茵陈挥发油的超临界CO2萃取法与水蒸气蒸馏法提取的比较

采用超临界CO2萃取法与水蒸气蒸馏法从菌陈中提取挥发油，用GC－MS法测定其化学成分和相对含量，对两种提取方法所得的挥发油进行比较，水蒸气蒸馏法提取菌陈挥发油的产率为0．03％（w），主要成分为匙叶桉油烯醇、吉玛烯D、反式－石竹烯、2，4－戊二炔苯、β－金石欢烯等；超临界CO2萃取法提取的产率为0．15％(w)，主要成分为百里酚、β－红没药烯、2－异丙基－4－甲基－1－甲氧基苯、异百里酚、2－特丁基－4－（2，4，4－三甲基戊基）苯酚、β－杜松烯等。     

超临界CO2流体萃取法与水蒸气蒸馏法提取荆芥穗挥发油化学成分的研究

采用超临界CO2萃取法(SFE)与水蒸气蒸馏法(SD)从荆芥穗中提取挥发油。采用SE-54毛细管柱进行分析,用气相色谱-质谱法对挥发油中各种化学成分进行鉴定,用归一化法测定各组分的含量。色谱条件:SE-54毛细管柱 (30 m×0.25 mm i.d.,0.25 μm),柱温50 ℃(3 min)5 ℃/min180 ℃(2 min)10 ℃/min260 ℃(50 min);分流进样,分流比1∶50;进样口温度280 ℃。在采用超临界CO2萃取法提取的挥发油中共鉴定出54种成分,其主要成分为长叶薄荷酮、薄荷酮、亚油酸氯化物等;在水蒸气蒸馏法提取的挥发油中共鉴定出39种成分,其主要成分为长叶薄荷酮、薄荷酮、柠檬烯等。超临界法较水蒸气法更加稳定可靠,重现性好,适用于中药挥发油的化学成分分析。     

超临界CO2萃取与水蒸气蒸馏法研究泽兰中挥发性有机物

以超临界CO2萃取法(SFE)提取中药泽兰中的挥发性有机物,经气相色谱-质谱联用(GC-MS)分析,人工解析质谱图及计算机谱库检索相结合进行化学成分结构鉴定,用面积归一化法计算各组分的相对含量。SFE法提取的产率为0.78%,共鉴定75种挥发性化合物,主要成分为植醇、石竹烯氧化物、十六酸、亚油酸、葎草烯等,比文献报道的该挥发油成分多且含量差异较大,其中松香芹醇、蒲勒烯、马鞭烯酮、香芹酮、十六酸、亚油酸、葎草烯、十六酸乙酯、亚麻酸等多种成分未见报道。与水蒸气蒸馏法(SD)提取的泽兰挥发油进行比较,后者提取的产率为0.12%,从中鉴定出50种化合物,主要成分为石竹烯氧化物、柠檬烯、α-蒎烯、葎草烯、月桂烯等。SFE与SD得到的成分仅有31种相同,其它各不相同。     

水蒸气蒸馏法与超临界CO2萃取法结合气相色谱-质谱分析胡椒木精油成分

以水蒸气蒸馏(SD)法和超临界CO_2萃取(SC-CO_2)法分别提取胡椒木叶片精油,经气相色谱-质谱(GC-MS)分析其组分差异,并通过DPPH·自由基清除能力和还原力测定对提取液品质进行判断。结果表明:SD法和SC-CO_2法获得的主要成分为脂类和烯烃类物质,且组分数量同为34种,但两种方法获得的化学成分有所不同。SD法中相对含量较高的为苯乙烯(43. 15%)、顺式肉桂酸甲酯(30. 33%)、α-石竹烯(1. 81%)、α-月桂烯(8. 41%)等;而SC-CO_2法获得相对含量较高的物质为顺式肉桂酸甲酯(73. 91%)、柠檬烯(11. 13%)、α-石竹烯(4. 12%)等。抗氧化试验表明,SC-CO_2法提取精油清除DPPH·自由基能力在8 mg/mL达到2,6-二叔丁基-4-甲基苯酚(BHT)抑制率的97. 27%,IC_(50)为3. 173 3,还原力在20 mg/mL达到Vc的34. 86%; SD法在20 mg/mL的抑制率仅为BHT的14. 27%,还原力在20 mg/mL时仅为Vc的5. 98%。两种提取方法的分析结果显示,不同提取工艺的选择对获得胡椒木精油中活性成分存在明显差异,差异主要为酚类、萜类等还原性和抗氧化性较强的物质,且SC-CO_2法获得的胡椒木精油中含有较多的驱虫抗菌活性物质,提取效果优于SD法。     

超临界CO_2萃取-分子蒸馏对白术挥发油的提取分离和GC-MS分析

用超临界CO2萃取技术提取白术挥发油，然后用分子蒸馏对所得的萃取物进行精分离，得到蒸出物；超临界萃取物收率为2．42％(w)，分子蒸馏蒸出物收率26．3％(w)；对超临界萃取物和分子蒸馏蒸出物分别进行GC—MS分析，结果超临界萃取物检测出33个化合物，分子蒸馏蒸出物检测出27个化合物，主要成分均为2，7-二甲氧基-3，6-二甲基萘、γ-芹子烯、大根香叶烯等，但相对含量有区别。     

薤白挥发油成分的超临界CO2萃取及GC-MS分析

采取超临界CO2萃取和水蒸气蒸馏两种方法提取薤白中的挥发油,比较了两种提取方法得到的挥发油的理化性质,并利用GC-MS对它们进行了定性、定量分析。两种方法的主要提取物均为含硫化合物,但超临界CO2萃取法得到的含硫化合物的数量和质量都高于水蒸气蒸馏法得到的提取物。采用水蒸气蒸馏法提取8 h得到的萃取率为1.72%。通过设计的超临界CO2萃取的正交实验,得到了最佳萃取工艺条件为:压力25 MPa,温度40℃,CO2流量为25L/h。最佳萃取时间为120 min,萃取率为4.41%,是水蒸气蒸馏法萃取率的2.8倍。实验结果表明,超临界CO2萃取法简单易行,可以较快速、有效地提取薤白中的挥发油。     

超临界CO2流体萃取辛夷精油的组分分析

采用超临界CO2流体萃取辛夷精油,萃取率为3．8％,比水蒸气蒸馏的萃取率高58％。利用气相色谱-质谱联用(GC-MC)法对辛夷精油进行组分的定性和定量分析,并与水蒸气蒸馏法所得辛夷精油的组分相比较,发现超临界CO2流体萃取所得辛夷精油的香气、品质、产率优于水蒸气蒸馏法所得辛夷精油。     

顶空-固相微萃取法与水蒸气蒸馏法提取沙棘挥发油组分的比较研究

优化了顶空-固相微萃取法(HS-SPME)提取沙棘挥发性成分的条件,并采用气相色谱-质谱联用技术(GC-MS)分别对HS-SPME法和水蒸气蒸馏法(SD)的提取物进行分析。结果显示,在萃取温度为70℃,萃取时间为50 min,解吸时间为7 min,平衡时间为20 min条件下,HS-SPME法鉴定出76种组分,占挥发性物质总量的90.19%,主要成分为酯类、醛类和酮类;而SD法提取物共鉴定出56种组分,占挥发性物质总量的91.98%,主要成分为酯类。2种方法共有组分为20种。两种方法提取的沙棘挥发油组分的种类及含量差异较大,HS-SPME法更适合沙棘挥发性组分的快速检测。     

栀子花挥发油超临界CO2萃取工艺优选分析

采用超临界CO2萃取法,使用正交试验设计方案,以提取率为指标,对萃取温度、萃取压力、分离压力和分离温度等影响因素进行考察。结果表明,超临界CO2萃取法萃取栀子花挥发油成分的最佳工艺条件为：萃取压力15mPa,萃取温度35℃,分离压力15mPa,分离温度25℃。该方法简便、可靠、选择性高,适于工业化生产。     

超临界流体萃取技术在提取中药挥发油中的应用

用超监介CO2流体萃取技术对多种中药挥发油的提取进行了综述,并将其与传统的水蒸馏法进行比较。结果表明,用超临界流体法不仅挥发油的收率高,而且提取时间也大大缩短。     

Rapid Extraction and Analysis of Essential Oil from Cinnamomum Cassia Presl.

An improved solvent-free microwave extraction（ISFME） was used for the extraction of essential oil from dried Cinnamomum cassia Presl. Two kinds of solid microwave absorption media[carbonyl iron powder（CIP） and graphite powder（GP）] were used. When ISFME was applied, the heating rate was enhanced and the extraction time was obviously shorter than that consumed in conventional solvent-free microwave extraction（CSFME）. Twenty-eight kinds of compounds in the essential oil were identified, and the total content fractions of the compounds obtained by CIP-ISFME, GP-ISFME, CSFME, and hydrodistillation（HD） were 96.65%, 96.06%, 97.22%, and 96.29%, respectively. The compounds in the essential oil obtained from Cinnamomum cassia Presl. by ISFME, CSFME, and HD were compared and the quantity of the essential oil was almost the same. The ISFME has been proved to be a feasible way to extract essential oil from dried samples, and there are several obvious advantages in ISFME over those of HD and CSFME, for example, shorter extraction time（30 min） and lower energy consumption.     

Comparison of Constituents and Insecticidal Activities of Essential Oil from Artemisia lavandulaefolia by Steam Distillation and Supercritical-CO2 Fluid Extraction

Essential oil was extracted from Artemisia lavandulaefolia DC.by steam distillation(SD) and supercritical-CO2 fluid extraction(SFE),respectively.The constituents of the essentil oils extracted with those two methods were analyzed by gas chromatography-mass spectrometry(GC-MS) and insecticidal activities of the essential oils were evaluated,then the results were compared to assess their biological activity.Thirty-one compounds were identified in the essential oil extracted by SD,and its main components were eucalyptol,α,α,4-trimethyl-3-cyclohexene-1-methanol and so on.Twenty-two compounds were identified for the essential oil extracted by SFE,and its main components were cyclodecene,n-hexadecanoic acid and so on.Six chemical compositions were all contained in the essential oils extracted by the two methods,i.e.,eucalyptol,α,α,4-trimethyl-3-cyclohexene-1-methanol,caryophyllene,[3aS-(3aα,3bβ,4β,7α,7aS)]-octahydro-7-methyl-3-methylene-4-(1-methylethyl)-1H-cyclopenta[1,3]cyclopropa-[1,2]benzene,nerolidol and(-)-Spathulenol.The fumigation toxicity of the essential oil obtained by means of SD to the adults of Sitophilus zeamais is significantly higher than that of the essential oil by means of SFE.The contact toxicity of the essential oil obtained by means of SFE to the adults of S.zeamais is higher than that of the essential oil obtained by means of SD,but the difference is not significant.     

微波辅助提取-气相色谱质谱联用测定肉桂中的挥发油

利用非极性溶剂微波辅助提取(NPSMAE)-气相色谱质谱联用研究了肉桂中的挥发油成分, 并测定了挥发油中的主要成分肉桂醛(Cinnamaldehyde)的含量. 考察了NPSMAE提取溶剂的种类、提取温度、提取时间及固液比等对测定的影响, 同时将NPSMAE与超声波辅助提取(UAE)及水蒸气蒸馏(HD)等方法进行了比较. 结果表明, 与常规提取方法相比, NPSMAE具有提取时间短、提取产率高等优点, 是一种实用的中药挥发油提取方法.     

白术挥发性成分的超临界流体萃取及其分析

采用超临界流体萃取白术挥发油成分,对萃取条件进行优化,并用气相色谱、气相色谱－质谱分析鉴定出超临界流体萃了的挥发油中22个化合物。最佳的超临界流体萃取条件为压力22.0MPa,温度60℃,0.5mL乙醇作改性,先静态萃取10min(CO2用量2.0mL),再动态萃取40min(CO2流速为0.3mL/min)。将超临界流体萃取与水蒸气蒸馏进行对比,水蒸气蒸馏5h的油收率仅为超临界流体萃取1h油收率的10.32%,证明超临界流体萃取替代传统萃取的必要性。     

超临界CO_2萃取连翘挥发油的正交试验和GC-MS分析

采用正交试验法对超临界CO2萃取连翘挥发油的条件进行了研究；结果显示最佳萃取条件为萃取压力30MPa，萃取温度35℃，解析压力6．7MPa，解析温度50℃，粉碎度0．55mm；按对结果的影响大小依次排列为萃取温度，粉碎度，萃取压力，解析压力，解析温度；用气相色谱－质谱联用技术测定了最佳萃取条件所得连翘挥发油的化学成分，从中鉴定出21种成分，并测定了其相对含量，主要成分为α－蒎烯、β－蒎烯、萜品醇－4、α－萜品醇、苯甲醇等。     

Rapid Extraction of Essential Oil from Dried Cinnamomum cassia Presl and Forsythia suspensa(Thunb.)Vahl by Ionic Liquid Microwave Extraction

Ionic liquid (IL) was used as the microwave absorption medium to extract essential oils from dried Cinnamomum cassia Presl and Forsythia suspensa (Thunb.) Vahl, and the ionic liquid microwave extraction (ILME) was developed. Some experimental parameters for ILME were examined. The proposed method was compared with other methods, including hydrodistillation (HD), microwave hydrodistillation (MHD), solvent‐free microwave extraction (SFME) and improved solvent‐free microwave extraction (ISFME). Experimental results showed that compared with other extraction methods the ILME had some advantages, such as time‐saving, simplicity and usage of green solvents. The extraction time was less than 18 min at the microwave power of 440 W and 1.5 mL of ionic liquid was required. The constituents of essential oils obtained by the five methods are not obviously different.     

超临界CO_2萃取-分子蒸馏对大蒜化学成分的提取与分离

采用超临界CO2流体萃取技术和分子蒸馏对大蒜化学成分进行萃取与分离，用气相色谱－质谱联用技术测定其化学成分；从超临界CO2萃取物中鉴定出16种成分，经分子蒸馏后，得到4种主要成分：二烯丙基二硫、3－乙烯基－1，2－二硫代环己－5－烯、2－乙烯基－1，3－二硫代环己－5－烯及二烯丙基三硫。