若干芳香化湿类及理气类中药的超临界二氧化碳萃取研究

对苍术、砂仁、香附等若干芳香化湿类及理气类中药进行了超临界CO2 萃取 ,并对其中部分萃取产物的组成进行了GC和GC -MS分析。结果显示 ,超临界CO2 萃取产物的质量与出油率较传统水蒸气蒸馏产物均有较大改善和提高     

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。     

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。     

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CO2萃取柚子叶挥发油的研究及GC-MS分析

采用超临界CO2萃取技术提取柚子叶的挥发性成分,以挥发油得率为衡量工艺参数的指标,通过正交试验法考察超临界CO2萃取过程中萃取温度、萃取压力、CO2的流量及萃取时间4个因素对柚子叶挥发油得率的影响。结果表明20MPa、萃取温度45℃、CO2流量7kg·h-1、萃取时间120min为最佳工艺。通过GC-MS对挥发油进行分析,从柚子叶挥发油中分离出144个组分,鉴定了61种成分,占化合物检出总量的90.4%。     

小茴香超临界CO_2萃取产物脂肪酸成分分析

通过脂肪酸的衍生化处理，再利用色谱（GC）和色谱一质谱（GC－MS）等分析手段，对小茴香超临界CO2萃取产物的脂肪酸成分进行了剖析，共鉴定出九种脂肪酸，其中，十八碳一烯酸、十八碳二烯酸和棕榈酸是其主要成分，分别占脂肪酸总量的75．12％、15．18％和5．34％．     

Zr-Mn-K催化剂超临界相合成甲醇与异丁醇的研究

用共沉淀法和超临界流体干燥法,分别制备了Ｚｒ－Ｍｎ－Ｋ沉淀型催化剂和超细催化剂．以正十一～十三烷的混合物为超临界介质,在反应温度３６０～４１０℃、合成气压力７．５ＭＰａ、ＧＨＳＶ１７００ｈ－１及介质压力２．０８ＭＰａ的实验条件下,分别考察了超细催化剂和沉淀催化剂的气相和超临界相催化合成气制甲醇、异丁醇的性能．气相和超临界相反应的研究均表明,超细催化剂催化合成异丁醇的活性高于沉淀催化剂;在超临界条件下反应,超细催化剂上产物的异丁醇含量较高（为２３％～３２％）,甲醇含量为２２％～３３％,其它醇均在１０％左右．气相与超临界相反应结果的对比显示,超临界流体促进产物的脱附与传递,提高了ＣＯ的转化率．但超临界流体对甲烷的萃取作用强于对醇的萃取,醇选择性低于气相反应．在超临界条件下合成甲醇、异丁醇仍遵循异丁醇形成的链增长机理,超临界流体改变了链增长各步骤的相对速度,致使超临界相反应的产物分布不同于气相反应的产物分布．     

超临界流体色谱分析番茄红素

以超临界CO2作为流动相，在压力15.0-20.0MPa，温度25－50℃，携带剂乙醇或正己烷的浓度分别为0－30％和0－20％的范围内考察了番茄红素及其氧化产物在C18色谱柱上的保留值的变化规律，确定了最佳的分离条件。对超临界丙烷萃取的番茄红素原料、萃取产物及萃余物进行了定量分析，考察了重复性及平行性。结果表明：在优化条件下，番茄红素的保留时间在3min以内，定量结果的重复性与平行性好。     

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。     

一种新型超临界流体萃取-高效液相色谱在线联用系统的构建

天然产物研究一直是植物学、化学和药学的重要研究领域．通过从天然产物中寻找生物活性成分和先导物是创制新药的有效途径之一．有效成分的提取是天然产物研究中最基本和最关键的环节．超临界流体萃取（Supercritical fluid extraction,简称SFE）是近年来发展较快的一种新型样品提取技术．超临界CO2作为最常用的萃取剂已被用于天然药物中非极性和弱极性有效成分的提取,尤其是挥发性和热敏性的物质．此外,通过加入适当的添加剂还可有效地萃取极性化合物,和传统的化学方法相比,     

溶剂抽提、水蒸气蒸馏和超临界萃取用于古蓬香脂组成分析方法的比较(英文)

 采用乙醇和丙酮溶剂抽提、ＣＯ２超临界萃取（ＳＦＥ）以及水蒸气蒸馏（ＳＤ）的方法提取古蓬香脂乳胶。对乙醇和丙酮提取物进行了ＨＰＬＣ和ＧＣ－ＭＳ分析。两个提取物的ＨＰＬＣ谱图十分相似，总共可分离出１７个组分。而乙醇提取物的ＧＣ－ＭＳ分析鉴定表明有２１个组分。ＳＦＥ提取物的ＧＣ－ＭＳ分析得到８个组分。ＳＤ提取物有１４个组分。在超临界流体中加入甲醇无论对提取物的组分数还是对其浓度都没有什么影响。     

Comparison of solid-phase microextraction, supercritical fluid extraction, steam distillation, and solvent extraction techniques for analysis of volatile consituents in Fructus Amomi

Four sampling techniques, solid-phase microextraction (SPME), supercritical fluid extraction (SFE), steam distillation (SD), and solvent extraction (SE), were compared for the analysis of volatile constituents from a traditional Chinese medicine (TCM) of the dried ripe fruit of Fructus Amomi (Sha Ren). A total of 38 compounds were identified by gas chromatography/mass spectrometry. Different SFE and SPME parameters (modifier content, extraction pressure, and temperature for SFE and fibers, extraction temperature, and time for SPME) were studied. The results by SFE and SPME were compared with those obtained by conventional SD and SE methods. The results showed that SFE and SPME are better sample preparation techniques than SD and SE. Due to SFE's requirement for expensive specialized instrumentation, the simplicity, low cost, and speed of SPME make it a more appropriate technique for extraction of volatile constituents in TCMs.     

川芎水蒸气蒸馏和超临界CO2提取物化学成分的GC-MS分析鉴别

用水蒸气蒸馏和超临界CO2提取方法对川芎药材中的化学成分进行提取,用气相色谱-质谱联用技术(GC-MS)对提取物进行分析,分别鉴定出30和34个化合物,测定了其相对含量。 结果表明,水蒸气蒸馏和超临界CO2提取物的主要成分均为(Z)-藁本内酯。 超临界CO2提取方法能提取出较多的川芎药效物质,如丁基酞内酯、丁烯基酞内酯、川芎内酯A、(Z)-藁本内酯、(E)-藁本内酯和川芎内酯I。 而水蒸气蒸馏提取物中除了川芎药效物质外,还含有较多的萜烯类化合物。 结果表明,超临界CO2对川芎药效物质的提取比水蒸气蒸馏法的效率高。 通过对川芎中带不饱和侧链与饱和侧链内酯类化合物质谱裂解规律的解析归纳,鉴别了川芎中不饱和侧链内酯类化合物如(Z)-藁本内酯、(E)-藁本内酯、丁烯基酞内酯和川芎内酯I以及饱和侧链内酯类化合物如丁基酞内酯和川芎内酯A。     

黄荆子挥发性成分的分析

分别采用水蒸汽蒸馏法和超临界流体CO2萃取法提取黄荆子中的挥发性成分.利用气相色谱-质谱(GC/MS)联用技术对其化学成分进行了分析鉴定,并通过面积归一法测定了各成分的相对含量.对两种提取方法的结果进行了比较.结果表明,子午岭的黄荆子中含有多种药用成分,而超临界流体CO2萃取法更能有效地提取黄荆子中的有效成分.     

Supercritical extraction of thyme (Thymus vulgaris L.)

Summary Chromatographic methods for the qualitative and quantitative analysis of thyme (Thymus vulgaris L.) extracts (essential oil obtained by steam distillation and extracts obtained by carbon dioxide supercritical fluid extraction and methylene chloride) are described. The composition of extracts obtained at different pressures (from 80 bar to 400 bar) and constant temperature (40°C) is discussed. The extraction system thyme— supercritical carbon dioxide was modelled by empirical equations defining the dependence of the total extract (TE) solubility and thymol solubility in CO₂ on the density of carbon dioxide.     

Superheated water extraction, steam distillation and SFE of peppermint oil

Superheated water extraction, steam distillation and supercritical fluid extraction (SFE) are compared for extraction of l-menthol, menthone, eucalyptol and other components of peppermint (mentha piperita) leaves. Different temperatures and pressures were investigated. SFE results at 25/40?°C and 6.5/8/10 MPa were comparable with those reported in the literature. Although SFE is a gentle way of extracting thermally unstable compounds, this method is too slow for commercial use in comparison with steam distillation at 100?°C. Superheated water extraction at 125/150?°C and 1–2 MPa exhibits higher extraction efficiency than the SFE method. Comparison of all experiments under the chosen conditions shows steam distillation to be the most effective extraction method.     

Superheated water extraction, steam distillation and SFE of peppermint oil

Superheated water extraction, steam distillation and supercritical fluid extraction (SFE) are compared for extraction of l-menthol, menthone, eucalyptol and other components of peppermint (mentha piperita) leaves. Different temperatures and pressures were investigated. SFE results at 25/40 °C and 6.5/8/10 MPa were comparable with those reported in the literature. Although SFE is a gentle way of extracting thermally unstable compounds, this method is too slow for commercial use in comparison with steam distillation at 100 °C. Superheated water extraction at 125/150 °C and 1–2 MPa exhibits higher extraction efficiency than the SFE method. Comparison of all experiments under the chosen conditions shows steam distillation to be the most effective extraction method. Received: 18 January 1998 / Revised: 9 April 1999 / Accepted: 15 April 1999     

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。     

Parameters optimization of supercritical fluid‐CO2 extracts of frankincense using response surface methodology and its pharmacodynamics effects

The volatile oil parts of frankincense (Boswellia carterii Birdw.) were extracted with supercritical carbon dioxide under constant pressure (15, 20, or 25 MPa) and fixed temperature (40, 50, or 60°C), given time (60, 90, or 120 min) aiming at the acquisition of enriched fractions containing octyl acetate, compounds of pharmaceutical interest. A mathematical model was created by Box‐Behnken design, a popular template for response surface methodology, for the extraction process. The response value was characterized by synthetical score, which comprised yields accounting for 20% and content of octyl acetate for 80%. The content of octyl acetate was determined by GC. The supercritical fluid extraction showed higher selectivity than conventional steam distillation. Supercritical fluid‐CO₂ for extracting frankincense under optimum condition was of great validity, which was also successfully verified by the pharmacological experiments.