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流体萃取重金属的研究进展

超临界CO2I充体与金属配合技术相结合开辟了重金属萃取的新途径,本文介绍了超临界CO2流体萃取重金属的研究现状,总结了影响萃因素,并对未来的发展趋势作了展望。     

在超临界CO2流体中的化学反应

超临界CO2流体中的化学反应是继超临界流体应用于萃取分离过程之后进一步将其应用于化学反应的新尝试。本文重点综述了超临界CO2流体中的化学反应研究进展, 并对其发展前景作了展望。     

超临界二氧化碳萃取柿叶黄酮的工艺研究

本文研究了超临界流体萃取柿叶总黄酮苷类化合物的影响因素,并对生产工艺进行了优化设计。试验结果表明:萃取时压力、温度、时间、CO2流量对萃取率的影响程度依次递减。最佳工艺条件为:萃取压力30MPa、萃取温度50℃、萃取时间3h、CO2流量30kg·h-1。用超临界流体萃取法得到的柿叶总黄酮苷类化合物萃取物纯度高,无异味,色泽金黄。     

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。     

超临界CO2流体萃取技术在中药有效成分提取中的应用

论述了超临界CO2流体萃取中药有效成分的优越性以及影响萃取效果的因素,并分析了其应用实例。     

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,     

超临界流体萃取-高效液相色谱离线联用分析灵芝中三萜类化合物

在系统考察压力、温度和时间对萃取率影响的基础上,利用超临界流体萃取技术提取了灵芝子实体中的三萜类化合物。其最佳萃取条件为:压力15 MPa,温度35℃,动态萃取时间120 m in,CO2流量1 mL/m in,背压阀温度50℃。此外,还建立了高效液相色谱梯度洗脱分离三萜类化合物的方法。通过比较超临界流体提取物和甲醇提取物的色谱图,发现两者具有相似的峰形,说明超临界流体能够达到与甲醇相近的萃取效果,可以取代甲醇作为新一代的绿色萃取溶剂。     

超临界CO2络合萃取金属离子的研究与应用

本文综述了国内外对超临界CO2络合萃取技术的研究与应用现状.总结并分析了超临界CO2流体萃取金属离子的原理、方法,动力学机理,络合剂和改性剂的选择,络合萃取过程的影响因素,并着重介绍了其在环境保护、核工业、冶金工业、化学分析、中药产业、保健品工业中的应用.最后指出了它目前存在的问题,并对未来研究方向进行了展望.     

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。     

人参中稀有皂苷临界二氧化碳超提取

针对人参稀有皂苷极性较小的特点,选择超临界二氧化碳流体(SFE-CO2)技术进行提取,最佳提取实验条件为:压力35 MPa,温度50 ℃,夹带剂为70%乙醇,夹带剂用量为1.7 mL/g。 利用高效液相色谱 电喷雾质谱联用分析方法分析其萃取产物,证明该提取方法的提取效率与超声提取接近,且该方法具有环境友好的特点。     

SFE-CO2 extract from Typhonium giganteum Engl. tubers, induces apoptosis in human hepatoma SMMC-7721 cells involvement of a ROS-mediated mitochondrial pathway

Typhonium giganteum Engl. (BaiFuzi) is one of the herbs commonly used in traditional Chinese medicine against cancer. In our previous studies, 37 compounds were identified the SFE-CO(2) (supercritical fluid extraction with CO(2)) extract by GC-MS, including the four major components [β-sitosterol (40.22%), campesterol (18.45%), n-hexadecanoic acid (9.52%) and (Z,Z)-9,12-octadecadienoic acid (8.15%)]. The anti-cancer mechanisms of the SFE-CO(2 )extract from T. giganteum Engl. tubers have not been reported as yet. In this paper, the molecular mechanisms of the SFE-CO(2) extract-mediated apoptosis in SMMC-7721 cells were further examined. SFE-CO(2) extract inhibited the growth of SMMC-7721 cells in a time- and dose-dependent manner, arrested the cell cycle in the S phase and G2/M phase, and induced apoptosis. In addition, reactive oxygen species (ROS) increase, reduction of mitochondrial membrane potential, a rise in intracellular calcium levels were found in SMMC-7721 cells after treated with the extract. Western blot analysis showed that the extract caused down-regulation of Bcl-2 expression, and up-regulation of Bax expression. Moreover, caspase-3 and caspase-9 protease activity significantly increased in a dose-dependent manner. Collectively, our results showed that the SFE-CO(2) extract from T. giganteum Engl. tubers induces apoptosis in SMMC-7721 cells involving a ROS-mediated mitochondrial signalling pathway.     

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 fluid CO₂ extraction of Acorus calamus L. (Arales: Araceae) and its contact toxicity to Sitophilus zeamais Motschusky (Coleoptera: Curculionidae)

Contact toxicities of Acorus calamus L. (Arales: Araceae) extracts obtained from four published extraction methods: soakage, soxhlet, ultrasonic and supercritical fluid CO? (SFE-CO?), were compared in this study. Under the given extraction conditions, SFE-CO? extract exhibited the highest contact toxicity against S. zeamais of the four methods. With the SFE-CO? method, extraction temperature, pressure, time and the amount of EtOH (the extraction solvent) were identified as having a significant effect on the extract. Orthogonal experiments showed that the optimal extraction parameters were: temperature--55°C, pressure--35?MPa, time--40?min and EtOH--150?mL per 200?g of dry powder. Under these conditions, the yield was 4.12% and the LD?? of the extract against S. zeamais after 96?h of treatment was 27.26?μg?cm?2. β-asarone was the dominant component of the extract derived from the SFE-CO? method, accounting for 24.39% of the extract. These results may contribute to the designing of large-scale production processes for obtaining A. calamus extract, which proves to be an effective alternative for the control of stored product insect pests.     

HPLC analysis of supercritical carbon dioxide and compressed propane extracts from Piper amalago L. with antileishmanial activity

Piper amalago L. leaves were extracted with supercritical carbon dioxide and compressed propane under different conditions, and with chloroform by the conventional maceration method. These methods were compared for the pyrrolidine alkaloid content. Supercritical carbon dioxide (SFE-CO?) at 313 K and 12.55 MPa showed the highest selectivity for the main compound (600.53 mg/g of extract). A gradient high-performance liquid chromatography (HPLC) method was developed and validated to quantify the alkaloid N-[7-(3',4'-methylenedioxyphenyl)-2(Z),4(Z)-heptadienoyl]pyrrolidine in the extracts. The HPLC method showed linearity, precision and accuracy, allowing the quantitative analysis of the alkaloid in all the samples. All the extracts were tested against the promastigote and intracellular amastigote forms of Leishmania amazonensis. The antileishmanial activity was evaluated in terms of inhibitory concentration for 50% of protozoa (IC??). The cytotoxicity was also evaluated against J774A1 macrophages, and the cytotoxic concentrations for 50% of macrophages were obtained (CC??). The SFE-CO? (313 K; 12.55 MPa) extract showed the highest antileishmanial activity with the following IC?? values of 16 and 7 μg/mL against the promastigotes and intracellular amastigotes forms, respectively. The extract showed low cytotoxicity with a CC?? value of 93 μg/mL.     

Supercritical fluid extraction of 2,4-D from soils using derivatization and ionic modifiers

Supercritical fluid extraction (SFE) with CO(2), a clean and rapid alternative to conventional organic solvent extraction techniques, was investigated for the extraction of 2,4-D from soils using a variety of pre-extraction soil treatments to enhance extraction recoveries. Initial experiments with silylation, ion-pairing, methyl esterification, and ionic displacement are reported. Methyl esterification and ionic displacement during SFE proved to be the most promising approaches for quantitative extraction. Although the SFE procedures were not fully optimized, comparison between SFE and a standard Soxhlet extraction method demonstrated the potential for improving analytical measurement for highly polar pesticides in soil by modifying SFE-CO(2) extraction with derivatizing reagents and ionic solutions.     

Extraction of Lepidium apetalum seed oil using supercritical carbon dioxide and anti-oxidant activity of the extracted oil

The supercritical fluid extraction (SFE) of Lepidium apetalum seed oil and its anti-oxidant activity were studied. The SFE process was optimized using response surface methodology (RSM) with a central composite design (CCD). Independent variables, namely operating pressure, temperature, time and flow rate were evaluated. The maximum extraction of Lepidium apetalum seed oil by SFE-CO? (about 36.3%) was obtained when SFE-CO? extraction was carried out under the optimal conditions of 30.0 MPa of pressure, 70 °C of temperature, 120 min of extraction time and 25.95 L/h of flow rate. GC-MS analysis showed the presence of four fatty acids in Lepidium apetalum seed oil, with a high content (91.0%) of unsaturated fatty acid. The anti-oxidant activity of the oil was assessed by the 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical-scavenging assay and 2,2'-azino- bis(3-ethylbenzthiazoline-6-sulphonic acid) diammonium salt (ABTS) test. Lepidium apetalum seed oil possessed a notable concentration-dependent antioxidant activity, with IC?? values of 1.00 and 3.75 mg/mL, respectively.     

The Bonding Nature of the Canonical Molecular Orbitals in Simple Diatomic Molecules

The bonding nature of the canonical molecular orbitals 2σg, 2σu and 3σg in the molecules N₂,O₂, F₂ and the related analogous molecular orbitals in the molecules P₂ and CO, is analysed using Weinhold's natural bond orbital set. When the canonical molecular orbitals can be well localized into natural bond orbitals, the covalent bond can be completely attributed to the bonding type natural bond orbitals. The decomposition of canonical molecular orbitals into the natural bond orbital basis then gives the weighted bond order as the component of the bonding portion in the canonical molecular orbital. The weighted bond order results match the photoelectron spectroscopy assignment quite satisfactorily.     

Experimental determination and prediction of the compressibility factor of high CO_2 content natural gas with and without water vapor

In order to study the effect of different CO2 contents on gas compressibility factor(Z-factor),the JEFRI-PVT apparatus has been used to measure the Z-factor of dry natural gas with CO2 content range from 10.74 to 70.42 mol%at the temperature range from 301.2 to 407.3 K and pressure range from 7 to 44 MPa.The results show that Z-factor decreases with increasing CO2 content in natural gas at constant temperature and increases with increasing temperature for natural gas with the same CO2 content.In addition,the Z-factor of water-saturated natural gas with high CO2 content has been measured.A comparison of the Z-factor between natural gas with and without saturated water vapor indicates that the former shows a higher Z-factor than the latter.Furthermore,Peng-Robinson,Hall-Yarborough,and Soave-Benedict-Webb- Rubin equations of state(EoS)are used for the calculation of Z-factor of high CO2 content natural gas with and without water vapor.The optimal binary interaction parameters(BIP)for PR EoS are presented.The measured Z-factor is compared with the calculated Z-factor based on three models,which shows that PR EoS combined with van der Waals mixing rule for gas without water and Huron-Vidal mixing rule for water-saturated gas,are in good agreement with the experimental data.     

基于金属氧化物脱硫剂的天然气深度脱硫

确立了基于GC-MS和GC-SCD的天然气中超微量硫化物定性定量分析方法与条件,并分析了北京城市天然气中的硫化物。结果表明,天然气中含有三种硫化物,主要成分为四氢噻吩(THT),占总硫的94.2%。采用共沉淀法制备了ZnO/Al₂O₃脱硫剂,采用浸渍法制备了ZnO/γ-Al₂O₃、CuO/γ-Al₂O₃和CuO-ZnO/γ-Al₂O₃脱硫剂,并进行了天然气中THT深度脱除的实验研究。结果表明, 采用浸渍法制备的CuO/γ-Al₂O₃和CuO-ZnO/γ-Al₂O₃脱硫剂同时具有良好的低温活性和高温活性,可在50~500℃的宽温下将THT脱除至物质的量分数10×10^-9以下,从而能够满足以天然气为燃料的分布式质子交换膜燃料电池电站对脱硫深度和脱硫温宽的要求。