Effect of enzymes on extraction of volatiles from celery seeds

Celery (Apium graveolens L.), belonging to the family Apiaceae, is widely used as a spice, in perfumery and pharmaceutical applications. It is reported to possess several nutraceutical attributes, such as anticoagulation activity of blood plasma and prevention of cardiovascular diseases. Effects of various enzymes on the extraction of volatile oil of celery are reported in the present study. The oil yield, after cellulase, pectinase, protease and viscozyme pretreatment, was in the range 2.2–2.3% as against 1.8% in a control sample, by steam distillation. Profiling of the celery oil thus obtained by GC–MS showed that limonene, the major terpene, increased from 63% to 82% with enzyme treatment. The other major flavour compounds identified were β-selinene (16–17%), butyl phthalide and sedanolide. The study demonstrated that enzymes facilitated the extraction of celery oil with increase in oil yield with little change in either flavour profile or physicochemical properties of the oil.     

超临界CO2-分子蒸馏纯化蒜油与水蒸气蒸馏法制取蒜油挥发性成分分析

采用分子蒸馏技术(MD)将超临界CO2(SFE)萃取的蒜油进行纯化,以顶空固相微萃取气质联用技术(HSSPME-GC-MS)分析蒜油中的挥发性成分,确定最佳工艺：进样速度1 滴/s,蒸馏温度60℃,刮膜转速250r/min。纯化的蒜油挥发性成分仅有4 种,二烯丙基二硫醚和二烯丙基三硫醚、2- 乙烯基-1,3- 二硫杂-4- 环己烯和3- 乙烯基-1,2- 二硫杂-5- 环己烯;与水蒸气蒸馏法制得的新鲜蒜油(F-GO)比较,SFE 法是一种理想的制取蒜油的方法;蒜油放置30d(S-GO)后有效成分含量下降,导致品质下降。     

Volatile constituents from Romanesco cauliflower

The volatile and semi-volatile constituents of Brassica oleracea L. var. Botrytis L., Romanesco group, Navona variety, were extracted by steam distillation from leaves and inflorescence, using a Likens–Nickerson-type apparatus. The extracts from fresh, ripening and frozen vegetables were investigated by gas chromatography and mass spectrometry. From the fresh leaves extract, a total of 61 compounds were identified, representing 96.8% of the oil. The major constituent was found to be hex-3(Z)-enol (61.1%). From fresh disrupted inflorescence tissues of Romanesco, 35 compounds were detected, representing 97.7% of the extract. Dimethyl disulfide, dimethyl trisulfide and hex-3(Z)-enol were identified as major constituents of the hydrodistillation products, representing, respectively, 30.2, 24.2 and 21.7% of the volatiles. From ripening and frozen inflorescence tissues, dimethyl disulfide and trisulfide were again detected as predominant components. In the latter, hex-3(Z)-enol had almost disappeared (0.8%) whereas dimethyl trisulfide represented 49.7% of the oil. This is the first report concerning the steam distillation compounds present in the leaves and inflorescence tissues of this species.     

A New Essential Oil Chemotype of Allium Roseum Analyzed by an Apolar Column

This study deals with the chemical characterization of a medicinal and an aromatic plant of the Tunisian flora: Allium roseum var. odoratissimum, and aimed to identify new bioactive natural compounds in its flower essential oil. These compounds were extracted by hydrodistillation and were analyzed by GC and GC/MS, using an apolar column. The most important compounds characterized were organo-sulphurous (46%), including methyl 2-propenyl trisulfide, di-2-propenyl trisulfide, di-1-propenyl disulfide, di-2-propenyl disulfide, dimethyl trisulfide, methyl 2-propenyl disulfide, and di-1-propenyl trisulfide, found as 10.75, 9.07, 5.81, 4.98, 3.90, 3.30, and 2.53%, respectively. Moreover, heneicosane and pentacosane were identified for the first time at relatively high rates (8.18 and 4.49%, respectively) in the Allium roseum essential oil. This essential oil composition exhibited newly identified sulphurous compounds at relatively high rates (46.53%) when compared with what was found while using polar column.     

Enzyme-assisted extraction of volatiles from cumin (Cuminum cyminum L.) seeds

The effect of various enzymes on the extraction of the volatile oil of cumin (Cuminum cyminum L.) is reported in the present study. The oil yield, after pre-treatment of cumin seeds with cellulase, pectinase, protease and Viscozyme, was in the range 3.2–3.3% compared to 2.7% in a control sample. Profiling of the cumin oil by GC–MS showed that the total hydrocarbon content was 63.7%, 66.1% and 70.1% in control, cellulase and Viscozyme treated samples, respectively. However, there was no change in the content of cuminaldehyde, the principal flavour-impact constituent, in any of the volatile oils. The study demonstrated that enzymes facilitated the extraction of cumin oil with increase in oil yield, with little change in either flavour profile or physicochemical properties of the oil.     

Evaluation of size reduction on the yield and quality of celery seed oil

The effect of grinding/flaking with and without pre-cooling of celery seeds on the yield and physical and chemical characteristics of volatile oil was evaluated. For smaller batches (200 g) with pre chilling and flaking, yields of oil were marginally but consistently higher (2.20%), compared to grinding celery at ambient temperature using a mini plate mill (1.9%) and with waring blender (1.8%). With flaking at room temperature the yield of oil was 2.0%. However, in large batches (10 kg), with steam distillation the yield of steam distilled oil was significantly higher for flaking (1.76%) as compared to the hammer mill powdering (1.4%), both at room temperature. Extraction of volatile oil from celery powder or flakes follows first order kinetics with an variance value of 0.04. Gas chromatograph (GC) and gas chromatograph–mass spectra (MS) analysis showed that in case of flaking, the volatile oil had higher levels of limonene, the major volatile compound and sedanenolide, the major character impact compound being present in almost equal quantities in both the cases of flakes and powder. Selective collection of volatile oil at different intervals of time of distillation gave products of different flavour profiles. Flaking had the advantage of higher yields of the volatile oil with better flavour quality. It was also observed that flaking of celery helped in overcoming the problem of clogging and choking which is associated with the conventional grinding.     

Investigation of the volatile aroma components of garlic leaves essential oil. Possibility of utilization to enrich garlic bulb oil

The volatile aroma components of Egyptian green garlic leaves essential oil was investigated for the first time. After the utilization of garlic bulbs to prepare garlic oil or after drying the bulbs to produce garlic powder, garlic leaves are considered to be waste material, which is disposed of without any benefit. In this investigation, green garlic leaves were distilled and the essential oil was subjected to GC and GC-MS identification. The yield of the oil was 0.06% (based on wet weight of the leaves). The most prominent compounds of the essential oil were diallyl trisulfide (32.32%), followed by diallyl disulfide (31.35%) and methyl allyl trisulfide (11.40%); these compounds are the same as those found in garlic bulb oil. This means that garlic leaf oil is a rich, renewable and priceless source of garlic aroma compounds which could be utilized in fortification and enriching of garlic bulb essential oil to increase its quantity without changing the quality. Utilization of green garlic leaves for production of essential oil will also save, to some extent, the costs of disposing of large amounts of leaves in garlic possessing factories, transforming them into profits.     

同时蒸馏萃取- 气质联机分析腌渍野韭菜花香成分

以乙醚为溶剂,采用同时蒸馏萃取法提取腌渍野韭菜花精油,提取率0.29%。用气相色谱- 质谱法结合气相色谱保留指数定性方法,从腌渍野韭菜花精油中鉴定出37 种挥发性成分,占精油总成分的95.75%。主要成分为二甲基三硫醚(28.18%)、二甲基二硫醚(18.13%)、甲基丙烯基二硫醚(14.24%)、甲基烯丙基三硫醚(4.89%)、甲基烯丙基二硫醚(3.19%)、甲基甲硫基甲基二硫醚(3.10%)、4- 乙烯基愈创木酚(2.93%)、二烯丙基二硫醚(2.71%)、二甲基四硫醚(2.67%)、3- 羟基-2- 丁酮(2.42%)、2- 乙烯基-2- 丁烯醛(1.54%)、2,5- 二甲基-1,3,4- 五硫三环(1.45%)、苯甲醇(1.31%)和甲硫基甲磺酰基甲烷(1.28%)等。其中硫醚和多硫醚类成分11 种,相对含量79.99%,是腌渍野韭菜花的特征香气成分。     

大葱挥发油含量与化学成分的分析

采用水蒸气蒸馏法提取莱芜鸡腿葱中的挥发油 ,测知其含量为 0 0 1 % ;并用毛细管气相色谱 /质谱法定性鉴别了挥发油中的 2 5种化学成分。其中含硫有机硫化合物为 2 0种 ;主要成分有 :丙基甲基硫代硫磺酸酯 ,甲基烯丙基硫代硫磺酸酯 ,甲基丙烯基三硫醚 ,烯丙基硫醇 ,甲丙基二硫醚 ,反式甲基烯丙基二硫醚 ,二甲基三硫醚 ,二丙基二硫醚 ,反式烯丙基丙基二硫醚 ,二甲基四硫醚 ,二丙基三硫醚 ,反式烯丙基丙基三硫醚 ,顺式烯丙基丙基三硫醚 ,甲硫醇 ,丙硫醇 ,二巯基甲烷 ,2 ,5 二甲基噻吩等含硫化合物 ,还鉴定出不饱和脂肪醛 1种 (3 ,7 二甲基 2 ,6 二辛烯醛 ) ,脂肪酮 1种 (十一酮 2 ) ,萜烯类化合物 2种 (2 甲基 庚稀 2和顺式 2 ,6 二甲基 2 ,6 辛二烯 ) ,挥发性无机化合物 1种 (SO2 )。     

二次分子蒸馏提取与市售大蒜油的气质联用分析和比较

采用二次分子蒸馏技术提取大蒜中大蒜油,并运用气相色谱- 质谱联用分析,通过计算机检索与标准谱图对照,鉴定大蒜油中组分和主要化学成分,比较提取所得大蒜油与市售大蒜油的化学成分差异。结果表明：经分子蒸馏法所得大蒜油产物中主要含有二烯丙基一硫化物、二烯丙基二硫化物、甲基二硫化物、二烯丙基硫代亚磺酸酯及三硫醚等化合物,未检测出环状二硫醚和四硫醚化合物。     

大蒜挥发油提取工艺的优化研究

采用L9(34)正交试验法,研究大蒜挥发油最优提取工艺。以挥发油得率为指标,以发酵温度、料液比、浸泡时间、蒸馏时间为研究因素,在单因素试验的基础上,进行正交试验。结果：影响大蒜挥发油提取的最主要因素为蒸馏时间,其次为加水量、发酵温度、浸泡时间。最佳提取工艺条件为：发酵温度35℃,料液比1:3.5(m/V),浸泡4h,提取2h。此提取工艺简便易行,在此最佳提取工艺条件下提取率为0.35%。     

不同提取方法所得茴香油的甄别研究

本试验通过对三种不同工艺提取的八角茴香油中有效成分的GC-MS比较分析,探索了溶剂提取法、水蒸汽蒸馏法、超临界CO2萃取法生产茴香油的初步甄别方法。研究结果表明：在GC-MS色谱图中,有?-水芹烯、樟脑这两种成分出现并且相对含量分别达到0.25%、0.15%及以上时,可以认为这种茴香油是超临界CO2萃取法得到的;而苯二甲酸单(2-乙基己基)酯、异丁香酚甲醚是溶剂提取法特有的成分;水蒸汽蒸馏法生产的茴香油中组分最少,而其中含有的甲基己烯雌酚是其特征性物质,但大茴香脑所占比重最大可以达到80%。     

大蒜精油抗菌活性研究

采用琼脂扩散法及肉汤稀释法研究了大蒜精油的抗菌活性.使用GC-MS分析此精油的成分,其中二烯丙基三硫醚(49.23%)及二烯丙基二硫醚(19.35%)为最主要成分.以枯草芽孢杆菌、金黄色葡萄球菌、表皮葡萄球菌、大肠杆菌、绿脓杆菌、变形杆菌、黑曲霉和白色念珠菌为供试菌种,结果显示大蒜精油对于所选的8种菌均有一定的抗菌活性,尤对黑曲霉、白色念珠菌和表皮葡萄球菌有较好的杀灭作用.实验证明大蒜精油在食品及医药工业有广泛的应用前景.     

Effects of Onion (Allium cepa L.) and Garlic (Allium sativum L.) Essential Oils on the Aspergillus versicolor Growth and Sterigmatocystin Production

Abstract: In the present study the effects of individual and combined essential oils (EOs) extracted from onion (Allium
cepa L.) bulb and garlic (Allium sativum L.) clove on the growth of Aspergillus versicolor and sterigmatocystin (STC) production were investigated. The EOs obtained by hydrodistillation were analyzed by GC/MS. Twenty one compounds were identified in onion EO. The major components were: dimethyl‐trisulfide (16.64%), methyl‐propyl‐trisulfide (14.21%), dietil‐1,2,4‐tritiolan (3R,5S‐, 3S,5S‐ and 3R,5R‐ isomers) (13.71%), methyl‐(1‐propenyl)‐disulfide (13.14%), and methyl‐(1‐propenyl)‐trisulfide (13.02%). The major components of garlic EO were diallyl‐trisulfide (33.55%), and diallyl‐disulfide (28.05%). The mycelial growth and the STC production were recorded after 7, 14, and 21 d of the A. versicolor growth in Yeast extract sucrose (YES) broth containing different EOs concentrations. Compared to the garlic EO, the onion EO showed a stronger inhibitory effect on the A. versicolor mycelial growth and STC production. After a 21‐d incubation of fungi 0.05 and 0.11 μg/mL of onion EO and 0.11 μg/mL of garlic EO completely inhibited the A. versicolor mycelial growth and mycotoxins biosynthesis. The combination of EOs of onion (75%) and garlic (25%) had a synergistic effect on growth inhibition of A. versicolor and STC production. Practical Application: A substitution of synthetic preservatives with natural antimicrobial compounds in food safety to control fungal contamination and mycotoxin production.     

Stabilization of sunflower oil by garlic extract during accelerated storage

Efficacy of garlic extract in stabilizing sunflower oil during accelerated storage has been studied. Extracts of garlic were prepared in different solvents; extract yield was in the range of 6.24–23.2% and antioxidant activity range in the linoleic acid system was 14.1–93.2%. Being highest in yield and antioxidant potential, methanolic extract was thermally evaluated by heating the extract at 185 °C for different intervals, i.e. 0–80 min and evaluating antioxidant activity of the heated extract in the linoleic acid system (71.6% inhibition). Methanolic extract of garlic at three different concentrations, i.e. 250 (SFO-250), 500 (SFO-500) and 1000 ppm (SFO-1000) were added to preheated RBD sunflower oil. BHA (SFO-BHA) and BHT (SFO-BHT) at 200 ppm served as standards besides the control. Weight gain (WG), antioxidant activity index (AAI), free fatty acid (FFA) content, peroxide value (PV), conjugated dienes (CD), conjugated trienes (CT) and thiobarbituric acid-reactive substances (TBARS) were taken as parameters for evaluation of effectiveness of garlic in stabilization of sunflower oil. Results from different parameters were in agreement with each other, suggesting the highest efficiency of SFO-1000, followed by SFO-BHT, SFO-BHA, SFO-500, SFO-250 and Ctrl. Results reveal garlic to be a potent antioxidant for stabilization of sunflower oil.     

月桂叶精油的3种制备方法比较及应用

采用超临界CO₂萃取、亚临界CO₂萃取和水蒸气蒸馏法分别制备月桂叶精油,采用正交试验分别优化超临界CO₂和亚临界CO₂萃取月桂叶精油工艺条件,采用GC/MS法分析3种精油的化学成分,并进行卷烟加香试验。结果表明:①超临界CO₂萃取最佳条件为萃取压力30 MPa、萃取时间1h、萃取温度55℃,月桂叶精油得率为2.37%;亚临界CO₂萃取最佳条件为萃取压力20 MPa、萃取时间1 h、萃取温度15℃,月桂叶精油得率为2.16%;二者得率均明显高于水蒸气蒸馏法(1.25%)。②超临界CO₂萃取月桂叶精油共检测出66种致香成分,主要为1,8-桉叶油素(16.43%)、a-乙酸松油酯(15.68%)、芳樟醇(12.84%)等;亚临界CO₂萃取月桂叶精油共检测出62种致香成分,主要为1,8-桉叶油素(17.22%)、a-乙酸松油酯(16.11%)、芳樟醇(11.84%)等;水蒸气蒸馏月桂叶精油检测出49种致香成分,主要为1,8-桉叶油素(18.39%)、a-乙酸松油酯(15.60%)、芳樟醇(9.60%)等。③超临界CO₂和亚临界CO₂萃取月桂叶精油在改善香气质、刺激性、余味方面效果相当,且均优于水蒸气蒸馏月桂叶精油。      

不同大蒜精油成分及生物活性对比分析

为了解白皮大蒜和紫皮大蒜精油成分及生物活性差异,采用水蒸气蒸馏法提取白皮大蒜和紫皮大蒜精油,通过气相色谱质谱联用仪(GC-MS)分析测定两种大蒜精油的可挥发性成分;用对倍稀释法研究两种大蒜精油对几种常见病原菌的抑制活性;采用小叶碟法测定两种大蒜精油对斜纹夜蛾的拒食活性;并检测白皮、紫皮大蒜精油对ABTS、DPPH和OH自由基的清除作用。结果表明:白皮大蒜精油鉴定出26种成分,占精油的95.79%;紫皮大蒜精油鉴定出22种成分,占精油的94.26%,主要杀菌物质大蒜辣素和大蒜新素在紫皮大蒜(59.34%)中的含量比白皮大蒜(50.11%)多;两种大蒜精油对实验用菌有明显抑制作用,尤其紫皮大蒜精油对枯草芽孢杆菌、白色念珠菌、热带假丝酵母菌和板栗疫病的抑制效果比白皮大蒜好;白皮大蒜和紫皮大蒜精油对斜纹夜蛾24h平均拒食率分别为52.97%和100%;白皮大蒜精油对ABTS和DPPH自由基的清除率高于紫皮大蒜精油,对OH自由基的清除率基本相当。     

Glucosinolate degradation products and other bound and free volatiles in the leaves and roots of radish (Raphanus sativus L.)

The volatile constituents from the leaves and roots of Raphanus sativus var. black, white and red were isolated by hydrodistillation in a Clevenger-type apparatus and were analysed by gas chromatography and gas chromatography–mass spectrometry. The major components found in the oil of all leaves were phytol (65.3–69.7%), hexadecanoic acid (2.5–14.3%), methyl linolenate (2.1–11.1%) and (Z)-3-hexen-1-ol (0.7–6.9%). Corresponding aliphatic or aromatic glucosinolate compounds identified in the leaves constituted only 0.3–5.7% of the isolated volatiles. They were 5-(methylthio)-4-pentenenitrile (0.3–2.2%), 4-(methylthio)butyl isothiocyanate (0.3–1.7%), 2-phenylethyl isothiocyanate (0.4%), 4-(methylthio)-3-butenyl isothiocyanate, 4-methylpentyl isothiocyanate, benzyl isothiocyanate and benzenepropanenitrile. The major components in the oil of all roots were hexadecanoic acid (30.3–49.9%), 4-(methylthio)butyl isothiocyanate (17.9–25.7%), methyl linolenate (8.5–21.7%), 5-(methylthio)-4-pentenenitrile (1.5–6.9%), dimethyl trisulfide (1.1–3.8%), 5-(methylthio)pentyl isothiocyanate (0.5–2.0%), 4-(methylthio)-3-butenyl isothiocyanate (0.2–1.8%) and 2-phenylethyl isothiocyanate (0.1–1.5%).     

分子蒸馏法分离提取大蒜精油

采用分子蒸馏技术,依据Box-Behnken 设计原理和响应面分析法,探讨分子蒸馏不同因素对分离、提取大蒜中大蒜精油的影响,选择最佳提取条件。结果表明：当控制系统的压力105Pa、进料速度1.2g/min、进料温度40～55℃范围内,蒸馏温度45.1℃时具有最好的二次分子蒸馏效果,大蒜精油的外观质量明显提高,平均总提取率可达0.476%,大蒜精油中水分为0.15%,纯度达99.85%。     

Influence of drying and extraction methods on yield and chemical composition of the essential oil of Satureja hortensis

The aerial parts of Satureja hortensis, cultivated in Iran (Research Station of Alborz, Karaj), were collected at the full-flowering stage and dried by three different drying methods (sun-drying, shade-drying and oven-drying at 45 °C). The essential oils of every treatment were obtained by hydro-distillation of the aerial parts. In addition, the essential oil of shade-dried sample was obtained by two other distillation methods (water- and steam-distillation and direct steam-distillation). The oils were analyzed by capillary GC and GC–MS. Statistical analysis showed no significant difference between oil yield (w/w) of the oven-dried sample (1.06%) compared to shade-dried (0.94%) and sun-dried (0.87%). The oil content of the shade-dried sample, obtained by hydro-distillation, was higher (0.94%) than that of the steam-distilled (0.27%). Twenty-three components were identified in the oil of S. hortensis in the different drying methods, including carvacrol (46.0–48.1%) and γ-terpinene (37.7–39.4%) as main components. Seventeen compounds were characterized in the oils of different distillation methods, including carvacrol (12.3–46%) and γ-terpinene (37.7–70.4%). Although the drying methods had no significant effect on oil composition of S. hortensis, the distillation changed the percentage of main components sharply (significant at 1%). The steam-distillation method produced the lowest amount of carvacrol and highest amount of γ-terpinene. The results showed that extraction by hydro-distillation gave the best results for S. hortensis, based on oil yield and carvacrol percentage.