Headspace solid phase microextraction and gas chromatography-olfactometry dilution analysis of young and aged Chinese "Yanghe Daqu" liquors

The aroma compounds of young and aged Chinese "Yanghe Daqu" liquor samples were extracted by solid phase microextraction (SPME) and analyzed by gas chromatography (GC)-olfactometry dilution analysis. The original liquor samples were diluted with deionized water to give a final alcohol content of 14% (v/v). The samples were stepwise diluted (1:1) with 14% (by volume) ethanol-water solution and then extracted by headspace SPME. The samples were preequilibrated at 50 degrees C for 15 min and extracted with stirring at the same temperature for 30 min prior to injection into GC. The aroma compounds were identified by both GC-MS and GC-olfactometry using DB-Wax and DB-5 columns. The results suggested that esters were the major contributors to Yanghe Daqu liquor aroma. Ethyl hexanoate, ethyl butanoate, and ethyl pentanoate had very high flavor dilution values in both young and aged liquors (FD > 8192). Methyl hexanoate, ethyl heptanoate, ethyl benzoate, and butyl hexanoate could also be very important because of their high flavor dilution values (FD > or = 256). Moreover, two acetals, 1,1-diethoxyethane and 1,1-diethoxy-3-methylbutane, also were shown high flavor dilution values in Yanghe Daqu liquors (FD > or = 256). Other aroma compounds having moderate flavor dilution values included acetaldehyde, 3-methylbutanol, and 2-pentanol (FD > or = 32). Comparing young and aged liquors, the aroma profiles were similar, but the aroma compounds in the aged sample had higher flavor dilution values than in the young ones.     

Characterization of aroma compounds of chinese "Wuliangye" and "Jiannanchun" liquors by aroma extract dilution analysis

Aroma compounds in Chinese "Wuliangye" liquor were identified by gas chromatography-olfactometry (GC-O) after fractionation. A total of 132 odorants were detected by GC-O in Wuliangye liquor on DB-wax and DB-5 columns. Of these, 126 aromas were identified by GC-mass spectrometry (MS). Aroma extract dilution analysis (AEDA) was further employed to identify the most important aroma compounds in "Wuliangye" and "Jiannanchun" liquors. The results showed that esters could be the most important class, especially ethyl esters. Various alcohols, aldehydes, acetals, alkylpyrazines, furan derivatives, lactones, and sulfur-containing and phenolic compounds were also found to be important. On the basis of flavor dilution (FD) values, the most important aroma compounds in Wuliangye and Jiannanchun liquors could be ethyl butanoate, ethyl pentanoate, ethyl hexanoate, ethyl octanoate, butyl hexanoate, ethyl 3-methylbutanoate, hexanoic acid, and 1,1-diethoxy-3-methylbutane (FD > or = 1024). These compounds contributed to fruity, floral, and apple- and pineapple-like aromas with the exception of hexanoic acid, which imparts a sweaty note. Several pyrazines, including 2,5-dimethyl-3-ethylpyrazine, 2-ethyl-6-methylpyrazine, 2,6-dimethylpyrazine, 2,3,5-trimethylpyrazine, and 3,5-dimethyl-2-pentylpyrazine, were identified in these two liquors. Although further quantitative analysis is required, it seems that most of these pyrazine compounds had higher FD values in Wuliangye than in Jiannanchun liquor, thus imparting stronger nutty, baked, and roasted notes in Wuliangye liquor.     

Purification of xylitol obtained by fermentation of corncob hydrolysates

Hydrolysates obtained by autohydrolysis-posthydrolysis of corncobs were detoxified with charcoal, concentrated, supplemented with nutrients, and fermented with Debaryomyces hansenii. After biomass removal, the fermented media contained 0.1137 kg of nonvolatile components (NVC)/kg of liquor, which corresponded mainly to xylitol (0.6249 kg/kg of NVC) but also to minor amounts of inorganic components (measured as ashes), proteins, nonfermented sugars (xylose and arabinose), uronic acids, arabitol, and other nonvolatile components (ONVC). The media were subjected to further processing (sequential stages of adsorption, concentration, ethanol precipitation, concentration, and crystallization) to obtain food-grade xylitol. Adsorption experiments were carried out at various solid-to-liquor ratios. Under selected conditions (1 kg of charcoal/15 kg of liquors), the xylitol content increased to 0.6873 kg/kg of NVC, and almost total decoloration was achieved. The resulting liquor was concentrated by evaporation to increase its NVC content to 0.4032 kg/kg of liquor (corresponding to a xylitol concentration of 0.280 kg/kg of liquor), and ethanol was added to precipitate a part of the NVC (mainly proteins, but also uronic acids, ashes, and other nonvolatile compounds). Refined liquors (containing 0.7303 kg of xylitol/kg of NVC) were concentrated again, and ethanol was added (to reach 40-60% volume of the stream) to allow crystallization at -10 or -5 degrees C. Under selected conditions, 43.7% of xylitol contained in the initial fermentation broth was recovered in well-formed, homogeneous crystals, in which xylitol accounted for 98.9% of the total oven-dry weight. Material balances are presented for the whole processing scheme considered in this work.     

Characterization of geosmin as source of earthy odor in different aroma type Chinese liquors

Earthy odor is one of the most frequent and serious causes for the aroma deterioration in Chinese liquor, which causes a dirty and dusty impression. The odor in Chinese liquor is similar to that of rice husk, one kind of auxiliary material widely used as a filler in the distillation process. So it is experientially hypothesized that such odor may derive from rice husk. In this paper, the gas chromatography-olfactometry (GC-O) technique and gas chromatography-mass spectrometry (GC-MS) were used to discover and identify the characteristic odoriferous zone of Chinese liquor marked by earthy odor. Geosmin was found to be responsible for this odor. The levels of the compound in ten bottled liquors and thirty liquors aging for different years belonging to four different aroma types were determined by the optimized headspace-solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) method. Quantitative analysis of bottled liquor revealed the presence of geosmin in all aroma type liquors with concentrations ranging from 1.10 μg/L to 9.90 μg/L, except for strong-aroma type liquor. Meanwhile in the aged liquors belonging to the same aroma type, geosmin was detected with significant concentrations and high odor activity values (OAVs) during different years of aging. However, geosmin was not detected in steamed rice husk nor in nonsteamed rice husk, which suggests that rice husk is not the origin of earthy odor in Chinese liquor, and there may be another origin of it during the brewing process.     

Detoxification of corn stover and corn starch pyrolysis liquors by ligninolytic enzymes of Phanerochaete chrysosporium

Phanerochaete chrysosporium (ATCC 24725) shake flask culture with 3 mM veratryl alcohol addition on day 3 was able to grow and detoxify different concentrations of diluted corn stover (Dcs) and diluted corn starch (Dst) pyrolysis liquors [10, 25, and 50% (v/v)] in defined media. GC-MS analysis of reaction products showed a decrease and change in some compounds. In addition, the total phenolic assay with Dcs samples demonstrated a decrease in the phenolic compounds. A bioassay employing Lactobacillus casei growth and lactic acid production was developed to confirm the removal of toxic compounds from 10 and 25% (v/v) Dcs and Dst by the lignolytic enzymes, but not from 50% (v/v) Dcs and Dst. The removal did not occur when sodium azide or cycloheximide was added to Ph. chrysosporium culture media, confirming the participation of lignolytic enzymes in the detoxification process. A concentrated enzyme preparation decreased the phenolic compounds in 10% (v/v) corn stover and corn starch pyrolysis liquors to the same extent as the fungal cultures.     

Optimizing headspace temperature and time sampling for identification of volatile compounds in ground roasted Arabica coffee

Equilibration time and temperature were the factors studied to choose the best conditions for analyzing volatiles in roasted ground Arabica coffee by a static headspace sampling extraction method. Three temperatures of equilibration were studied: 60, 80, and 90 degrees C. A larger quantity of volatile compounds was extracted at 90 degrees C than at 80 or 60 degrees C, although the same qualitative profile was found for each. The extraction of the volatile compounds was studied at seven different equilibration times: 30, 45, 60, 80, 100, 120, and 150 min. The best time of equilibration for headspace analysis of roasted ground Arabica coffee should be selected depending on the chemical class or compound studied. One hundred and twenty-two volatile compounds were identified, including 26 furans, 20 ketones, 20 pyrazines, 9 alcohols, 9 aldehydes, 8 esters, 6 pyrroles, 6 thiophenes, 4 sulfur compounds, 3 benzenic compounds, 2 phenolic compounds, 2 pyridines, 2 thiazoles, 1 oxazole, 1 lactone, 1 alkane, 1 alkene, and 1 acid.     

Estimation of potassium concentration in oil palm (Elaeis guineensis Jacq.) leaf tissue by simple and inexpensive water extraction method

Estimation of potassium (K) concentration in oil palm leaf tissue is routinely carried out in oil palm plantations to manage fertilizer application for getting higher fresh fruit bunch (FFB) production. Since K in plant tissue is not bound to organic complexes and it is extractable by water, this study was carried out to extract K from oil palm leaf tissue by water extraction method. The results were compared with other established methods like 1 normal (N) ammonium acetate (NH₄OAc) extraction, 0.5 N hydrochloric acid (HCl) extraction, and diacid digestion. The proposed water extraction method consists of shaking of 0.5 g finely ground oil palm leaf tissue with distilled water at 1:60 ratio [sample-to-water weight (w)/volume (v)] for a period of 20 min in a reciprocating shaker, filtration of the content, and measurement of K concentration in filtrate by flame photometer. The results of analysis of 30 oil palm leaf samples collected from various production systems under different soil types and management practices for K concentration revealed the close agreement of water extraction method with other established methods. The mean value of K extracted by water extraction method was within 1–10% of the K extracted by other established methods. Water-extractable K was significantly correlated with K extracted by other methods and it could be predicted by other methods. The values of standard error and coefficient of variation for K extracted by different methods were very low, which indicated that the water extraction method was comparable with other established methods.     

Effects of olive, canola, and sunflower oils on the formation of volatiles from the Maillard reaction of lysine with xylose and glucose

Some important edible oils (extra virgin olive oil, canola oil, and sunflower oil) were added to aqueous glucose-lysine or xylose-lysine model systems to investigate their effect on the formation of volatiles from the Maillard reaction (MR). The volatile compounds were extracted by a Likens-Nickerson apparatus and quantified. Pyrazines, Maillard reaction products with an important impact on food flavor, appeared to be particularly sensitive to the presence of the oils in both the xylose-lysine and glucose-lysine model systems. The unsubstituted pyrazine was formed more with olive oil, less with canola oil, and even less with sunflower oil, whereas 2-methylpyrazine, 2,5-methylpyrazine, and 2,3-dimethylpyrazine were formed less with olive oil, more with canola oil, and even more with sunflower. The oxidative states of the oils and their fatty acid fingerprints were determined: the results indicated that the relative amounts of the pyrazines are sensitive to the degree of unsaturation of the oil. The autoxidation of the volatile compounds generated from the MR, investigated by the addition of free radical modulators (antioxidants alpha-tocopherol, 2,6-di-tert-butyl-4-methylphenol, and rosemary extract; or pro-oxidant alpha,alpha'-azobis-isobutyronitrile, a free radical initiator), was limited in respect to aqueous model systems.     

马铃薯茎叶挥发性成分的两种提取方法比较

应用水蒸气蒸馏-溶剂萃取法和微波辅助-溶剂萃取法提取了成熟期马铃薯茎叶挥发性成分。用乙醚为萃取溶剂的水蒸气蒸馏法提取时,以0.533%（m/m）得油率获得精油;以正己烷为溶剂的微波辅助萃取法的最适提取条件为：温度60℃,时间9 min,液料比10︰1（V/m）,在此条件下的得油率为0.528%（m/m）。用GC-MS分析检测出水蒸气蒸馏法获得的精油含有81个成分,解析鉴定出占精油相对含量79.386%的43种物质,醇类化合物（24.789%）为主要成分;微波法获得的精油检测出78个成分,解析鉴定出占总精油82.226%的36种成分,酯类化合物（44.482%）为主要成分。2种提取方法获得的精油成分有很大的差别。     

Processing of rice husk autohydrolysis liquors for obtaining food ingredients

Rice husks are of a lignocellulosic nature, with a hemicellulose fraction made up of substituted arabinoxylan. Rice husks were treated with hot, compressed water (autohydrolysis reaction) under optimized conditions to cause the hydrolytic degradation of arabinoxylan. The reaction products contained volatile components and nonvolatile components (NVC), which were made up of hemicellulose-derived products (substituted oligosaccharides and monosaccharides) and other nonvolatile solutes (ONVS). To decrease the content of ONVS, concentrated autohydrolysis liquors were first subjected to ethyl acetate extraction and then subjected to various alternative treatments (solvent precipitation, freeze-drying solvent extraction, or ion exchange). The resulting liquors were assayed for composition and yield determination. Material balances are presented for the several processes considered. The best results in terms of purification were obtained with sequential stages of ethyl acetate extraction and ion exchange, which led to concentrates with hemicellulose-derived compounds (sugars and substituted sugar oligomers) accounting for 92 wt % of the NVCs.     

菜籽蛋白的提取和纯化

为了对菜籽饼进行综合利用,以低温压榨制油的双低菜籽饼为原料,探讨了菜籽蛋白的提取和纯化工艺.通过料液pH值的先后调节对比、正交、提取次数和纯化试验,得到较佳工艺条件:采用先调pH值法,水溶液的pH值为12,提取时间为20 min,温度为室温,提取3次,通过pH5和7的两步沉淀,经干燥得到分离蛋白,蛋白纯度达84.8%,得率为38.9%,且有害物质残留较少.先调pH值法与后调法相比,总的提取率可提高20个百分点,达90%以上.     

Determination of theaflavins including methylated theaflavins in black tea leaves by solid-phase extraction and HPLC analysis

A quantitative method for four theaflavins and two methylated theaflavin derivatives in black tea leaves was developed by solid-phase extraction and a high-performance liquid chromatographic method with photodiode array detection. The theaflavins in black tea leaves were extracted three times with 40 vol 50% aqueous ethanol (mg dry tea powder/mL) containing 2% ascorbic acid. The ethanol extracts were diluted 4-fold with distilled water. All diluted extracts were directly applied to the solid-phase C18 cartridge column without concentration. The fraction of theaflavins was obtained by 40% ethanol extraction after rinsing with water followed with 15% ethanol extraction. An aliquot of theaflavins after concentration was injected onto an ODS C18 reversed-phase column, and four theaflavins and two methylated theaflavins were sufficiently separated by a linear gradient system using distilled water and acetonitrile with 0.5% acetic acid. This analytical method is sensitive for the determination of a small amount of methylated theaflavins, since various interfering substances produced during the fermentation process were eliminated in advance by solid-phase extraction. Using this analytical method, we also demonstrated that methylated theaflavins were easily produced during the manufacture of black tea.     

Simple and efficient method for the estimation of residues of flubendiamide and its metabolite desiodo flubendiamide

An analytical method was standardized for the estimation of residues of flubendiamide and its metabolite desiodo flubendiamide in various substrates comprising cabbage, tomato, pigeonpea grain, pigeonpea straw, pigeonpea shell, chilli, and soil. The samples were extracted with acetonitrile, diluted with brine solution, and partitioned into chloroform, dried over anhydrous sodium sulfate, and treated with 500 mg of activated charcoal powder. Final clear extracts were concentrated under vacuum and reconstituted into HPLC grade acetonitrile, and residues were estimated using HPLC equipped with a UV detector at 230 lambda and a C18 column. Acetonitrile/water (60:40 v/v) at 1 mL/min was used as mobile phase. Both flubendiamide and desiodo flubendiamide presented distinct peaks at retention times of 11.07 and 7.99 min, respectively. Consistent recoveries ranging from 85 to 99% for both compounds were observed when samples were spiked at 0.10 and 0.20 mg/kg levels. The limit of quantification of the method was worked out to be 0.01 mg/kg.     

玉米茎秆汁液防治坡面土壤侵蚀的室内模拟试验

该文通过室内人工模拟降雨试验,研究了地表施加玉米茎秆汁液对降雨产流产沙强度的影响,旨在探索玉米茎秆汁液是否可以作为土壤改良剂来减少产流产沙强度。试验设计了2种玉米茎秆汁液的施加量(400和800 g)、4种施加浓度(10%、25%、50%和75%)和4种降雨强度(50、25、75、100 mm/h)。结果表明,各施加浓度和施加量的玉米茎秆汁液都能够减少降雨产流产沙强度,且相同条件下的产沙强度减小程度大于产流强度减小程度。当玉米茎秆汁液的施加量为400 g时,随着施加浓度从10%增加至25%、50%和75%,减流百分比分别为31.243%、31.685%、34.595%和39.475%,减沙百分比分别为23.167%、41.993%、37.918%和64.606%;当玉米茎秆汁液的施加量为800 g时,随着施加浓度从10%增加至25%、50%、75%,减流百分比分别为37.583%、56.433%、63.170%和76.360%,减沙百分比分别为48.214%、77.219%、88.572%和95.539%。当施加量和降雨强度相同时,产流产沙强度与施加浓度之间呈显著的指数函数递减关系,产沙强度随降雨强度的变化呈显著的幂函数递增关系。当施加量为400 g时,各施加浓度下的产流强度与降雨强度之间呈显著的线性函数递增关系,当施加量为800 g时,各施加浓度下的产流强度随降雨强度呈显著的指数函数递增关系。研究为水力侵蚀的防治提供了新思路,为水蚀荒漠化的防治提供了新方法。     

Relationship between procyanidin and flavor contents of cocoa liquors from different origins

The flavor of eight cocoa liquors of different origins (Africa, America, and Asia) and different varieties (Fine grades: criollo, trinitario, and nacional. Bulk-basic grade: forastero.) was analyzed by headspace solid-phase microextraction mass spectrometry (HS-SPME-MS). Their procyanidin contents were quantified by HPLC-UV (280 nm). Fine varieties with short fermentation processes proved to contain more procyanidins, while criollo from New Guinea and forastero beans showed the highest aroma levels. The levels of cocoa aroma compounds formed during roasting are shown to vary directly with bean fermentation time and inversely with residual procyanidin content in cocoa liquor. Measurement of antioxidant activity in cocoa liquor proved to be a useful tool for assessing residual polyphenols.     

微波提取法对樱桃、猕猴桃和枸杞多糖特性的影响

微波提取是近年来发展迅速的天然产物提取技术之一。为考察微波提取对多糖得率、结构及生物学功能的影响,论文采用微波功率1 000 W和提取温度140℃,以不同提取时间5,10 和20 min分别对樱桃、猕猴桃和枸杞中多糖进行提取。结果表明,微波提取多糖的得率、相对分子质量和抗氧化性低于传统提取方法,随着微波提取时间延长,多糖相对分子质量逐步降低,但多糖得率与抗氧化性无显著变化;微波提取得到的多糖在单糖组成上与传统提取方法有一定的差异。该研究结果对应用微波提取水果多糖条件的选择及多糖品质控制有一定的参考价值。     

Optimization of extraction of phenolic compounds from flax shives by pressurized low-polarity water

Pressurized low-polarity water (PLPW) extraction of phenolic compounds from flax shive was investigated using statistically based optimization and the "one-factor-at-a-time" method. Extraction variables examined using central composite design (CCD) included temperature, flow rate, and NaOH concentration of the extracting water. Extraction of phenolic compounds including p-hydroxybenzaldehyde, vanillic acid, syringic acid, vanillin, acetovanillone, and feruric acid was affected by temperature and NaOH concentration; and extraction of all phenolic compounds, except ferulic acid, increased with temperature and NaOH concentration of the extracting water. Flow rate had little effect on concentration of phenolic compounds at equilibrium, but the extraction rate at the early phase was higher for higher flow rates. The mechanism of PLPW extraction of flax shive phenolics was also investigated using a two-site kinetic model and a thermodynamic model. To determine the extraction mechanism, flow rate was varied from 0.3 to 4.0 mL/min while temperature and NaOH concentration were fixed at 180 degrees C and 0.47 M, respectively. The flow rate tests showed the extraction rates of total phenolic (TP) compounds increased with flow rate and can be described by a thermodynamic model. The results from the thermodynamic model demonstrated that a K(D) value of 30 agreed with the experimental data in the flow rate range of 0.3-4.0 mL/min. When the effect of the three independent variables was evaluated simultaneously using CCD, a maximum TP concentration of 5.8 g/kg of dry flax shive (DFS) was predicted from the combination of a high temperature (230.5 degrees C), a high initial concentration of NaOH (0.63 M), and a low flow rate (0.7 mL/min). Maximum TP concentration of 5.7 g/kg of DFS was obtained from extraction conditions of 180 degrees C, 0.3 or 0.5 mL/min, and 0.47 M NaOH at equilibrium. A second-order regression model generated by CCD predicted a maximum TP concentration of 5.8 g/kg of DFS under the same extraction conditions, which is well matched with the results from experimental data.     

蛋黄油的提取及其氧化产物挥发性成分分析

为提高淘汰蛋鸡副产物——卵泡的利用率,本研究以鸡卵泡为试验原料,经提取卵磷脂、脱去胆固醇后,将其卵泡残渣以溶剂萃取法提取出蛋黄油,通过单因素试验和正交试验研究了提取温度、提取时间、料液比和乙醇浓度对蛋黄油提取的影响。之后将提取的蛋黄油进行氧化调控,采用气相离子迁移色谱(GC-IMS)进行测定与分析。正交试验结果表明,鸡卵泡中蛋黄油提取的最佳工艺条件:提取温度80℃,提取时间55 min,料液比1∶10,乙醇浓度95%。氧化蛋黄油中含有多种挥发性物质,包括4种醇类、3种醛类、2种酯类、2种酮类、1种呋喃,其中3-甲基丁醛是氧化蛋黄油的特征风味物质。本研究结果为开发利用蛋鸡副产物,提高产品附加值提供了新思路。