均匀设计法优化超临界CO2萃取丁香精油工艺研究

采用单因素试验和均匀设计法U_6(6~4)试验结合的方法优化利用超临界CO_2萃取技术提取丁香精油的工艺。单因素试验研究温度、压力、CO_2流速、颗粒度因素对丁香精油得率的影响,利用均匀设计法优化获得最优萃取工艺。试验结果显示,超临界CO_2萃取丁香精油的最佳工艺条件为:萃取温度55℃、萃取压力25 MPa、CO_2流速1.5 L/min、颗粒度150目。最优工艺条件下,丁香精油得率26.86%,丁香精油中主要成分含量:丁香酚59.91%、β-石竹烯18.02%、乙酰基丁香酚13.97%;主要成分总量91.90%。     

均匀设计法优化丁香精油提取工艺及其抑菌活性研究

采用单因素试验和均匀设计试验法U6(64)优化有机溶剂萃取丁香精油工艺;分离鉴定冬枣主要致病菌青霉菌和浆胞,并研究丁香精油对青霉菌和浆胞的抑制作用。结果表明:最佳提取工艺为溶剂选用正己烷、萃取温度80℃、颗粒度110目、料液比1∶15(g/mL),丁香精油收率为22.98%;丁香精油对青霉、浆胞的最小抑菌浓度(minimal inhibitory concentration,MIC)为2.0μL/mL和2.5μL/mL,其中活性成分中丁香酚和乙酰基丁香酚完全抑制青霉菌的浓度为350 mg/L和300 mg/L,β-石竹烯对青霉菌没有抑制效应。     

微波法和水蒸气蒸馏法提取丁香精油的研究

以丁香为原料,分别采用微波法和水蒸气蒸馏法提取精油,探讨微波萃取对丁香精油提取率和精油品质的影响。以丁香精油提取率为指标,通过正交试验优化微波提取条件,采用气相色谱-质谱(GC-MS)法鉴定其化学成分,并与水蒸气蒸馏法提取的精油进行比较。结果表明,微波萃取丁香精油的最佳工艺参数为微波功率300 W、料液比1∶4(m∶V)、微波时间25s、提取次数4,该条件下精油的提取率可达到20.65%,远远高于水蒸气蒸馏法的11.33%;从该精油中鉴定出19种成分,其中3种丁香精油有效成分的得率分别为丁香酚13.2%、石竹烯4.4%、乙酰基丁香酚2.2%,石竹烯和乙酰基丁香酚得率分别是水蒸气蒸馏精油的2.8倍和2倍。微波萃取是丁香精油较有效的提取方式。     

艾纳香与马尾松精油的成分分析及抗氧化研究

为了研究艾纳香精油和马尾松精油的生物活性功能,采用水蒸气蒸馏法提取艾纳香精油和马尾松精油,利用气相色谱-质谱联用法(GC-MS)对艾纳香精油和马尾松精油成分进行分析,并用DPPH·、ABTS~+·清除法对艾纳香精油和马尾松精油的体外抗氧化性活性进行研究。结果表明:艾纳香精油中鉴定出38个组分,占总含量的88.20%,其主要成分为龙脑(19.55%)、β-石竹烯(11.19%)、花椒油素(8.08%)、β-石竹烯氧化物(7.08%);马尾松精油中鉴定出59个组分,占总含量的92.43%,其主要成分为β-石竹烯(12.89%)、α-蒎烯(7.26%)、大根香叶烯D (6.85%)和双环大根香叶烯(5.91%)。艾纳香精油和马尾松精油对DPPH·和ABTS~+·均具有清除活性,其中艾纳香精油和马尾松精油清除DPPH·的IC_(50)值分别为1.86mg/mL和17.71mg/mL;清除ABTS~+·的IC_(50)值分别为0.41mg/mL和3.51mg/mL。     

白豆蔻精油超临界CO2萃取工艺优化及挥发性成分分析

以白豆蔻为原料,利用水蒸气蒸馏（SDE）法和超临界流体萃取（SFE）法提取白豆蔻精油。以萃取率为评价指标,采用单因素试验及正交试验优化萃取工艺,并采用气质联用（GC-MS）法分析两种提取方法所得白豆蔻精油的组成。结果表明,最佳萃取工艺条件为：萃取压力25 MPa、萃取温度50 ℃、CO2流量14 mL/min、提取时间4.0 h。在此优化条件下,SFE提取白豆蔻精油得率为6%,为SDE提取精油的1.5倍。GC-MS分析结果表明,共检出挥发性化合物158种,其中SDE和SFE提取精油中分别检出97种、111种,独有化合物分别有47种、61种,共有化合物有50种。两种提取方法所得精油的组成相似,主要成分有桉叶油醇、α-蒎烯、4-异丙基甲苯、顺式十五烯酸、棕榈酸等,但含量差异较大。结果表明SFE是提取白豆蔻精油的有效方法。     

超临界CO2 萃取雪峰蜜橘橘皮精油的中试条件研究

以橘皮为原料,采用超临界CO₂ 萃取技术(SFE)提取雪峰蜜橘橘皮中精油和色素,通过正交试验确定萃取的最佳中试条件,并利用气相色谱- 质谱法(GC-MS)分析最佳中试工艺条件下生产的橘皮精油成分。结果表明：最佳中试提取工艺条件为萃取压力30MPa、萃取时间1h、萃取温度40℃、CO2 流量21.27L/min,此时提取物(色素＋精油)提取率4.56%。其中精油共检测出21 种成分,主要成分为D- 柠檬烯、α- 金合欢烯、白菖油萜、β- 榄香烯、β- 蒎烯等,其中D- 柠檬烯和α- 金合欢烯的总含量达90% 以上。     

超临界萃取结合分子蒸馏纯化生姜精油及其挥发性成分分析

为研究超临界萃取结合分子蒸馏纯化生姜精油的最佳工艺参数,鉴定生姜精油的挥发性成分,以舒城黄姜为原料,通过单因素试验和正交试验优化了超临界CO₂流体萃取(supercritical CO₂ fluid extraction, SFE)生姜油的最佳工艺条件,考察了分子蒸馏(molecular distillation, MD)温度对分离纯化生姜精油效果的影响,并通过气相色谱-质谱联用对生姜精油的挥发性成分进行了分析。结果表明,超临界CO₂流体萃取结合分子蒸馏(SFE-MD)纯化生姜精油的最佳工艺条件为萃取压力24 MPa、萃取温度45℃、萃取时间2 h、分子蒸馏温度80℃,在此条件下,生姜精油的综合得率为2.53%,显著高于水蒸气蒸馏精油得率0.96%(P<0.05)。挥发性成分分析显示,α-姜烯、β-倍半水芹烯、β-红没药烯是生姜精油的主要挥发性成分,百分含量达70%以上,其中α-姜烯百分含量为42.13%,高于水蒸气蒸馏生姜精油α-姜烯百分含量40.59%。该方法绿色环保,萃取率高,精油品质好,为生姜精油的进一步研...     

雪峰蜜桔果皮精油组分与CO2超临界萃取工艺条件的相关性研究

选择萃取压力、萃取时间、萃取温度分别为20MPa、1h、30℃;30MPa、1h、30℃;30MPa、1h、 40℃三组工艺条件,用CO2超临界萃取法(SFE)提取蜜桔果皮精油,将精油和色素进行分离后,用气相色谱-质谱法(GC-MS)对精油成分进行分析.结果表明,采用20MPa、1h、30℃条件提取的精油样品鉴定出22种化学成分,采用30MPa、1.5h、30℃;30MPa、1h、40℃条件提取的样品均鉴定出21种化学成分;同时,精油的化学成分与CO2超临界萃取法的提取条件具有相关性,提高萃取温度可以大大提高精油中β-蒎烯和橙花醇的含量,提高萃取压力可以提高精油中白菖油萜的含量.     

超临界CO2萃取姜挥发油及GC-MS分析

正交试验法时超临界CO2提取生姜挥发油的提取条件进行研究.结果表明,最佳提取条件为:原料粒径为03mm,萃取压力25 MPa,温度40℃,CO2流量30 kg/h,萃取时间100min,所得姜精油呈浅黄色,得率由传统水蒸气蒸馏法的1%左右提高到4.38%.采用气相色谱-质谱联用技术测定最佳提取条件下所得生姜挥发油的化学成分及其相对质量分数,共分离出58种成分并鉴定出其中38种,主体呈香成分为柠檬烯、α-蒎烯、莰烯、金合欢烯、β-水芹烯、β-倍半水芹烯、姜烯等烯类.主体辣味成分为6-姜醇.     

Mal-β-CD对黑胡椒精油的包合作用研究

研究Mal-β-CD对黑胡椒精油的包合作用。以包埋率为指标,以包合温度、包合时间和Mal-β-CD和β-石竹烯的摩尔比为变量,通过正交试验确定最佳包合反应工艺参数是包合温度70℃,包合时间90min,Mal-β-CD和β-石竹烯的摩尔比为1∶1;通过红外扫描和热重分析,确认Mal-β-CD-β-石竹烯包合物的形成,热重分析表明β-石竹烯经Mal-β-CD包埋后,耐热性显著提高;Mal-β-CD包合黑胡椒精油的包合产物稳定性较好,水溶性好,包合物的临界湿度为67%。     

花椒精油亚临界流体萃取工艺优化及GC-MS分析

以甘肃武都大红袍花椒为原料,采用水蒸气蒸馏萃取法（SDE）及亚临界流体萃取法（SFE）提取花椒精油。以花椒精油得率为评价指标,采用单因素试验和正交试验优化SFE萃取工艺,并采用气质联用法（GC-MS）对比分析SDE和SFE花椒精油的香气成分。结果表明,最佳萃取工艺为：萃取3次、萃取温度40 ℃、萃取时间40 min、料液比1.0∶2.0（g∶mL）。在此优化条件下,SFE花椒精油得率为15.11%,为SDE精油得率的3.7倍。GC-MS分析结果表明,共检测出48种挥发性物质,包括烯烃类20种、酯类8种、醇类8种、醛类3种、芳香烃类2种、呋喃类2种、酮类2种、萜类1种、酸类1种和萘类1种。SDE和SFE分别检出37种、40种挥发性物质,两种提取方法所得精油的组成相似,SFE精油得率较SDE高且留香型持久,是提取花椒精油的有效提取方法。     

Flavour compounds of Lavandula angustifolia L. to use in food manufacturing: Comparison of three different extraction methods

Sixty compounds of Lavandula angustifolia L. cultivated in Friuli Venezia Giulia (North-East Italy) were identified and quantified by GC-MS and GC-FID from essential oils obtained by means of hydrodistillation, and from extracts obtained by supercritical CO₂ extraction (SFE) and ultrasound-assisted extraction (US). Using absolute calibration, a true quantification of 1-8 cineol, camphor, linalool, linalyl acetate and β-caryophyllene was carried out. The best extracts, in terms of amount of isolated compounds, flavour quality and stability were those obtained with SFE. Sonication performed at low amplitude for 5 min offered respect to high amplitude a promising alternative to hydrodistillation as a source of lavender flavouring ready to use for alcoholic beverages or/and confectionery products.     

谷糠油成分的超临界CO2流体萃取及GC-MS分析

采用超临界CO2流体萃取法从谷糠中萃取谷糠油,用气相色谱-质谱联用技术对其甲酯化产物进行分析,用归一化法测定其相对百分含量。结果表明：最适宜的萃取工艺条件为萃取压力30MPa,萃取温度45℃,萃取时间70min。谷糠油中共鉴定出18种成分,其中三十六烷占28.42%、2,6-二叔丁基对甲酚占19.6%、油酸甲酯占7.77%、2,4-二叔丁基-6-甲基苯酚占6.06%、亚油酸甲酯占5.16%。     

Comparison of essential oils of clove buds extracted with supercritical carbon dioxide and other three traditional extraction methods

Supercritical fluid extraction (SFE) of essential oil from clove buds with CO₂ was explored. The effect of different parameters, such as temperature (30 °C, 40 °C, 50 °C), pressure(10 MPa, 20 MPa, 30 MPa) and particle size (three degree index), on the extraction yield and the content of eugenol in extracts was investigated using three-level orthogonal array design. The experimental results show that the temperature has the largest effect on the eugenol content of the extracts, and particle size has the maximum effect on the oil yield. The essential oil of 19.56% yield, in which the maximum content of eugenol in extracts is 58.77%, can be extracted from clove buds at pressure of 10 MPa and temperature of 50 °C. Essential oil of clove buds obtained by SFE, hydrodistillation, steam distillation and Soxhlet extraction were further analyzed by gas chromatography/mass spectrometric detection to compare the extraction methods. Twenty three compounds in the clove oils have been identified, showing that the composition of the clove oil extracted by different methods is mostly similar, whereas relative concentration of the identified compounds is apparently different. General characteristics of the clove oils obtained by different methods were further compared, and SFE is considered as the optimum process among the four processes for obtaining clove oil with high quality.     

超临界CO2提取葛缕子精油及其成分分析

目的:优化葛缕子精油的提取工艺并对其成分进行分析。方法:以葛缕子籽粒为原料,采用超临界CO₂技术提取葛缕子精油,并通过气相色谱—质谱(GC-MS)对精油挥发性成分进行分析。结果:超临界CO₂提取葛缕子精油的最佳工艺条件为提取釜温度50℃,分离釜温度40℃,提取釜压力30 MPa,分离釜压力0.4 MPa,二氧化碳流速20 g/min,提取时间90 min,此条件下精油得率为4.79%。与同时蒸馏萃取(SDE)法相比,超临界CO₂流体能快速扩散到样品颗粒内部并充分溶解其中的精油成分,具有提取时间短、得率高、无溶剂残留的优点。超临界CO₂法制备的葛缕子精油中,主要成分为D-柠檬烯(50.96%)和香芹酮(46.65%),挥发性成分种类及含量均高于同时蒸馏萃取法的。结论:超临界CO₂法比同时蒸馏萃取法更适合葛缕子精油的提取。     

气相色谱-质谱法测定卵叶娃儿藤超临界CO2流体萃取物中挥发性成分

采用超临界CO2(SFE)从卵叶娃儿藤中萃取有效成分,萃取条件为:萃取釜压力35MPa,温度50℃,萃取时间3h,夹带剂95%乙醇用量20ml。采用气相色谱-质谱法对其挥发性成分进行鉴定,用归一化法测定各组分的含量。色谱条件:HP-5MS石英毛细管柱(0.25mm×30m×0.25μm),柱温60℃,恒温1min,以4℃/min升至280℃,保持10min;分流进样,分流比20:1。进样口温度250℃。在采用超临界CO2萃取法提取的卵叶娃儿藤提取物中共检出37种成分。     

Comparative Gas Chromatographic–Mass Spectrometric Evaluation of Hop (Humulus lupulus L.) Essential Oils and Extracts Obtained Using Different Sample Preparation Methods

The main aim of investigations was to identify chemotypes and determine differences between some domestic hop varieties and wild hops, which were collected from some regions of Lithuania and cultivated at the same edafoclimatic conditions in hops collection of Kaunas Botanical Garden of Vytautas Magnus University. One of objectives was to compare essential oils of hops (2 years harvest) by the evaluation of volatiles content. Among the main components of hop essential oils monoterpenes (β-myrcene) and sesquiterpenes (α-humulene and β-caryophyllene) were determined using gas chromatography coupled with mass spectrometry (GC-MS). Retention parameters (t _R, calculated retention index, and Kovats retention index) and m/z value of molecular ion for selected compounds from hop essential oils were determined. Samples were prepared by applying solid phase microextraction (SPME), supercritical fluid extraction (SFE) and accelerated solvent extraction (ASE). The steam distillation was used to obtain hop essential oils. The chemometric comparison of domestic and wild hops based on GC-MS analysis data was carried out. The obtained statistical results allow us to classify the investigated wild forms and domestic varieties of hops according to the similarities of their chemotypes. The concentration of β-myrcene, α-humulene in hop essential oils obtained from cones 2 years harvests is much higher than other volatile organic compounds (15.2–23.7 % in total contribution). In analysed essential oils β-farnesene is a constituent in higher quantity of hop essential oils obtained from cones from second time harvest than from cones from first harvest. This can be explained by the year-to-year vegetation conditions difference.