咖啡精油超临界CO2萃取工艺优化及理化特性分析

以云南保山小粒咖啡豆为对象,根据国家标准,测定生、熟咖啡豆的营养成分,在单因素实验的基础上,以响应面优化超临界CO₂萃取咖啡精油的工艺参数;测定生、熟咖啡精油理化指标,并通过气相色谱-氢火焰离子化检测器（GC-FID）分析生、熟咖啡精油的脂肪酸组成。结果表明:经烘焙处理后,熟咖啡豆中水分、水浸出物、咖啡因、总糖、粗纤维和粗脂肪含量与生咖啡豆中的存在显著差异（P<0.05）;超临界CO₂萃取生咖啡精油的最佳工艺条件为萃取压力25 MPa,萃取温度54 ℃,萃取时间150 min,在此条件下咖啡精油萃取得率为13.98%。烘焙处理前后,咖啡精油各常规理化指标无显著差异,且均符合国家标准要求。通过GC-FID分别检测到15和16种脂肪酸,其中亚油酸、棕榈酸、硬脂酸和油酸等为主要脂肪酸,烘焙对咖啡豆脂肪酸组成影响不明显,但各脂肪酸的含量存在一定差异。烘焙对咖啡豆及咖啡精油的各项指标均有一定程度的影响,为云南地区咖啡产业发展提供科学依据。     

A comparative study of chemical attributes and levels of amines in defective green and roasted coffee beans

Differences in chemical attributes (proximate composition, water activity, sucrose, acidity and pH levels) and amine levels between defective and healthy coffee beans were studied. Before roasting, significant differences (p < 0.05) were observed for the ash contents of the coffee samples, with the highest values found for black beans. Moisture content was higher for non-defective beans in comparison to defective beans. Non-defective coffee beans had higher lipids contents than both sour and black beans. There were no significant differences (p > 0.05) for protein levels between defective and non-defective beans. After roasting, protein levels remained constant, there was a small decrease in ash contents and a slight increase in oil contents of black and sour beans. Both black and sour beans had higher acidity levels than immature and non-defective beans. Acidity levels decreased after roasting. Water activity levels also decreased with roasting, with slightly higher levels for defective beans in comparison to non-defective ones. Sucrose levels were much higher in non-defective beans, and the lowest values were in black beans, prior to roasting. After roasting, only traces of sucrose were found. Total amine levels were much lower for black beans, in comparison to the other coffee samples. Putrescine was the prevailing amine in all samples. Histamine was only detected in the defective coffee samples. Small amounts of serotonin, cadaverine and tryptamine were found in some of the samples. After roasting to a light degree, only traces of serotonin were detected and no amines were detected after roasting to medium and dark degrees.     

Discrimination between defective and non-defective Brazilian coffee beans by their volatile profile

The coffee roasted in Brazil is considered to be of low quality, due to the presence of defective coffee beans that depreciate the beverage quality. In view of the fact that coffee flavour is directly related to the volatile compounds produced during roasting, the objective of the present study was to perform a comparative evaluation of the volatile fraction of defective (black, immature, sour) and healthy coffee beans, in order to find possible chemical markers for detection of defective coffee beans in roasted coffee. Volatiles extraction and concentration was performed by solid phase micro-extraction (SPME) of the roasted coffee headspace, using a triple phase (divinylbenzene/carboxen/polydimethylsiloxane) fiber. Analysis of the volatile profiles was performed by GC–MS. The results obtained showed that the proposed methodology was adequate for extraction, concentration and analysis of the coffees volatile profile. Several substances were identified as possible markers for differentiating black, sour and immature beans from healthy coffee beans. Statistical analysis of the data by principal components (PCA) demonstrated that the volatile profile enables the differentiation of healthy and defective coffees. The data were separated into two major groups, one represented by immature and black beans and the other by healthy and sour coffee beans. Such results indicated that black and sour beans can be associated to fermentation of immature and of healthy beans, respectively.     

Volatile compounds as potential defective coffee beans’ markers

Although Brazil is the largest raw coffee producer and exporter in the world, a large amount of its Arabica coffee production is considered inappropriate for exportation. This by-product of coffee industry is called PVA due to the presence of black (P), green (V) and sour (A) defective beans, which are known to contribute considerably for cup quality decrease. Data on the volatile composition of Brazilian defective coffee beans are scarce. In this study, we evaluated the volatile composition of defective coffee beans (two lots) compared to good quality beans from the respective lots. Potential defective beans’ markers were identified. In the raw samples, 2-methylpyrazine and 2-furylmethanol acetate were identified only in black-immature beans and butyrolactone only in sour beans, while benzaldehyde and 2,3,5,6-tetramethylpyrazine showed to be potential markers of defective beans in general. In the roasted PVA beans, pyrazine, 2,3-butanediol meso, 2-methyl-5-(1-propenyl)pyrazine, hexanoic acid, 4-ethyl-guayacol and isopropyl p-cresol sulfide also showed to be potential defective coffee beans’ markers.     

咖啡豆烘焙过程中油脂脂肪酸组成、挥发性风味及活性成分的演变规律

以云南小粒种咖啡豆为试材,系统研究烘焙过程中咖啡油脂理化性质、脂肪酸组成、挥发性成分及活性成分的变化规律。结果表明：随着烘焙度加深,油脂色泽加深;酸价呈增加的趋势,由1.60 mg/g增至3.75 mg/g;碘值反之,由142.04 g/100 g降至83.12 mg/100 g;茴香胺值先增大后减少,其值在3.40～16.26之间;皂化值略有降低,但无显著差异;共鉴定出11 种脂肪酸,主要为亚油酸相对含量在43.06%～64.39%之间,其次为硬脂酸和棕榈酸相对含量在12.67%～27.55%之间,油酸相对含量为9.03%～17.20%;脂肪酸组成影响不明显,但各脂肪酸的含量存在一定差异;利用气相色谱-质谱从极浅度到法式重度的咖啡油脂样品中分别检出25、33、36、53、54、59、64 种和58 种挥发性成分,主要成分有呋喃类化合物、吡嗪类化合物、酮类化合物、吡咯类化合物等,其种类和含量均呈减小趋势;活性成分中咖啡豆醇、α-生育酚、γ-生育酚、δ-生育酚含量均减少;而总酚含量不断增加,由7.75 mg/100 g升至15.96 mg/100 g。本研究结果可为咖啡精深加工及资源高值化利用提供理论依据和技术支撑。     

基于机器视觉的咖啡生豆快速检测与分级研究

目的 为了实现咖啡生豆的快速无损等级评估,建立一种基于机器视觉的咖啡生豆快速检测分级方法。方法 本次研究提取咖啡生豆图像预处理后的形状和颜色共13种特征,首先通过特征分布图分析与主成分分析找到13类缺陷豆的显著特征,并确定其显著特征值范围来判定缺陷豆,然后对正常豆按粒度大小判断其等级,最后在MATLAB App Designer平台上设计了咖啡生豆快速检测与分级界面。结果 研究表明,利用机器视觉技术能很好地识别各个类别咖啡生豆,检测一级咖啡生豆准确率为94.77%、二级为93.2%、三级为95.85%,13类缺陷豆平均准确率为82.25%,咖啡生豆检测平均准确率达到91.52%,检测300g咖啡生豆总用时25.3156s。结论 提高了咖啡生豆分级的智能化水平,分级过程平稳且快速,为今后咖啡生豆在线检测分选提供了技术支持。     

Physicochemical characteristics of green coffee: comparison of graded and defective beans

ABSTRACT:  Defective (triage) coffee beans are beans rejected after separating the graded ones according to the size and color. These coffee beans represent about 15% to 20% of coffee production in India but are not utilized for beverages since these affect the quality of coffee brew. In the present study, physical characteristics such as bean density, brightness, titratable acidity, pH, moisture, and total soluble solids and also chemical composition, namely, caffeine, chlorogenic acids, lipids, sucrose, total polyphenols, and proteins, were evaluated in defective as well as in graded green coffee beans. The physical parameters such as weight, density, and brightness of defective coffee beans were low compared to the graded beans, which is due to the presence of immature, broken, bleached, and black beans. Caffeine content was low in triage beans compared to graded beans. Chlorogenic acids, one of the composition in coffee responsible for antioxidant activity, was found to be intact (marginally high in some cases) in defective coffee beans. Hence, triage coffee beans can be evaluated as a source of antioxidant or radical scavenging conserve for food systems.     

云南不同地区烘焙咖啡豆主要成分分析及类黑精组成成分

以云南3个咖啡主产区(普洱、怒江、德宏)的生咖啡豆为原料,通过不同程度(轻度、中度、重度)烘焙,对其主要成分进行分析,并提取类黑精,采用热裂解-气相色谱-质谱(pyrolysis-gas chromatography-mass spectrometry,Py-GC-MS)联用技术分析咖啡类黑精的化学组成。结果显示:随着烘焙程度加深,咖啡豆的蛋白质和粗脂肪含量增加,总氨基酸含量降低,其中蛋白质含量最高为重度烘焙后的普洱咖啡豆(16.3 g/100 g),氨基酸含量最高为普洱生咖啡豆(9.41%),粗脂肪含量最高为中度烘焙后的德宏咖啡豆(13.85 g/100 g),矿物质元素中含量较高的为K、Mg、P、Ca,普洱咖啡豆经重度烘焙后K含量最高(2.2 g/100 g)。Py-GC-MS分析结果表明:不同产地、不同烘焙程度咖啡豆的类黑精组成差异明显,但也存在共性特征,咖啡因和酸类相对含量最高,其次是胺类、酯类、酚类、吡咯类、呋喃类、吡啶类、醛类、醇类、酮类等。     

Extraction of coffee diterpenes and coffee oil using supercritical carbon dioxide

Commercial green and roasted coffee beans were used to maximize oil extraction and conditions were studied to obtain the highest and lowest diterpene levels on green and roasted coffee oil, respectively. Thus, operational temperatures (60–90 °C) and pressure (235–380 bar) were optimized for coffee oil extraction. Oil content levels and diterpene oil concentration were compared to the results obtained with the extraction with Soxhlet apparatus, using hexane as solvent. In general, an inverse correlation was observed between the amount of extracted oil and diterpene concentration levels. As a result, different oil contents with different diterpene concentrations could be obtained. The HPLC analysis of cafestol and kahweol in the oil extracted from green coffee beans at 70 °C/253 bar resulted in the highest concentration (453.3 mg 100 g⁻¹), which was 48% lower than in the oil extracted with hexane while in the oil extracted from roasted coffee beans at 70 °C/371 bar, resulted in 71.2% reduction of diterpenes.     

云南不同地区生咖啡豆的风味前体物质研究

本文通过测定云南德宏、保山、临沧和普洱四个地区生咖啡豆中风味前体物质组成和含量,结合一元方差分析(ANOVA)和主成分分析(PCA)进行统计学分析,探索了不同地区生咖啡豆中风味前体物质的差异性。实验结果表明:氨基酸总量最高为德宏咖啡(10.31%),最低为保山咖啡(9.07%);蛋白质测定结果与氨基酸相类似;而德宏和临沧咖啡中脂肪和脂肪酸含量均小于普洱和保山咖啡;单糖总量最高为普洱咖啡(17.21%),最低为保山咖啡(15.95%)。PCA分析和方差分析表明,普洱咖啡中脂肪酸和其他地区均呈显著性差异(P0.05);保山咖啡中氨基酸同其他地区均呈显著性差异;而临沧咖啡中单糖、蛋白质、脂肪和保山咖啡均呈显著性差异;除少数样品外,大部分样品在PCA的二维得分投影图上按特性各自聚为一类。本研究可为云南咖啡的烘焙加工提供理论参考。     

Assessment of green coffee bean metabolites dependent on coffee quality using a 1H NMR-based metabolomics approach

There is increasing interest in the coffee grade or quality with the rise of coffee consumption, but a classical, chemical analysis-based understanding of the coffee bean grade is still limited. We therefore report the identification of green coffee bean metabolites related to coffee bean quality using a ¹H NMR-based metabolomic analysis of well-established specialty-grade green coffee beans, in particular, of a single species (Coffea arabica). The higher levels of sucrose and the lower levels of γ-aminobutyric acid (GABA), quinic acid, choline, acetic acid and fatty acids observed in specialty or high-grade green coffee beans, compared to commercial-grade beans, were suggestive to be multiple markers for characterizing specialty green coffee bean. In particular, variations in sucrose and GABA levels between specialty and commercial coffees could be a consequence of different environmental conditions, for example, biotic or abiotc stresses, at growing regions. These results highlight an alternative method of metabolomic approach for grading green coffee bean.     

Evaluation of the potential of FTIR and chemometrics for separation between defective and non-defective coffees

The objective of this work was to evaluate the potential of Fourier transform infrared spectroscopy (FTIR) for the discrimination of defective and non-defective coffee beans. Defective (black, immature and sour) and non-defective Arabica coffee beans were submitted to FTIR analysis by transmittance readings employing KBr discs and reflectance readings employing attenuated total reflectance (ATR) and diffuse reflectance (DR) accessories. Multivariate statistical analysis (PCA, clusters) was performed in order to verify the possibility of discrimination between defective and non-defective coffee samples. A clear separation between defective and non-defective coffee beans was observed, based on both PCA and cluster analysis of the reflectance spectra (ATR and DR accessories) and of the first derivatives of the transmittance spectra (KBr discs). Such results indicate that FTIR analysis has the potential for the development of a fast and reliable analytical methodology for the discrimination between defective and non-defective coffee beans.     

茶叶籽油研究进展

茶叶籽油从山茶科山茶属植物茶树的成熟种子中提取,富含不饱和脂肪酸和多种生理活性成分,可制成高级食用油、美容护肤品用油和医疗专用油,具有广阔的开发利用前景。本文综述了近年来茶叶籽油提取制备工艺、脂肪酸组成和含量分析、生理活性成分检测的研究进展,并针对生产实践中茶树结实率低、茶叶籽含油率中等两大问题,论述了改良茶园栽培管理技术增强茶叶籽丰产性、分子育种法提高茶叶籽含油率的可行性,旨在为制备优质的茶叶籽油提供参考。     

Chemical characterisation of non-defective and defective green arabica and robusta coffees by electrospray ionization-mass spectrometry (ESI-MS)

The coffee roasted in Brazil is considered to be of low quality, due to the presence of defective coffee beans that depreciate the beverage quality. These beans, although being separated from the non-defective ones prior to roasting, are still commercialized in the coffee trading market. Thus, it was the aim of this work to verify the feasibility of employing ESI-MS to identify chemical characteristics that will allow the discrimination of Arabica and Robusta species and also of defective and non-defective coffees. Aqueous extracts of green (raw) defective and non-defective coffee beans were analyzed by direct infusion electrospray ionization mass spectrometry (ESI-MS) and this technique provided characteristic fingerprinting mass spectra that not only allowed for discrimination of species but also between defective and non-defective coffee beans. ESI-MS profiles in the positive mode (ESI(+)-MS) provided separation between defective and non-defective coffees within a given species, whereas ESI-MS profiles in the negative mode (ESI(−)-MS) provided separation between Arabica and Robusta coffees.     

Discrimination between immature and mature green coffees by attenuated total reflectance and diffuse reflectance Fourier transform infrared spectroscopy

The objective of this work was to evaluate the potential of Fourier transform infrared spectroscopy (FTIR) in the characterization and discrimination between immature and mature or ripe coffee beans. Arabica coffee beans were submitted to FTIR analysis by reflectance readings employing attenuated total reflectance (ATR) and diffuse reflectance (DR) accessories. The obtained spectra were similar, but in general higher absorbance values were observed for nondefective beans in comparison to immature ones. Multivariate statistical analysis (principal component analysis, PCA, and agglomerative hierarchical clustering, AHC) was performed in order to verify the possibility of discrimination between immature and mature coffee samples. A clear separation between immature and mature coffees was observed based on AHC and PCA analyses of the normalized spectra obtained by employing both ATR and DR accessories. Linear discriminant analysis was employed for developing classification models, with recognition and prediction abilities of 100%. Such results showed that FTIR analysis presents potential for the development of a simple routine methodology for separation of immature and mature coffee beans. Practical Application: The ultimate goal of this research is to be able to propose improvements in the way immature coffee beans are separated from graded mature beans in coffee facilities (cooperatives and other coffee producer's associations). The results obtained herein point toward FTIR as a potential tool for the aimed improvements.     

Relationship between acid value of extracted fatty matter and age of green coffee beans

The work described in this paper was aimed at attempts to determine the changes in the acidity of the fatty matter of green coffee beans during storage under tropical conditions, and to relate them to the age of coffee beans, and to the panel assessment of colour and cup-test of the roasted coffee. On the basis of systematic studies a relationship between acid value and coffee age has been found. The coffee beans stored under tropical conditions for up to 4 years showed relatively large increases in acid value, which correlated with average responses of the tasters. In comparison, samples stored under European conditions showed lesser increases in acid value over 5 years, and little change in taste assessment. The determination of acid value is considered to be a useful objective quality control test.     

Evaluation of green coffee beans quality using near infrared spectroscopy: A quantitative approach

Characterisation of coffee quality based on bean quality assessment is associated with the relative amount of defective beans among non-defective beans. It is therefore important to develop a methodology capable of identifying the presence of defective beans that enables a fast assessment of coffee grade and that can become an analytical tool to standardise coffee quality. In this work, a methodology for quality assessment of green coffee based on near infrared spectroscopy (NIRS) is proposed. NIRS is a green chemistry, low cost, fast response technique without the need of sample processing. The applicability of NIRS was evaluated for Arabica and Robusta varieties from different geographical locations. Partial least squares regression was used to relate the NIR spectrum to the mass fraction of defective and non-defective beans. Relative errors around 5% show that NIRS can be a valuable analytical tool to be used by coffee roasters, enabling a simple and quantitative evaluation of green coffee quality in a fast way.     

An investigation into green coffee press cake as a renewable source of bioactive compounds

The residual biomass of coffee, obtained after the oil extraction from coffee beans, called coffee beans residual press cake, has been attracted interest as a source of compounds with antioxidant capacity. This study investigated the effects of ethanolic and methanol-acetone extracts of green coffee beans (GCB) and its residual press cake (GCC) on the phenolic composition and antioxidant capacity. Antioxidant capacity was assayed through five different methods (total phenolic compounds, •DPPH, ABTS, FRAP and β-carotene bleaching assay), and the phenolic profile of the samples through High Performance Liquid Cromatography. GCB and GCC enclosed chlorogenic (55.16 and 64.96 mg g⁻¹, respectively) and caffeic (25.07 and 44.37 mg g⁻¹, respectively) acids as the major components, and the cake presented higher antioxidant capacity than the actual green bean. Antioxidant capacity was higher for GCC extracted with methanol and acetone. This study on the evaluation of the effects of the type of solvent on the bioactive compounds from GCB and GCC showed that this by-product can be a source of new value-added products, such as phenolic antioxidant adjuncts for food or pharmaceutic processing.     

Influence of the postharvest processing method on polysaccharides and coffee beverages

Fresh coffee fruits were subjected to different types of postharvest processing. Intact fruits were processed using the dry method (DI), peeled fruits were processed using the semi‐dry method (DP) and fruits were processed using the wet method (W). The extraction of polysaccharides from the seeds from the unprocessed and processed fruits indicated that arabinogalactans and (galacto)mannans were the main polysaccharides. Higher amounts of polysaccharides were extracted from processed coffee. Among the treatments, lower amounts of water‐soluble galactomannans were obtained from coffee beans processed by the dry and wet methods. The polysaccharides obtained from beverages prepared using beans from DI, DP and W methods showed different yields, total sugar and protein contents. Galactomannans and AGPs were also present in the coffee beverages. Although differences were found in the chemical compositions, no differences were observed in the viscosity or surface tension of coffee beverages from the DI, DP and W methods.     

Deep fat frying of frozen foods in sunflower oil. Fatty acid composition in fryer oil and frozen prefried potatoes

The fatty acid pattern was used to evaluate the alteration of a sunflower oil that had been used 20 times to fry various frozen foods with frequent replenishment (FR) or without replenishment (NR) of the used oil with fresh oil during frying. Furthermore, the fat extracted from potatoes fried in the sunflower oil from fryings 1, 5, 8, 12, 16 and 20 was also analysed by gas–liquid chromatography to compare its fatty acid profile with that of the corresponding fryer oil. The amount of unaltered fatty acids decreased from 96.2 mg per 100 mg oil in the unused sunflower oil to 89.6 mg per 100 mg oil after 20 fryings in the FR oil and to 88.9 mg per 100 mg oil in the NR oil, following a linear adjustment (r > 0.97; p < 0.001). Linoleic acid also decreased while palmitic and oleic acids increased in the bath oil. Fatty acid variations were more pronounced in NR than FR oil for major fatty acids and not only related to the degradation of unsaturated fatty acids but also to the interactions between the bath oil and the fried food fat. Thus the increase in palmitic acid of the fryer oil could be due to migration of this fatty acid from the prefried frozen potatoes as revealed by the composition of the fat extracted from those potatoes. Although the fatty acid variation (eg myristic, palmitic, oleic, trans–cis isomers of linoleic and linoleic acids) was not equivalent in FR or NR fryer oil and in the fat of the potatoes, the changes in total unaltered fatty acids were not significantly different in oil and potatoes. Present data suggest that frequent addition of fresh oil throughout the frying process minimises the fatty acid changes, contributing to the obtainment of fried foods with a healthy fatty acid profile. © 2000 Society of Chemical Industry