& 2005, Elsevier Ltd. All Rights Reserved. This article is reproduced from the previous edition, pp. 1512 1517, & 1995, Elsevier Ltd.

Survey of Major Analytes


The major analytes of coffee include caffeine, chlorogenic acids, and avor and volatile aromatic components. The major analytes in cocoa are methylxanthines, mainly theobromine and trace amounts of caffeine, cocoa fat, and lipids. Other analytes of interest in cocoa are tannins, pigments, and aroma components. The major analytes of tea are the methylxanthine alkaloids, including caffeine and theophylline, polyphenols (catechins, tannins, and related avanols), and volatile and aromatic components. Analysis of black tea would also include theaavins and thearubigens, which are oxidation and condensation products of polyphenols.

Introduction
The beverages coffee, cocoa, and tea can be considered complex mixtures of naturally occurring substances (for example, methylxanthine alkaloids, avonoids, organic acids, pigments, and nutritional elements) and compounds generated during industrial processes, such as roasting, fermentation, and decaffeination. This article will provide a brief overview of the major chemical components commonly encountered in coffee, cocoa, and tea, together with the standard procedures for the extraction and analyses of these major components.

Sample Preparation and Extraction Techniques


Sample Preparation

Green coffee beans are ground to pass a No. 40 sieve before extraction and analysis. Roasted coffee beans

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and tea samples are ground to pass a No. 30 sieve before analysis. Soluble coffee solids, instant tea, and cocoa powder are analyzed after thorough mixing to ensure homogeneity. Cocoa products other than cocoa are extracted with petroleum ether to remove fat before extraction and analysis of alkaloids and other nonvolatile components.
Extraction Techniques

Methylxanthine alkaloids Caffeine in coffee and tea The BaileyAndrew method, the PowerChesnut method, and the Levine method have been adopted by the Association of Ofcial Analytical Chemists (AOAC) for the extraction and determination of caffeine in coffee and tea. In the BaileyAndrew method, 510 g of ground sample is weighed into a 1 l Erlenmeyer ask with 500 ml of water. The mixture is heated to boiling, and 10 g of magnesium oxide (MgO) is added. The mixture is boiled over low ame for a period of 2 h, water being added periodically to prevent frothing. After cooling, water is added to make to weight (1000 g) and the mixture is ltered. Twenty milliliters of sulfuric acid is added to 200 ml of clear ltrate. The acidied sample is extracted successively with 25, 20, 15, 10, 10, 10 ml portions of chloroform. Five milliliters of potassium hydroxide solution (1%) is added to the pooled chloroform extract. The remaining aqueous potassium hydroxide layer is washed with two 10 ml portions of chloroform. All chloroform portions are collected into a Kjeldahl ask. After evaporation of the chloroform, the amount of caffeine extracted is determined by measuring the total nitrogen (Kjeldahl method). In the PowerChesnut method, 10 g of coffee sample is transferred into a Soxhlet extractor with ethanol, and extracted with ethanol for up to 8 h. The ethanolic extract is transferred into a porcelain dish containing 10 g of high-density MgO and 100 ml of water. Ethanol in the mixture is evaporated by slow heating on a steam bath. The residue is moistened with hot water and ltered into a 1 l ask. The ltrate is acidied with 20 ml of sulfuric acid and brought to boiled for 30 min. After cooling, the acid extract is ltered into a separator. The ltrate is extracted with chloroform (six 25 ml portions). The combined chloroform extract is washed with 5 ml of 1% KOH solution. The chloroform phase is drained into an Erlenmeyer ask and the KOH portion is washed with two portions of chloroform (10 ml each). All chloroform extracts are pooled, and the volume of extract is reduced to 10 or 15 ml by distillation. The remaining chloroform extract is transferred to a weighing beaker, and the residual solvent is

evaporated. The residue is dried for 30 min at 1001C. The amount of caffeine is determined by weighing or by nitrogen determination using the Kjeldahl method. The Levine method is used in preparing samples for the spectrophotometric determination of residual caffeine in decaffeinated coffees. An acidic Celite column is prepared by adding 2 ml of sulfuric acid (4 mol l 1) to 2.0 g of Celite 545. The mixture is transferred into a 25 mm ID 250 mm glass column plugged with ne glass wool at both ends. A basic column is prepared by mixing 3 g of Celite 545 with 2 ml of sodium hydroxide (2 mol l 1); this is then transferred into a 25 mm ID 250 mm glass column with a ne glass wool plug at the bottom. Coffee sample (1.0 g decaffeinated coffee or 0.5 g decaffeinated soluble coffee) is treated with 5 ml of ammonia solution and heated over a steam bath for 2 min. Six grams of Celite 545 is added to adsorb the alkaline mixture and the alkalicoffeeCelite mixture is applied directly onto the basic Celite column. The basic column is mounted on top of the acidic column. Water-saturated ether (150 ml) is passed through both basic and acidic columns. The acidic column is washed with an additional 50 ml of ether. The ether portions are discarded. Caffeine is eluted from the acidic column with 50 ml of water-saturated chloroform solution. Theobromine in cocoa The Wadsworth method is used for the extraction of theobromine from cocoa powder or defatted cocoa products. Ten grams of sample is put in a porcelain dish and mixed with 2 3 g of fresh calcined MgO. Water (920 ml) is added, a few milliliters at a time, and mixed thoroughly to ensure uniform consistency and wetting of all particles. The mixture is heated on a steam bath for 30 min, with mixing at regular intervals to maintain uniform consistency and to prevent drying. After heating, the mixture is transferred into a 250 ml ask and refluxed with 150 ml of tetrachloroethane for 30 min. The hot extract is ltered into a 200 ml ask. The residue is refluxed with three additional portions of tetrachloroethane (120 ml) for up to 30 min. Solvent in the 200 ml ask is removed by distillation after each reux and ltration step, until the volume is reduced to between 3 ml and 5 ml. The residue is cooled and treated with 65 ml of ether, mixed by swirling the ask. The ether mixture is stoppered and left standing until the supernatant is clear (up to an hour or more). The ether mixture is ltered with preweighed ltered paper and dried at 1001C. The weight of precipitated theobromine collected after ltration and removal of ether is determined by weighing. A correction of 0.004 g is added to account for the amount of theobromine dissolved in the ether.

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An aqueous extraction method is used to extract both the theobromine and caffeine from defatted cocoa products for analysis by liquid chromatography (LC). In this method, 0.6 g of cocoa is placed in an extraction tube with a polytetrauoroethylene-lined screw cap. The sample is extracted twice with 30 ml portions of petroleum ether, centrifuged, and the ether phase, which contains fat, is discarded. The residue, after removing all residual solvent, is transferred into an Erlenmeyer ask with boiling chips and added with 95 ml of water. The mixture is boiled for 25 min. After cooling, several portions of the mixture are transferred into screw-capped centrifuge tubes and centrifuged at 2000 g for 5 min. The supernatant is ltered through a 0.45 mm membrane lter, and the ltrate is analyzed by LC. Organic Acids, polyphenols, and lipids Chlorogenic acids in coffee One gram of roasted ground coffee is transferred into a 750 ml Erlenmeyer ask. Boiling water (400 ml) is added, and the mixture is boiled gently for 15 min, then cooled rapidly under cold tap water. The mixture is transferred into a 500 ml volumetric ask, diluted to volume, and ltered. The rst 2550 ml of the ltrate is discarded. Chlorogenic acid in the ltrate is determined by a spectrophotometric or chromatographic method. For soluble coffee solids, 0.35 g of sample is transferred into a 500 ml ask and diluted to volume. For green coffee, 0.7 g of ground sample is extracted with petroleum ether (25 ml) in a 50 ml centrifuge tube. After mixing and centrifugation, petroleum ether is removed by decanting. The residue is washed with two additional portions of petroleum ether. Residual solvent is removed by drying under a stream of dry air. The residue is transferred with a few milliliters of water into the 750 ml Erlenmeyer ask. Boiling water is added and the sample is extracted following the same procedure as in roasted coffee. Alternative extraction procedures using aqueous alcohols have also been employed. Cocoa fat and lipids The lipid components in cocoa are extracted into petroleum ether by either the Knorr Tube method or by Soxhlet extraction. Both are adopted by AOAC, and the latter method by both AOAC and the Ofce International du Cacao et du Chocolat. In the Knorr Tube method, 23 g of cocoa powder or grated chocolate product is transferred into a Knorr Tube tted with 6 mm of tightly packed mat of washed asbestos lter. The extraction tube is connected to suction by a two-way stopcock, and the stem of the extraction tube is connected to a preweighed Erlenmeyer ask. The extraction tube is lled up to two-thirds capacity by petroleum ether.

After thorough mixing, the ether phase is separated by standing, and drained into the Erlenmeyer ask by suction. The extraction process is repeated up to 10 times for complete extraction of fat. The solvent is evaporated and the sample is dried at 1001C. The amount of fat in the sample is determined by weighing. In the Soxhlet method, 45 g of cocoa powder is placed in a 500 ml beaker and treated with 45 ml of boiling water with stirring. The mixture is acidied with hydrochloric acid (8 mol l 1, 55 ml). Antibumping beads are added and mixture is boiled for 15 min. The acid digest is ltered after boiling and cooling. The beaker is rinsed several times with water until the ltrate is free of chloride, as tested by adding 0.1 mol l 1 silver nitrate. The lter paper with the collected residue is put in an extraction thimble and dried in a small beaker at 1001C for 618 h. The dried extraction thimble is placed in a Soxhlet extractor. The digestion beaker and drying beaker are washed with 50 ml portions of petroleum ether into the extraction thimble. The sample is refluxed for 4 h with gentle heat. The extraction solvent is siphoned into a preweighed Erlenmeyer ask. The solvent is subsequently removed by distillation on a steam bath, and the ask is dried at 1001C for up to 2 h. The amount of fat is determined by weighing. Tannins and pigments in cocoa Tannins and coloring matters in defatted cocoa powder and related products can be extracted by shaking consecutively with 150 ml and 100 ml portions of acidied 82% ethanol (10 ml HCl and 432 ml ethanol, diluted to 500 ml with water), at 551C. The solvent is separated by centrifugation. Ethanolic extracts are pooled and evaporated. Alternatively, tannins and catechins in acetone extract can be precipitated with cinchonine sulfate and measured gravimetrically. In this extraction method, 25 g of sample is extracted overnight with 40% acetone (200 ml, cold). The acetone extract is ltered through a Whatman No. 41 paper. The residue is washed with 20 ml of 40% acetone. Water is added to make up to 250 ml. Saturated cinchonine sulfate (150 ml) is added to 25 ml of tannin-containing ltrate. The precipitate formed is ltered off and dried. The dried weight is multiplied by 0.534 to obtain the tannin content. Catechins, polyphenols, and tannins in tea Catechins and related avanols are water soluble, and can be extracted by boiling with water, or by shaking with aqueous acetone. Volatile and aromatic components Volatile and aromatic components in coffee are concentrated by

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passing puried helium gas directly over the sample (50 g of ground coffee) or the beverage (made from 2 g of coffee). The gas is aspirated through an adsorption tube (60 mm 4 mm ID) containing 90 mg of a porous polymer (Tenax, 60/80 mesh, preconditioned for 24 h at 3001C in helium). Aromatic components are desorbed by heating and swept into the injection port of a gas chromatograph for the analysis of individual components. Volatile and aromatic components of tea and tea infusion are also concentrated by aqueous distillation and the cold-trapping method. In this method, the sample is suspended in water in a 2 l round-bottomed ask connected to a rotary evaporator. The condenser is connected to cold traps containing freezing mixture ( 151C to 181C) or dry iceacetone mixture ( 781C). The aqueous mixture is distilled twice at 701C, 2530 mmHg. The distillate is saturated with sodium chloride and extracted with ether. The ether extract is dried over anhydrous sodium sulfate and concentrated by distillation of the solvent at 401C. Components in the ether extract are analyzed by gas chromatography.

caffeine in decaffeinated coffees. Other methods using alumina columns (KumTatt method), alkaline extraction, and combinations of various types of columns have also been used in sample cleanup. Thin-layer chromatography Methylxanthines analysis by TLC has the advantages of high sample throughput and low cost. The major disadvantage of TLC methodology is its nonquantitative nature. Separation is achieved by chromatography on silica gel plates, using a variety of organic solvent mixtures as eluting solvents. Some typical solvent mixtures are: chloroformmethanol (9:1; v/v); benzeneacetone (3:7; v/v); chloroformcarbon tetrachloridemethanol (8:5:1; v/v/v); chloroformethanolformic acid (88:10:2; v/v/v). Separation of methylxanthines has also been achieved using paper chromatography or with cellulose plate using a butanolhydrochloric acidwater (100:11:28; v/v/v) mixture. Liquid chromatography Analysis of methylxanthines by LC is carried out with C18 reversed-phase columns, with acidic buffer mobile phases, and monitoring by UV absorption at B270280 nm, or at 254 nm. The LC procedure adopted by the AOAC for the analysis of caffeine utilizes a mBondapak (Waters) C18 column, with a mobile phase of watermethanolacetic acid (74:25:1; v/v/v) and detection at 280 nm. Other solvent systems, such as wateracetonitrileacetic acid (81:18:1; v/v/v) and phosphoric acid (7 mmol l 1)acetontrilemethanol (92:4:4; v/v/v), have also been used successfully in separating methylxanthines in foods and beverages. LC methods using normal-phase columns, such as Lichrosorb Si-60, with mobile phase composition of chloroform2-propanolacetic acid (96:2:2 or 92:7:1; v/v/v) and detection at 275280 nm have also been applied to the analysis of methylxanthines, but are less robust. Quantication of methylxanthines is achieved by using either external standards or by using xanthine derivatives as internal standards; examples are 8-chlorotheophylline and 8-hydroxy-ethyltheophylline. Gas chromatography The AOAC method for the analysis of caffeine by GC uses a packed glass column, 6 ft (B180 cm) in length by 4 mm ID, packed with 10% DC-200 oil on 80100 mesh Gas Chrom Q, using nitrogen carrier gas and a thermionic potassium chloride detector. The injector temperature is 2201C, the column temperature is 1901C, and the detector temperature is 2201C. A wide variety of column-packing materials and detection modes can be used. For example, separation of caffeine, theophylline, and theobromine can be achieved with

Analytical Procedures
Coffee

Caffeine The analyses of methylxanthines in coffee and tea are conducted: (1) by measuring the total nitrogen in extracts, either derived from the Bailey Andrew extraction in the case of caffeine or by the Wadsworth method in the case of theobromine; (2) by spectrophotometric methods; and (3) by chromatographic methods, including thin-layer chromatography (TLC), LC, and gas chromatography (GC). The major advantage of chromatographic methods over spectrophotometric methods is the ability of the former to separate and quantify several methylxanthines (caffeine, theophylline, and theobromine) simultaneously. Spectrophotometric methods for the analysis of caffeine Caffeine is quantied spectrophotometrically by measuring the ultraviolet (UV) absorbance at wavelengths between 270 and 280 nm. The major drawback of such methods is the presence of interfering substances. Such interferences can be reduced, but not eliminated, by using derivative techniques. Sample cleanup by various types of columns and background correction procedures is used to purify caffeine before spectrophotometric measurement. For example, in the Levine method, sample cleanup is achieved by a series of acidic and basic Celite columns. This method is adopted by AOAC for the analysis of

FOOD AND NUTRITIONAL ANALYSIS / Coffee, Cocoa, and Tea

283

3% OV-17 on Gas Chrom Q (100120 mesh) by isothermal or temperature programming, with electron-capture detector, ame ionization detector (FID), or nitrogenphosphorus detector (NPD). Chlorogenic acids Spectrophotometric analysis Spectrophotometric determination of total chlorogenic acid content in green coffee extract is conducted by measuring the absorbance at 324 nm, as in the AOAC standard procedures. Modication of this method by purication and extraction of the sample has been applied to eliminate interferences in roasted coffee. The formation of colored complexes with borates, molybdates, and periodates enables more accurate determination of specific classes of chlorogenic acids. Gas chromatography The complete separation and analysis of chlorogenic acids by capillary GC requires derivatization of the phenolic or carboxylic acid functions by silylating agents, such as hexamethyldisilazane or N,O-bistrimethylsilylacetamide, or a mixture of both. Liquid chromatography Analyses of chlorogenic acids are carried out with reversed-phase LC systems, both in gradient and isocratic modes. The typical analytical system employs C18 columns of 5 mm packing, with a mobile-phase gradient of 2547.5% methanol in pH 2.5 citrate buffer (0.025 mol l 1), or isocratic elution with 30% methanol in pH 2.5 citrate buffer (0.025 mol l 1), with UV detection at 310330 nm. Volatile and aromatic components Separation of volatile components is achieved on either fused silica capillary columns or packed columns. Individual volatile components are detected with a FID and identied by the use of reference standards. Methods using specific detectors, such as the NPD, sulfurspecific ame photometric detector, and mass-selective detector (MSD) have also been used. The MSD has the additional advantage of providing structural identication of the individual components.
Cocoa

a nominal back-pressure of 2000 psi (B14 000 kPa). Concentrations of theobromine and caffeine in cocoa extracts are determined from a calibration graph, using the external standard method. Cocoa fat and lipids In AOAC methodologies, the composition of fat and fatty acids in cocoa fat extracts are analyzed and characterized by physicochemical methods, including refractive index, melting point, saponication value and unsaponiable material, iodine number, ReichertMeissl and Polenske values. Volatile and aromatic components Cocoa volatile and aromatic components are analyzed by capillary GC, with samples derived from headspace enrichment or cold-trapping techniques. Analysis is similar to that of coffee volatiles; FIDs are used and identication is by the use of reference compounds.
Tea

Methylxanthines: caffeine and theophylline The amount of caffeine in tea is determined by spectrophotometric and chromatographic methods, as described above for coffee. Separation of caffeine from theophylline is achieved by chromatographic methods. Polyphenols: catechins and avanols Flavanols and tea polyphenols are commonly analyzed using paper chromatography, TLC, and LC. GC has also been used, but derivatization of the hydroxyl groups with silylation is required to increase the volatility of these analytes. Paper chromatography and thin-layer chromatography Tea avanols can be separated by two-dimensional paper chromatography, using water as the rst dimension solvent, and a mixture of butanolacetic acidwater (4:1:5; v/v/v) as the second dimension. A similar procedure can be carried out using TLC with cellulose plates. Different avanol components are visualized by uorescence under UV radiation, either before or after exposure to fuming ammonia. Other visualizing agents are bis-diazotized benzidine and vanillin. Liquid chromatography Separation and quantitative analysis of avanols and polyphenols may be conducted by C18 reversed-phase LC methods, using either isocratic or gradient modes. In one example of the isocratic separation method, the solvent system used consists of acetic acidmethanoldimethylformamidewater (1:2:40:157; v/v/v/v). Eluting peaks are monitored by UV absorption at 254 nm.

Theobromine and caffeine Separation and quantitative analyses of theobromine and caffeine are carried out using C18 reversed-phase columns, with monitoring by UV absorption at 280 nm. In the AOAC method, a Waters LC system is used, with a mBondapak C18 column, 30 cm length 4 mm ID and 10 mm packing. The mobile phase is methanol acetic acidwater (20:1:79; v/v/v) at 1 ml min 1 with

284 FOOD AND NUTRITIONAL ANALYSIS / Coffee, Cocoa, and Tea

Gas chromatography The utility of GC for the analysis of catechins and polyphenols is quite limited, given the polar and nonvolatile nature of these compounds. Derivatization of a polyphenol extract with silylating agent and subsequent separation of the trimethylsilyl derivatives of avanols can be achieved by chromatographing on a glass column 5 ft (B150 cm) in length 4 mm ID packed with 3% OV-1 on diatomite. Tannins, theaavins, and thearubigens Tannins and theaavins are pigmented products in black tea formed after oxidation and condensation of green tea avanols during the fermentation process. These compounds are analyzed by spectrophotometric, colorimetric, and chromatographic methods, using LC and GC. Spectrophotometric and colorimetric methods Spectrophotometric analysis of theaavins is carried out at 380 and 460 nm on isobutyl methyl ketone or ethyl acetate extracts of black tea infusions. Theaavins are also determined by using Flavognost reagent (diphenyl boric acid ethanolamine), which forms a green chromophore by reacting with the benztropolone nucleus of theaavins. The color developed is measured at 600 nm. Liquid chromatographic methods Separation and quantitative analysis of theaavins and thearubigens has also been achieved by gel permeation chromatography on Sephadex LH-20, monitoring the eluting peaks at 380 nm. Reversed-phase LC separation has also been conducted using a C18 column, with a mobile phase consisting of 29% aqueous acetone and 1% acetic acid.

decrease in the ratio of 2-methylfuran to 2-butanone in coffee aroma with time has also been observed. However, the use of such ratios of individual aroma components as measures of coffee quality has not been ofcially established.
Cocoa

Quality evaluation of cocoa bean and cocoa powder is by visual inspection for contamination, moldiness, and by aroma/avor and tasting. Physical analysis of cocoa bean and cocoa powder includes analysis for total moisture (o8%) and fat (o55%). Additionally, the quality of cocoa is characterized by the iodine number (degree of unsaturation of the fatty acid components), unsaponiable matter, and GC analysis (for volatile and aroma components).
Tea

Quality assessment of tea is conducted by evaluation of the color and appearance of the tea leaves and the tea infusion formed, as well as by GC analysis of the aroma of both the tea leaves and the infusion. For example, (Z)-3-hexenyl hexanoate is a major contributor to the aroma of fresh green tea. This component is found to decrease with storage. The astringent taste of tea is mainly due to the presence of unoxidized avanols and polyphenolics (e.g., catechins). Gradual and continued oxidation of these components with storage time would result in changes in both color and taste of the product. The brothy taste of green tea is due to the presence of amino acids, notably L-threonine. A decrease in the amino acid contents during storage would also result in deterioration of quality.

Limitations of Current Technology Analysis of Coffee, Cocoa, and Tea for Despite the fact that major components in coffee, cocoa, and tea can be analyzed and measured by the Quality Assurance Purposes
Coffee

The avor and aroma qualities of the common coffee beverages are dependent on the source of the coffee bean used, soil and climatic conditions, as well as the duration and temperature of roasting. The determination of the quality of roasted coffee is mainly by tasting of the brew by professional tasters. Such processes are qualitative only. Chemical analysis of coffee quality is based on headspace analysis of the aroma components of roasted or brewed coffee. For instance, drastic decreases in methylfuran and methylethylketone in coffee aroma have been observed in roasted and ground coffee within a few days, which may be correlated to coffee staleness. A

methodologies outlined above, there are many minor components in these beverages that have not been extensively studied. For example, roasting of coffee induces caramelization, condensation, pyrolysis, and Maillard reactions; the nature and composition of these reaction products (collectively termed melanoidins) are dependent on the temperature and duration of roasting. Although these reaction products in roasted coffee constitute as much as 30% of dry weight, their chemical identities are largely unknown. The relationship of melanoidin content to quality, taste, and avor of the product is not well understood and analytical procedures for determining these components are lacking. The manufacturing processes of black tea involve extensive oxidation and polymerization of

FOOD AND NUTRITIONAL ANALYSIS / Alcoholic Beverages 285

polyphenols and results in the formation of theaavins and thearubigens. The formation of these condensation products is dependent on the duration of oxidation during fermentation. Analytical methods for the characterization of aroma components remain to be established and the relationship between individual components and product quality has yet to be elucidated.
See also: Derivatization of Analytes. Extraction: Solvent Extraction Principles. Food and Nutritional Analysis: Contaminants; Oils and Fats. Gas Chromatography: Detectors. Lipids: Fatty Acids. Liquid Chromatography: Food Applications. Sample Handling: Comminution of Samples. Sensory Evaluation. Spectrophotometry: Organic Compounds.

Further Reading
AOAC (1990) Ofcial Methods of Analysis, 15th edn., vols. I and II. Arlington, VA: Association of Ofcial Analytical Chemists, Inc.

Chatt EM (1953) Cocoa: Cultivation, Processing, Analysis. New York: Interscience. Charalambous G (1978) Analysis of Foods and Beverages, Headspace Techniques. London: Academic Press. Charalambous G (1986) Handbook of Food and Beverage Stability: Chemical, Biochemical, Microbiological, and Nutritional Aspects. London: Academic Press. Charalambous G and Inglett G (1983) Instrumental Analysis of Foods, Recent Progress, vol. 2. London: Academic Press. Clarke RJ and Macrae R (1985) Coffee, vol. 1, Chemistry. London: Elsevier Applied Science. Sivetz M (1963) Coffee Processing Technology. Westport: AVI Publishing Co. Sievetz M and Desrosier NW (1979) Coffee Technology. Westport: AVI Publishing Co. Spiller GA (1984) The Methylxanthine Beverages and Foods: Chemistry, Consumption, and Health Effects. New York: Alan R. Liss. Willson KC and Clifford MN (1992) Tea: Cultivation to Consumption. London: Chapman & Hall.

Alcoholic Beverages
J F Cacho and R Lopez, University of Zaragoza, Zaragoza, Spain
& 2005, Elsevier Ltd. All Rights Reserved. This article is a revision of the previous-edition article by Xuejun Zhang, pp. 15041512, & 1995, Elsevier Ltd.

Introduction
Alcoholic beverages comprise a large group of beverages that contain varying amounts of alcohol (ethanol). Alcoholic beverages produced on an industrial scale include beer, wine, and China rice wine, and distilled spirits such as brandy, whisky, rum, gin, cognac, vodka, tequila, pisco, and China distilled spirit. The components of alcoholic beverages are highly complex and over 1300 compounds have been identied in various beverages. The constituents of each alcoholic beverage can be divided into major, minor, or trace components. The major constituents usually consist of ethanol and water. The minor or trace constituents are fusel alcohols, organic acids, carbonyl compounds, esters, aldehydes, lactones, sulfur compounds, sugars, preservatives, and colorants. There are two general approaches to analyzing the components of alcoholic beverages. The rst, and most usual, is by using

chemical and physiochemical analysis. The other is to use sensory evaluation. In recent years, instrumental analytical methods have become an important tool for analyzing minor and trace constituents of alcoholic beverages. The most widely used methods are ultraviolet (UV)visible spectrophotometry, gas chromatography (GC), liquid chromatography (LC), mass spectrometry (MS), and paper chromatography, and thin-layer chromatography. This article will review the methods applied for the determination of major and minor components in alcoholic beverages.

Sensory Assessment
Sensory assessment is a scientific discipline used to evoke, measure, analyze, and interpret responses to those properties of a substance (food or beverage) that are perceived by the ve human senses: sight, smell, taste, touch, and hearing. Even though individual judgments are subjective, the techniques of sensory evaluation use objective scientific testing methods principally based on working with a panel of assessors. Two types of analytical objective tests can be observed: (1) The discriminative tests: is there a difference between several products? (2) The

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