Effect of different extraction methods on the recovery of chlorogenic acids,caffeine and Maillard reaction products in coffee beans

Water and ethanolic extracts were obtained from green and roasted (3 different roast degrees) Arabica and Robusta coffee beans. Three types of water extracts were prepared from the examined, finely ground material through: (a) brewing with boiling water, (b) boiling in water, and (c) boiling in water under elevated pressure. All these extracts were lyophilized. Two types of ethanolic extracts were derived from the examined material through (a) extraction of the finely ground coffee beans and (b) extraction of the solid residue that remained after boiling the coffee beans in water under elevated pressure. These ethanolic extracts were dried. Both water and ethanolic extracts were analyzed for concentration of potential antioxidants such as chlorogenic acids and caffeine (by HPLC) and Maillard reaction products (measurements of absorbance at 420 nm). Concentration of chlorogenic acids in Robusta extracts varied between 0.4 and 36.0 g × 100 g⁻¹ dry extract weight (db.), while in Arabica extracts it ranged from 0.1 to 22.4 g × 100 g⁻¹ db. Extracts of dark roasted Arabica contained more chlorogenic acids than those of Robusta. Concentration of caffeine, which in green and roasted coffee beans is maintained at the similar level, tended to increase in Robusta extracts with the roast degree and temperature of extraction with water, while in case of Arabica extracts there was no noticeable tendency. Caffeine concentrations varied between 0.12 and 8.41 g × 100 g⁻¹ db. and between 0.03 and 6.53 g × 100 g⁻¹ db. in Robusta and Arabica extracts, respectively. Ethanolic extracts were characterized by relatively higher caffeine concentrations and lower contents of brown pigments and chlorogenic acids as compared to water extracts. The richest in antioxidants were extracts of green Robusta coffee beans derived through boiling in water under elevated pressure.     

Consumption of green coffee and the risk of chronic diseases

ABSTRACT

Green coffee contains macro nutrients such as carbohydrates, protein, fat, as well as minor components such as caffeine, trigonelin and chlorogenic acid. Phenolics, chlorogenic acids and brown pigments are sources of natural antixodants. High polypehonic materials found in green coffee and especially chlorogenic acid in it have an important place. It is considered that; green coffee has effects on body mass, blood glucose and lipid levels, blood pressure, prevention from cardiovascular diseases which is based on chlorogenic acid consisting antioxidant activity. However, many topics like toxicological effects, doses, amounts, usage in the body, advantages and disadvantages, etc. of these active molecules need to be examined. For these reasons this article was rewieved to evaluate health effects of green coffee.     

Microwave-assisted extraction of chlorogenic acids from green coffee beans

Microwave-assisted extraction (MAE) has been considered as a potential alternative to conventional solvent extraction for the isolation of phenolic compounds from plants. Aqueous and alcoholic extracts of green coffee bean obtained by MAE were quantitatively analysed for total yield of extracts, chlorogenic acids, caffeine and total polyphenol content. The extracts were also evaluated for radical-scavenging activity, using 1,1-diphenyl-β-picrylhydrazyl radical. Under optimum conditions of time (5 min), temperature (50 °C) and wattage (800 W), the maximum chlorogenic acids and caffeine could be extracted with water as solvent. The extracts contained chlorogenic acids and caffeine in the ranges of 31–62% and 22–40%, respectively. The yields of MAE under optimum conditions were higher than those from the conventional solvent extraction at 5 min and 50 °C and the extracts showed radical-scavenging activity of >75%, even at the concentration of 25 ppm. The MAE process can thus be predicted and controlled for industrial application.     

基于高效液相色谱法分析烘焙程度对咖啡中绿原酸含量的影响（网络首发、推荐阅读）

探究烘焙程度对10支不同产地（产地一：云南，产地二：非洲，产地三：美洲）卡蒂姆咖啡豆中7种绿原酸化合物含量影响。采用高效液相色谱法测定生豆和烘焙豆中绿原酸、新绿原酸、隐绿原酸、异绿原酸A、异绿原酸B、异绿原酸C和5-阿魏酰奎宁酸含量。经响应面法优化7种绿原酸化合物的最佳提取条件为100 mL 0.1%磷酸溶液沸水浴提取30 min，7种绿原酸化合物在2~150 mg/L质量浓度范围内，线性相关系数良好，相关系数均大于0.999 4，方法检出限0.005~0.500 mg/g，定量限0.02~2.00 mg/g，咖啡生豆中绿原酸的含量最高，其次是5-阿魏酰奎宁酸。随着烘焙程度增加，绿原酸和5-阿魏酰奎宁酸含量显著降低（P<0.05），新绿原酸和隐绿原酸含量先升高再降低，异绿原酸A的降解速度明显高于异绿原酸B和异绿原酸C，绿原酸、5-阿魏酰奎宁酸的降解速度与其余5种绿原酸相比，较为稳定。通过对不同烘焙程度下7种绿原酸化合物含量变化的研究，可以进一步针对咖啡绿原酸功效成分进行评价，为咖啡烘焙和品质控制提供参考依据。     

Separation and characterisation of chlorogenic acid‐rich conserves from green coffee beans and their radical scavenging potential

Methanolic extract (Me₁) obtained from low‐grade green coffee beans (LCB), which is one of the major by‐products in the coffee industry, was enriched with phenolics by different methods viz., partitioning in solvents, chromatographic separation using dowex & diaion HP20 resins and precipitation by lead acetate. Separated fractions and Me₁ were analysed for total polyphenol, chlorogenic acid, caffeine and radical scavenging activity (RSA). Chlorogenic acid isomers of Me₁ and the isolated fractions were analysed by HPLC. Me₁ found to contain total polyphenol (16.60 ± 0.4%), chlorogenic acids (CGAs) (29.60 ± 0.9%), caffeine (7.52 ± 0.2%) and exhibited RSA (92.50%) at 100 ppm concentration. Precipitation method resulted significantly (P ≤ 0.05) higher phenolics (46.33 ± 0.5%) as well as CGAs (43.50 ± 0.7%). HPLC analysis indicated that the composition of 5‐Caffeoylquinic acid (5‐CQA) was more in all the isolated fractions.     

Micronised-roasted coffee from unripe fruits improves bioactive compounds and fibre contents in rice extruded breakfast cereals

Unripe green coffee is one of the by-products from coffee processing that does not have many applications in higher value-added food products. This study aimed to evaluate the chemical, technological, and sensory properties of rice-based breakfast cereal made with micronised-roasted coffee (MRC) from green coffee fruits. The products were elaborated with different MRC concentrations (2, 5 and 9%) and manufactured in a single screw extruder. Data were analysed by analysis of variance and Tukey's test (p < 0.05). The increase in MRC concentration improved the contents of caffeine, chlorogenic and caffeic acids in the breakfast cereals, and reduced the luminosity and expansion index due to the presence of brown colour and fibres from coffee beans. The cereal made with 5% of MRC was more accepted by consumers. Thus, MRC has proven to be a potential source of bioactive compounds, fibres and natural brownish colour for breakfast cereals.     

Geographical and genotypic segmentation of arabica coffee using self-organizing maps

Several statistical methods have been developed in an attempt to reproduce the human capability of pattern recognition. Self-organizing maps (SOMs) are a type of artificial neural network (ANN) with unsupervised learning designed to examine the structure of multidimensional data. This study aimed to conduct a segmentation of the geographical and genotypic coffee grown in the coffee region of Paraná — Brazil using the SOM for cluster analysis. Fourteen arabica coffee genotypes from two different cities were collected (Paranavaí and Cornélio Procópio). Density, caffeine, chlorogenic acids, tannins, total and reducing sugars, proteins, and lipids of the green coffee beans were analyzed. Using these data, the SOM was able to discriminate the 14 genotypes and also segmentation of the geographical origin was observed. Reducing sugars, caffeine, and chlorogenic acid were the most important variables for separation of the region of cultivation of arabica coffee genotypes. It was concluded that the SOM was able to recognize the coffee genotypes and geographical origin using the chemical profile data.     

Correlation between cup quality and chemical attributes of Brazilian coffee

Brazilian arabica coffee is classified for trading according to the quality of the beverage obtained after roasting and brewing. In the present study, Brazilian green and roasted coffee beans were investigated for possible correlations between cup quality and the levels of sucrose, caffeine, trigonelline and chlorogenic acids, determined by HPLC analysis. Trigonelline and 3,4-dicaffeoylquinic acid levels in green and roasted coffee correlated strongly with high quality. To a lesser extent, caffeine levels were also associated with good quality. On the other hand, the amount of defective beans, the levels of caffeoylquinic acids (predominantly 5-caffeoyilquinic acid), feruloylquinic acids, and their oxidation products were associated with poor cup quality and with the Rio-off-flavor. The fact that similar correlations between cup quality and chemical attributes were observed in green and light roasted samples – the latter used for coffee cup classification – indicates that chemical analysis of green beans may be used as an additional tool for coffee quality evaluation.     

Comparison of nine common coffee extraction methods: instrumental and sensory analysis

The preparation of a cup of coffee may vary between countries, cultures and individuals. Here, an analysis of nine different extraction methods is presented regarding analytical and sensory aspects for four espressi and five lunghi. This comprised espresso and lungo from a semi-automatic coffee machine, espresso and lungo from a fully automatic coffee machine, espresso from a single-serve capsule system, mocha made with a percolator, lungo prepared with French Press extraction, filter coffee and lungo extracted with a Bayreuth coffee machine. Analytical measurements included headspace analysis with HS SPME GC/MS, acidity (pH), titratable acidity, content of fatty acids, total solids, refractive indices (expressed in °Brix), caffeine and chlorogenic acids content with HPLC. Sensory analysis included visual, aroma, flavor and textural attributes as well as aftersensation. The technical differences in the extraction methods led to a higher concentration of the respective quantities in the espressi than in the lunghi. Regarding the contents per cup of coffee, the lunghi generally had a higher content than the espressi. The extraction efficiency of the respective compounds was mainly driven by their solubility in water. A higher amount of water, as in the extraction of a lungo, generally led to higher extraction efficiency. Comparing analytical data with sensory profiles, the following positive correlations were found total solids ? texture/body, headspace intensity ? aroma intensity, concentrations of caffeine/chlorogenic acids ? bitterness and astringency.     

Antioxidant activity,polyphenols, caffeine and melanoidins in soluble coffee: The influence of processing conditions and raw material

The production of soluble coffee starts with the selection of beans and is followed by roasting, grinding, extraction and drying. Lyophilised soluble coffees extracted by various methods from light, medium and dark-roasted arabica and robusta beans were evaluated for antioxidant activity (AA) using ABTS, Folin, DPPH and FRAP techniques. Caffeine, chlorogenic acid (5-CQA) and melanoidin content was also quantified. The data were analysed by principal component analysis. The AA values derived from the various methods used were correlated. Roasting resulted in the degradation of 5-CQA and formation of melanoidins, while AA was largely unaffected by roasting. The extraction of soluble coffee more prominently affected the AA of light-roasted coffee, mainly because it favoured the extraction of 5-CQA. The larger caffeine content in robusta coffee resulted in greater AA. All of soluble coffee products studied possessed antioxidant potential, which was conferred by their concentrations of phenolic compounds, caffeine and melanoidins.     

Identification of Chemical Clusters Discriminators of Arabica and Robusta Green Coffee

The chemical parameters pH, soluble solids, caffeine, trigonelline, total chlorogenic acids, total caffeoylquinic acids, 3-O-caffeoylquinic acid, 4-O-caffeoylquinic acid, 5-O-caffeoylquinic acid, total dicaffeoylquinic acids, 3,4-O-dicaffeoylquinic acid, 3,5-O-dicaffeoylquinic acid, 4,5-O-dicaffeoylquinic acid, total feruloylquinic acids, 3-O-feruloylquinic acid, and 5-O-feruloylquinic acid were measured in Arabica (C. arabica) and Robusta (C. canephora) green coffees in order to determine discrimination parameters. In general, Robusta green coffee showed higher values for pH, soluble solids, caffeine, total caffeoylquinic acids, total dicaffeoylquinic acid, and total feruloylquinic acid, but the content of soluble solids was not significantly different in both species of green coffee. Through application of a multivariate analysis, it was concluded that these chemicals form three clusters, being the group of caffeine, trigonelline, 3-O-caffeoylquinic acid, 4-O-caffeoylquinic acid, 3-O-feruloylquinic acid, 5-O-feruloylquinic acid, 3,4-O-dicaffeoylquinic acid, 3,5-O-dicaffeoylquinic acid, and 4,5-O-dicaffeoylquinic acid highly discriminating for Arabica and Robusta green coffees.     

Fast simultaneous analysis of caffeine, trigonelline, nicotinic acid and sucrose in coffee by liquid chromatography–mass spectrometry

A rapid liquid chromatography–mass spectrometry method for the simultaneous quantification of caffeine, trigonelline, nicotinic acid and sucrose in coffee was developed and validated. The method involved extraction with hot water, clarification with basic lead acetate and membrane filtration, followed by chromatographic separation using a Spherisorb^® S5 ODS2, 5 μm chromatographic column and gradient elution with 0.3% aqueous formic acid/methanol at a flow rate of 0.2 mL/min. The electrospray ionization source was operated in the negative mode to generate sucrose ions and in the positive mode to generate caffeine, trigonelline and nicotinic acid ions. Ionization suppression of all analytes was found due to matrix effect. Calibrations curves prepared in green and roasted coffee extracts were linear with r² > 0.999. Roasted coffee was spiked and recoveries ranged from 93.0% to 105.1% for caffeine, from 85.2% to 116.2% for trigonelline, from 89.6% to 113.5% for nicotinic acid and from 94.1% to 109.7% for sucrose. Good repeatibilities (RSD < 5%) were found for all analytes in the matrix. The limit of detection (LOD), calculated on the basis of signal-to-noise ratios of 3:1, was 11.9, 36.4, 18.5 and 5.0 ng/mL for caffeine, trigonelline, nicotinic acid and sucrose, respectively. Analysis of 11 coffee samples (regular or decaffeinated green, ground roasted and instant) gave results in agreement with the literature. The method showed to be suitable for different types of coffee available in the market thus appearing as a fast and reliable alternative method to be used for routine coffee analysis.     

Can near‐infrared reflectance of green coffee be used to detect introgression in Coffea arabica cultivars?

Most new coffee cultivars disseminated over the last 15 years are derived from the Timor Hybrid (Coffea arabica × C canephora). Introgression of genes from the C canephora genome has been estimated at between 9 and 29% of the genome. It has been shown that introgression can have a negative impact on the cup quality of cultivars derived from the Timor Hybrid. Consequently, coffee buyers or roasters may wish to assess whether the coffee they are purchasing comes from introgressed varieties. The possibility of distinguishing between non‐introgressed Arabicas and genotypes carrying chromosome fragments introgressed from C canephora was investigated (i) using some classical chemical compounds (caffeine, chlorogenic acids, trigonelline, fat and sucrose) and (ii) using a new approach based on spectra acquired by near‐infrared reflectance of green coffee. Near‐infrared spectra were obtained for 129 samples from two collections (Nicaragua and Costa Rica) of introgressed and non‐introgressed coffee trees. The spectral collections were treated by principal component and factorial discrimination. When the introgressed coffee trees were compared with the non‐introgressed trees using the chemical compounds, small but significant differences were found in caffeine, trigonelline and chlorogenic acid contents. However, the small variations in those compounds are not enough to detect introgression. The spectral collections treated by principal component and factorial discrimination made it possible to class from 92.30 to 94.87% of the analysed samples correctly, while the percentages of correctly classified samples in the verification file varied from 88.23 to 94.11%. The NIRS method appears to be an efficient method for determining whether a green coffee comes from an introgressed variety. Copyright © 2005 Society of Chemical Industry     

The influence of coffee bean maturity on the content of chlorogenic acids,caffeine and trigonelline

This paper reports changes, with coffee fruit maturity, in the coffee bean content of chlorogenic acids, caffeine and trigonelline. The major change was a sigmoidal increase in total caffeoylquinic acid essentially in parallel with the total dry matter gain, and representing between 5% and 12% thereof. The corresponding changes in the contents of several other chlorogenic acids, caffeine and trigonelline were slight on a mass per 100 beans basis.     

Recovery of Phenolic Antioxidants and Functional Compounds from Coffee Industry By-Products

The recovery process of the phenolic compounds from the coffee industry by-products and their antioxidant activity were investigated in this work. The coffee by-products (coffee pulp, husk, silver skin, and spent coffee) were obtained from coffee processing industry. The phenolic conserves were extracted using solvent mixture of isoproponal and water. The yield of the conserve was highest in case of silver skin (25%) followed by spent waste (19%) and cherry husk (17%) when pretreated with viscozyme. The conserve enclosed chlorogenic acid as major component when analyzed with high-performance liquid chromatography. The bioactive conserves prepared from coffee by-products possessed 65%–70% antioxidant activity. Apart from these, the coffee by-products encompassed total dietary fiber of 40%–80%. Whereas the soluble and insoluble fiber proportion of the coffee by-product ranged between 16–35% and 18–64%, respectively. The antioxidant activity of coffee by-product fiber ranged from 1.5 to 2.0 mmol trolox/100 g and is analogous to that of widespread fruits and fresh vegetables. The hydration properties such as water holding capacity of each by-product was strictly related to the amount of insoluble fiber and to the granulometry. This is the first report on the isolation of bioactive and functional compounds from coffee by-products and can be a source of new value-added products such as phenolic antioxidant adjunct for food processing.     

咖啡中功能性成分分离检测技术及安全性评价

咖啡以其独特的风味口感以及生理活性成为世界范围内最重要的食品类商品之一。咖啡的生理活性主要来自于咖啡中的咖啡因、绿原酸以及类黑精等功能性成分,这些成分具有醒脑提神、抗忧郁、抗氧化、抗菌以及预防癌症等方面的生物活性。因此,咖啡中功能性成分的分离提取、分析检测以及其安全性评价已经成为目前研究的热点。本文对咖啡中功能性成分咖啡因、绿原酸和类黑精的分离检测技术及其安全性评价研究进展进行综述,为咖啡中功能性成分的分离分析以及科学使用提供前沿的科学参考。     

Bioactive composition and antioxidant potential of different commonly consumed coffee brews affected by their preparation technique and milk addition

Coffee is one of the most popular beverages in the world, prepared and consumed in many different ways. Taste, aroma and composition of the coffee brew vary depending on the preparation method. Therefore, this study investigates the effect of different brewing methods on the polyphenol and methylxanthine composition and antioxidant capacity of thirteen different coffee brews. The content of total phenols and flavonoids was determined spectrophotometrically and the content of chlorogenic acid derivates (3-CQA, 4-CQA and 5-CQA) and caffeine using the high performance liquid chromatography (HPLC-PDA). Antioxidant capacity of coffee brews was evaluated by using the ABTS (2,2-azino-bis(3-ethylbenzthiazoline-6-sulfonic acid)) and FRAP (ferric-reducing antioxidant power) assays. Instant coffee brews showed the highest values in content of total phenols, chlorogenic acid derivates, caffeine and antioxidant capacity, which significantly decreased by milk addition. The antioxidant capacity of coffee brews was in compliance with the total phenol content and content of chlorogenic acid derivates.     

分相萃取法制备高纯度绿原酸的工艺研究

以杜仲叶为原料提取绿原酸,将大孔树脂和混合溶剂分相法相结合,对绿原酸进行精制纯化,使绿原酸的纯度达到99.5%(HPLC 法)。在萃取工艺中选定有机溶剂乙酸乙酯为萃取剂,考察萃取时间、pH 值、萃取次数对萃取率的影响,并通过响应面法建立萃取率和萃取时间、pH 值、萃取次数之间的关系,得到最佳萃取工艺 条件为萃取时间4.00min、pH2.97、萃取次数4 次,此时绿原酸萃取率达到95.1%。在分相工艺中,首先对分相剂进行筛选,选定非极性溶剂正己烷为分相剂,再对分相剂的用量进行研究,最终确定其用量为萃取液总体积的40%,绿原酸转移率达93% 以上。     

Chemical characterization and antioxidant properties of a new coffee blend with cocoa,coffee silverskin and green coffee minimally processed

The search for new technologies and ingredients with interesting characteristics and potential for incorporation into functional foods emerges in parallel with the demand for alternative sustainable and economically viable blends. Pursuing these aims, the formulation of a new coffee blend with 94% roasted coffee powder (Coffea canephora cv. Robusta and Coffea arabica, 70/30, w/w), 3% cocoa powder, 2% coffee silverskin and 1% golden coffee (green coffee minimally processed) was developed. The influence of the ingredients in the blend was compared with two other commercial coffee blends (in capsule and in a sealed package with a one-way degassing valve), being characterized the formulation, the physicochemical parameters, as its innovation. It is concluded that the developed coffee blend shows an enriched content of bioactive compounds (chlorogenic acids, trigonelline, theobromine and caffeine), displays an important antioxidant capacity and was favorably appreciated due to its sensory characteristics. Moreover, the addition of skin by-product becomes an additional valorization and the processing of green coffee and cocoa was minimized by adding innovation and an optimized extraction.     

烘焙度对冷萃咖啡理化指标与风味成分的影响

以亚洲咖啡豆为研究对象,分别选取浅、中、深3 种烘焙度的中国云南和印度尼西亚苏门答腊产的卡蒂姆种咖啡豆,比较分析冷萃与热萃方式对萃取浓度、萃取率、可滴定酸、总酚、总糖、咖啡因、葫芦巴碱、绿原酸、抗氧化活性与挥发性成分的差异,并进行主成分分析,从而探究烘焙度对冷萃咖啡理化指标与风味成分的影响规律。结果表明,随着烘焙度增加,冷萃咖啡的萃取浓度、萃取率均显著上升,可滴定酸、总酚、葫芦巴碱、绿原酸、抗氧化活性均显著下降（P＜0.05）。冷萃咖啡较热萃咖啡拥有更高的萃取浓度、萃取率与总糖含量（P＜0.05）,而可滴定酸、总酚含量、抗氧化活性较热萃显著偏低（P＜0.05）。经顶空固相微萃取-气相色谱-质谱检测分析发现,浅烘咖啡豆萃取液中的挥发性成分含量显著低于烘焙度高的咖啡萃取液,深烘咖啡豆萃取液中挥发性成分种类与总含量最多。进一步通过主成分分析能较好区分冷萃和热萃咖啡,两者挥发性成分贡献率具有较大差异。2-丁酮、2-丁烯醛等花香类物质对浅烘冷萃咖啡贡献率更高,而2-甲基吡嗪、糠醇等呈现烘焙坚果类香气物质对浅烘热萃咖啡贡献率更高;2,6-二乙基吡嗪、川芎嗪等烘焙坚果类香气物质对中烘冷萃和热萃咖啡具有较高的贡献率;2-乙烯基呋喃、甲基糠硫醇、2,5-二乙基吡嗪、糠基甲基硫醚等物质对深烘冷萃咖啡有较高贡献率,二甲基二硫、对甲酚、1-甲基吡咯等物质对深烘热萃咖啡贡献率更高。相对于热萃咖啡,烘焙度对冷萃咖啡抗氧化能力与挥发性成分的影响更大。