Specific screening for color precursors and colorants in beet and cane sugar liquors in relation to model colorants using spectrofluorometry evaluated by HPLC and multiway data analysis

A comparison was made of the fluorophores in beet thick juice and cane final evaporator syrup, which are comparable in the production of cane and beet sugar; that is, both represent the final stage of syrup concentration prior to crystallization of sugar. To further elucidate the nature of the color components in cane and beet syrup, a series of model colorants was also prepared, consisting of mildly alkaline-degraded fructose and glucose and two Maillard type colorants, glucose--glycine and glucose--lysine. Fluorescence excitation--emission landscapes resolved into individual fluorescent components with PARAFAC modeling were used as a screening method for colorants, and the method was validated with size exclusion chromatography using a diode array UV--vis detector. Fluorophores from the model colorants were mainly located at visible wavelengths. An overall similarity in chromatograms and absorption spectra of the four model colorant samples indicated that the formation of darker color was the distinguishing characteristic, rather than different reaction products. The fluorophores obtained from the beet and cane syrups consisted of color precursor amino acids in the UV wavelength region. Tryptophan was found in both beet and cane syrups. Tyrosine as a fluorophore was resolved in only beet syrup, reflecting the higher levels of amino acids in beet processing. In the visible wavelength region, cane syrup colorant fluorophores were situated at higher wavelengths than those of beet syrup, indicating formation of darker colorants. A higher level of invert sugar in cane processing compared to beet processing was suggested as a possible explanation for the darker colorants.     

不同酶和酵母对干红葡萄酒香气影响的差异分析

为提高甘肃河西产区蛇龙珠干红葡萄酒的香气品质,优化酿酒工艺,该文采用顶空固相微萃取和气相色谱-质谱联用技术,分析比较了添加不同浸渍酶和酵母发酵的蛇龙珠干红葡萄酒的香气构成。结果显示:蛇龙珠干红葡萄酒中初步定性香气化合物75种,主要为酯、醇、酸、萜烯和酚类物质。比较酯类、萜烯类等香气成分质量浓度和香气物质释放总量,EX-V酒样明显高于EX和HC酒样,D254酒样明显高于BDX酒样。各组酒样主要香气成分构成相似,但微量香气成分差异显著。果香是香气强度最高的香气系列,植物香、脂肪香、花香次之,其香气强度EX-V酒样高于EX和HC酒样,D254酒样高于BDX酒样。浸渍酶和酵母对甘肃河西产区蛇龙珠干红葡萄酒香气品质的影响评价显示,浸渍酶EX-V优于EX和HC,酵母D254优于BDX。研究结果可为甘肃河西产区蛇龙珠干红葡萄酒香气品质的提高及酿造工艺研究提供科学数据参考。     

红曲中非酿酒酵母的分离鉴定及其对黄酒风味成分的影响

为探究红曲中非酿酒酵母对黄酒风味成分的影响,首先对红曲中的酵母菌株进行分离纯化,并采用分子生物学方法进行鉴定,然后将分离的非酿酒酵母菌株分别与红曲霉相结合,以纯种发酵的方式酿造红曲黄酒,分析各酒样中有机酸、氨基酸、挥发性物质等风味成分的组成及含量。结果表明,分离获得的4株非酿酒酵母CKS-2为威克汉姆酵母(Wickerhamomyces sp.)、CKS-3为季也蒙毕赤酵母(Meyerozyma guilliermondii)、CKS-4为胶红酵母(Rhodotorula mucilaginosa)、CKS-7为德尔布有孢酵母(Torulaspora delbrueckii),其中,CKS-7具有较好的产乙醇和苹果酸能力,发酵酒样中丝氨酸、组氨酸、色氨酸和亮氨酸的含量也较高,并且具有良好的合成2-苯乙醇、异戊醇、棕榈酸乙酯等挥发性风味成分的能力。本研究对红曲黄酒品质提升,以及筛选潜在可应用于红曲黄酒酿造的优良非酿酒酵母菌株具有一定作用。     

优选非酿酒酵母胞外酶增香酿造干白葡萄酒效果

为了研究非酿酒酵母胞外酶促进葡萄酒发酵产香的效果,该文在爱格丽葡萄汁酒精发酵12 h后,分别添加优选胶红酵母(Rhodotorula mucilaginosa,RM)胞外酶液,优选发酵毕赤酵母(Pichia fermentans,PF)胞外酶液和商业糖苷酶制剂(almondβ-glucosidase,AG)(10 mU/mL),以不添加酶制剂的酿酒酵母纯发酵为对照,发酵过程中每24 h取样,采用HS-SPME-GC/MS(headspace solid-phase microextraction-gas chromatography/mass spectrometry)监测挥发性成分的生成变化。葡萄酒含糖量低于2 g/L时终止发酵,低温满罐密封储存,次年4月,进行葡萄酒香气仪器和感官量化分析。胞外酶液共测得6种风味酶活性,其中RM酶液中的β-D-葡萄糖苷酶、α-L-鼠李糖苷酶、β-D-木糖苷酶活性均显著(P<0.05)高于PF中的,而α-L-阿拉伯糖苷酶和酯酶在PF酶液中活性更高(P<0.05)。发酵过程中,胞外酶处理显著促进了(P<0.05)品种香气和发酵香气物质的生成,其中RM酶液显著提高了萜烯类物质和苯乙基类化合物含量,其作用效果分别比商业酶处理高41.7%和31.8%,PF酶液显著促进了发酵香气化合物的生成,尤其是脂肪酸乙酯含量约为对照的2倍。酒样感官分析结果显示,两株酵母的胞外酶处理表现出各自增香酿造的优势,其中RM酶液促进温带酸果类香气的效果突出,PF酶液显著提升了柑橘类香气。研究结果为酵母风味酶应用于葡萄酒的增香酿造提供了理论和实践指导。     

Characterization of the most odor-active volatiles of orange wine made from a Turkish cv. Kozan (Citrus sinensis L. Osbeck)

The aroma-active compounds of cv. Turkish Kozan orange wine were analyzed by sensory and instrumental analyses. Liquid-liquid extraction with dichloromethane was used for extraction of volatile components. According to sensory analysis, the aromatic extract obtained by liquid-liquid extraction was representative of orange wine odor. A total of 63 compounds were identified and quantified in orange wine. The results of the gas chromatography-olfactometry analysis showed that 35 odorous compounds were detected by the panelists. Of these, 28 aroma-active compounds were identified. Alcohols followed by terpenes and esters were the most abundant aroma-active compounds of the orange wine. Among these compounds, ethyl butanoate (fruity sweet), 3-methyl-1-pentanol (roasty), linalool (floral citrusy), gamma-butyrolactone (cheesy burnt sugar), 3-(methylthio)-propanol (boiled potato, rubber), geraniol (floral citrusy), and 2-phenylethanol (floral rose) were the most important contributors to the aroma of the orange wine because they were perceived by all eight panelists.     

Liquid chromatography coupled to isotope ratio mass spectrometry: a new perspective on honey adulteration detection

A new procedure to determine individual sugar (sucrose, glucose, and fructose) 13C isotope ratios, using liquid chromatography-isotope ratio mass spectrometry (HPLC-IRMS), has been developed to improve isotopic methods devoted to the study of honey authenticity. For this purpose 79 commercial honey samples from various origins were analyzed. Values of delta13Choney ranged from -14.2 to -27.2", and delta13Cprotein ranged from -23.6 to -26.9". A very strong correlation is observed between the individual sugar 13C ratios, which are altered in the event of sugar addition, even at low levels. The use of Deltadelta13C [fruct-glu], Deltadelta13C [fruct-suc], and Deltadelta13C [gluc-suc] systematic differences as an authenticity criterion permits the sugar addition [C3, beet sugar; or C4, cane sugar, cane syrup, isoglucose syrup, and high-fructose corn syrup (HFCS)] to be reliably detected (DL = 1-10%). The new procedure has advantages over existing methods in terms of analysis time and sensitivity. In addition, it is the first isotopic method developed that allows beet sugar addition detection.     

Assessment of antioxidant activity of cane brown sugars by ABTS and DPPH radical scavenging assays: determination of their polyphenolic and volatile constituents

Seven cane brown sugars (four from La Réunion, two from Mauritius, and one from France) were investigated for their polyphenol content and volatile composition in relation to their free radical scavenging capacity determined by ABTS and DPPH assays. The thin layer coated on the sugar crystal was extracted by Soxhlet extractor with dichloromethane. The volatile compounds of brown sugars were studied by GC-MS, and 43 compounds were identified. The total phenolic content of brown sugars was determined according to the Folin-Ciocalteu method. Phenolic compounds were quantified in the brown sugar extracts by LC-UV-ESI-MS. Brown sugar aqueous solutions exhibited weak free radical scavenging activity in the DPPH assay and higher antioxidant activity in the ABTS assay at relatively high concentration. The brown sugar extracts showed interesting free radical scavenging properties despite the low concentration of phenolic and volatile compounds. Sugar is a common foodstuff traditionally used for its sweetening properties, which might be accompanied by antioxidant properties arising from molecules (polyphenols, Maillard products) other than sucrose of the cane brown sugars.     

Isolation and characterization of novel benzoates, cinnamates, flavonoids, and lignans from Riesling wine and screening for antioxidant activity.

A German Riesling wine has been fractionated with the aid of countercurrent chromatography. After purification by HPLC, the structures of 101 compounds were established by mass spectrometry and NMR spectroscopy. Seventy-three of the isolated compounds exhibited a phenolic or benzylic structure. Fifty-four compounds were reported for the first time as Riesling wine constituents. New compounds identified in this work included twelve benzoic and cinnamic acid derivatives. In addition to two isomeric (E)-caffeoyl ethyl tartrates, the glucose esters of (E)-cinnamic, (E)-p-coumaric, and (E)-ferulic acid, as well as the 4-O-glucosides of (E)- and (Z)-ferulic acid, have been identified for the first time in Riesling wine. The structures of two additional phenylpropanoids were elucidated as 3-hydroxy-1-(4-hydroxy-3-methoxyphenyl)-propan-1-one and 2,3-dihydroxy-1-(4-hydroxy-3-methoxyphenyl)-propan-1-one. Moreover, two ethyl esters, i.e., ethyl protocatechuate and ethyl gallate, as well as the glucose ester of vanillic acid, were newly detected in Riesling wine. Novel representatives in the flavonoid group were dihydrokaempferol, dihydroquercetin, and four dihydroflavonol glycoconjugates, i.e., the 3-O-glucosides of dihydrokaempferol and dihydroquercetin, as well as the 3-O-xyloside and the 3'-O-glucoside of dihydroquercetin. Additionally, six novel lignans, i.e., lariciresinol 4-O-glucoside, three isolariciresinol derivatives, and two secoisolariciresinols, as well as three neolignans were isolated. Structural elucidation of the newly isolated wine constituents is reported together with the determination of their antioxidant activity.     

Optimization of multiple headspace solid-phase microextraction for the quantification of volatile compounds in dry fermented sausages

Multiple headspace solid-phase microextraction (HS-SPME) is a stepwise method that eliminates the influence of the matrix sample on the quantitative analysis of solid samples. The process was optimized for the analysis of volatile compounds in dry fermented sausages by gas chromatography and mass spectrometry. Different amounts of fermented sausages and different vial volumes were studied to obtain the theoretical exponential decay of the peak area of the four successive extractions in order to calculate the total area in the sausage. The highest number of volatile compounds analyzed by multiple HS-SPME in dry fermented sausages was obtained in a 10 mL headspace vial with 0.07 g of sample in the presence of water, 0.75 mg butylated hydroxytoluene, and 0.5 g sodium chloride. Finally, the method was characterized in terms of linearity and detection limits and applied to analyze the volatile compounds present in fermented sausages manufactured with either nitrate or nitrite.     

Headspace solid phase microextraction (SPME) analysis of flavor compounds in wines. Effect of the matrix volatile composition in the relative response factors in a wine model.

The application of headspace solid phase microextraction (SPME) for flavor analysis has been studied. Headspace SPME sampling was tested for nine common wine flavor compounds in 10% (v/v) aqueous ethanol: linalool, nerol, geraniol, 3-methyl-1-butanol, hexanol, 2-phenylethanol, ethyl hexanoate, ethyl octanoate, and ethyl decanoate. The chemical groups (monoterpenoids, aliphatic and aromatic alcohols, and esters) showed specific behavior in SPME analysis. SPME sampling parameters were optimized for these components. Relative response factors (RRFs), which establish the relationship between the concentration of the compound in the matrix liquid solution and the GC peak area, were estimated for all compounds. Log(10)(RRF) varied from 0 (3-methyl-1-butanol) to 3 (ethyl decanoate), according to their molecular weight. Quantification by SPME was shown to be highly dependent on the matrix composition; the compounds with higher RRF were the less affected. As a consequence, the data obtained with this methodology should be used taking into consideration these limitations, as shown in the analysis of four monovarietal Bairrada white wines (Arinto, Bical, Cerceal, and Maria Gomes).     

Chemical characterization of dissolvable tobacco products promoted to reduce harm

In 2009, the R. J. Reynolds Tobacco Co. released a line of dissolvable tobacco products that are marketed as an alternative to smoking in places where smoking is prohibited. These products are currently available in Indianapolis, IN, Columbus, OH, and Portland, OR. This paper describes the chemical characterization of four such products by gas chromatography-mass spectrometry (GC-MS). The dissolvable tobacco products were extracted and prepared by ultrasonic extraction using acetone, trimethylsilyl derivatization, and headspace solid phase microextraction (SPME). The following compounds were identified in the dissolvables using either ultrasonic extractions or trimethylsilyl derivatization: nicotine, ethyl citrate, palmitic acid, stearic acid, sorbitol, glycerol, and xylitol. The following compounds were identified in the dissolvables using headspace SPME: nicotine, ethyl citrate, cinnamaldehyde, coumarin, vanillin, and carvone. With the exception of nicotine, the compounds identified thus far in the dissolvables are either flavoring compounds or binders. The concentration of free nicotine in the dissolvables was determined from the Henderson-Hasselbalch equation and by measuring the pH and nicotine concentration by GC-MS. The results presented here are the first to reveal the complexity of dissolvable tobacco products and may be used to assess potential oral health effects.     

Similarities in the aroma chemistry of Gewürztraminer variety wines and lychee (Litchi chinesis sonn.) fruit

GC/O analysis of canned lychees indicated that cis-rose oxide, linalool, ethyl isohexanoate, geraniol, furaneol, vanillin, (E)-2-nonenal, beta-damascenone, isovaleric acid, and (E)-furan linalool oxide were the most odor potent compounds detected in the fruit extracts. However, on the basis of calculated odor activity values (OAVs), cis-rose oxide, beta-damascenone, linalool, furaneol, ethyl isobutyrate, (E)-2-nonenal, ethyl isohexanoate, geraniol, and delta-decalactone were determined to be the main contributors of canned lychee aroma. When these results were compared with GC/O results of fresh lychees and Gewürztraminer wine, 12 common odor-active volatile compounds were found in all three products. These included cis-rose oxide, ethyl hexanoate/ethyl isohexanoate, beta-damascenone, linalool, ethyl isobutyrate, geraniol, ethyl 2-methylbutyrate, 2-phenylethanol, furaneol, vanillin, citronellol, and phenethyl acetate. On the basis of OAVs, cis-rose oxide had the highest values among the common odorants in the three products, indicating its importance to the aroma of both lychee fruit and Gewürztraminer wines. Other compounds that had significant OAVs included beta-damascenone, linalool, furaneol, ethyl hexanoate, and geraniol. This indicated that while differences exist in the aroma profile of lychee and Gewürztraminer, the common odorants detected in both fruit and wine, particularly cis-rose oxide, were responsible for the lychee aroma in Gewürztraminer wine. When headspace SPME was used as a rapid analytical tool to detect the levels of selected aroma compounds deemed important to lychee aroma in Gewürztraminer-type wines, cis-rose oxide, linalool, and geraniol were found to be at relatively higher levels in Gewürztraminers. No cis-rose oxide was detected in the control wines (Chardonnay and Riesling), while lower levels were detected in the Gewürztraminer-hybrid wine Traminette. Gewürztraminers produced in the Alsace region showed differences in the levels of the 3 monoterpenes when compared to those from New York State, which could be attributed to differences in viticultural and enological practices between regions.     

Whey liquid waste of the dairy industry as raw material for potable alcohol production by kefir granules

Kefir granular biomass was used in the fermentation of sweet whey and proved to be more effective compared to single-cell biomass of kefir yeast. The operational stability of the biocatalyst was assessed by carrying out 20 repeated batch fermentations. Levels of ethanol productivity reached 2.57 g L(-1) h(-1)), whereas the yield was 0.45 g/g. The fermentation time was only 8 h. Mixtures of sweet whey with molasses were fermented at initial densities ranging from 4.2 to 10.2 degrees Be and resulted in ethanol yield factors between 0.36 and 0.48 g of ethanol/g of utilized sugar. Lower degrees Be values led to an increase of percentages of ethyl acetate on total volatiles determined and a reduction of amyl alcohols. The addition of 1% black raisin extract to whey appears to promote whey fermentation, whereas the same was not observed in the case of white sultana extract addition. It was finally established that it is preferable to ferment mixtures of whey-molasses by adding molasses in whey after the completion of whey fermentation.     

Effect of carbohydrate substrate on fermentation by kefir yeast supported on delignified cellulosic materials

The suitability of delignified cellulosic (DC) material supported kefir yeast to ferment raw materials that contain various single carbohydrates, for the production of potable alcohol and alcoholic drinks, is examined in this investigation. Results are reported of fermentations carried out with sucrose, fructose, and glucose in synthetic media. Repeated batch fermentations at various initial sugar concentrations of sucrose, fructose, and glucose were performed at 30 degrees C in the presence of the aforementioned biocatalyst. The results clearly show feasible yields in the range of 0.38-0.41 g/g, alcohol concentrations of 7.6-8.2% v/v, fermentation time of 90-115 h, and conversion of 92-96%. DC material supported kefir fermented 11-fold more rapidly than free cells and 9-fold more rapidly in comparison to kissiris supported kefir. The main volatile byproducts such as amyl alcohols (mixture of 2-methyl-1-butanol and 3-methyl-1-butanol), ethanal, and ethyl acetate were formed in all sugar fermentation products. The formation of 65-110 ppm of ethyl acetate is as high and even higher than that obtained with traditional wine yeasts. The increase of the initial concentration of sugar in the fermentation media resulted in an increase in contents of volatiles. The fine aroma that was obtained in the product of fructose could be attributed to the high percentage of ethyl acetate on total volatiles. The efficiency of DC material supported kefir was the same for the fermentations of individual sugars or a mixture of fructose, sucrose, and glucose. When whey with raisin extracts was fermented, lower yields were obtained but the aroma of the product was even better.     

Comparison of the concentrations of phenolic constituents in cane sugar manufacturing products with their antioxidant activities

Polyphenol content and free radical scavenging capacity of seven kinds of sugar manufacturing products (A sugars, clear juices, syrups, massecuite, and A, B, and C molasses) were studied. Seventy-two samples were collected at different stages of the process during two sugar harvests from a local sugar factory (Bois-Rouge, La Réunion). The total phenolic content of sugar products was determined according to the Folin-Ciocalteu assay. Polyphenols of sugar products were extracted with ethyl acetate and quantified by LC-UV-ESI-MS during all of the process. ABTS and DPPH assays were applied to aqueous solution of sugar products, which exhibited interesting free radical scavenging activity. Comparatively, ethyl acetate extracts exhibited higher antioxidant activity. Multivariate analyses (principal component analysis and canonical discriminant analysis) demonstrated a significant correlation between polyphenols and antioxidant activity. Moreover, it was observed that the sugar process results in an increase of the phenolic content and the free radical scavenging capacity of the different products. These products and especially molasses proved to be a rich source of natural antioxidants and may represent an interesting alternative to synthetic food antioxidants.     

加热处理对蜂蜜酒香气物质的影响

为研究适合蜂蜜酒发酵的优良工艺条件,以2批荆条蜜(白色和浅琥珀色)为原料,在酒精发酵前对发酵醪液进行加热处理,以不加热处理的样品为对照,采用酿酒酵母FX10进行发酵,发酵结束后测定蜂蜜酒的各项理化指标及挥发性化合物的含量。结果表明,供试酒样中共检测出77种挥发性物质,其中酯类39种、醇类20种、酸类8种、萜烯类4种、羰基化合物6种。加热处理可以显著增加蜂蜜酒中香气物质的种类和含量,含量较高的香气物质有乙酸乙酯、乙酸苯乙酯、乙酸异戊酯、己酸乙酯、辛酸乙酯、癸酸乙酯、月桂酸乙酯、9-十六碳烯酸乙酯、异戊醇、β-苯乙醇、辛酸和癸酸。对蜂蜜酒中香气物质进行主成分分析,发现加热处理的酒样中酯类物质对酒香贡献较大;对照酒样中酯类物质对酒香贡献较小,而醇类物质是其主要挥发性成分。本研究结果为蜂蜜酒的生产提供了一定的理论依据。     

Odor potency of aroma compounds in Riesling and Vidal blanc table wines and icewines by gas chromatography-olfactometry-mass spectrometry

This study aimed to elucidate the odor potency of aroma compounds in Riesling and Vidal blanc (syn. Vidal) table wines and icewines from the Niagara Peninsula using stir bar sorptive extraction-gas chromatography-olfactometry-mass spectrometry. Dilution analysis determined the most odor-potent compounds in Vidal and Riesling icewines (n = 2) and table wines (n = 2) from a commercial producer. The top 15 odor-potent compounds in each wine were identified and quantified, resulting in 23 and 24 compounds for Riesling and Vidal, respectively. The most odor-potent compounds were β-damascenone, decanal, 1-hexanol, 1-octen-3-ol, 4-vinylguaiacol, ethyl hexanoate, and ethyl 3-methylbutyrate. In general, icewines had higher concentrations of most aroma compounds compared to table wines. Through computation of odor activity values, the compounds with the highest odor activity for the icewines were β-damascenone, 1-octen-3-ol, ethyl octanoate, cis-rose oxide, and ethyl hexanoate. In table wines the highest odor activity values were found for ethyl octanoate, β-damascenone, ethyl hexanoate, cis-rose oxide, ethyl 3-methylbutyrate, and 4-vinylguaiacol. These findings provide a foundation to determine impact odorants in icewines and the effects of viticultural and enological practices on wine aroma volatile composition.     

Identification of components responsible for the odor of cigar smoker's breath

Following smoking 1/2 of a cigar, the most odorous cigar tobacco smoke components extracted from the surface of the tongue by nylon-meshed swabs and then extracted from the swab headspace by solid phase microextraction were ethyl pyrrole, 2,3-dimethyl pyrazine, and 2-ethyl pyridine. Similar classes of compounds were identified from the headspace of an aqueous simulated saliva solution treated with cigar smoke. The most odorous compounds were 2,3,5-trimethyl pyridine, 2,5-dimethyl pyrazine, and 2-ethyl-3,5-dimethyl pyridine. Pyridines and pyrazines, the most prominent classes of odorous compounds identified in this experiment, may be generated during cigar pyrrolysis by cleavage of nicotine or by Maillard reaction.     

Volatile Compounds in Crumb of Whole‐Meal Wheat Bread Fermented with Different Yeast Levels and Fermentation Temperatures

The influence of fermentation temperatures (8, 16, and 32°C) and yeast levels (2, 4, and 6%) on the formation of volatile compounds in the crumb of whole‐meal wheat bread was investigated. Volatile compounds were extracted by dynamic headspace extraction and analyzed by gas chromatography–mass spectrometry. Results were evaluated with multivariate data analysis and ANOVA. Bread fermented at a high temperature (32°C) had higher peak areas of the Maillard reaction products 2‐furancarboxaldehyde, 2‐acetylfuran, 2‐methylpyrazine, and phenylacetaldehyde compared with bread fermented at lower fermentation temperatures. Bread fermented at low temperatures (8 and 16°C) was characterized by having higher peak areas of the fermentation products 3‐methylbutanal, 2‐methylbutanal, ethyl acetate, ethyl hexanoate, ethyl propanoate, and 3‐methylbutanol. Fermentation of bread with 6% yeast resulted in a higher peak area of the important fermentation product 2‐phenylethanol. It also reduced the peak areas of important lipid oxidation products. The peak area of 2,3‐butanedione was also relatively higher in bread fermented with 6% yeast compared with lower yeast levels; however, an interaction was seen between the high yeast level and all three fermentation temperatures. In contrast, fermentation with a low yeast level (2%) resulted in bread with relatively higher peak areas of 2‐ and 3‐methylbutanal, as well as (E)‐2‐nonenal and (E,E)‐2,4‐decadienal, which are important lipid oxidation compounds in bread.