金属离子的超临界流体萃取技术的进展

超临界流体萃取技术在分离方面发展迅速,应用前景十分广泛。文中综述了超临界流体技术的萃取机理及对金属离子萃取的研究。     

超临界萃取装置的研制及其应用

超临界流体萃取是近的上来兴起的一种新的分离技术，报道了将超临界萃取原理与回流技术相结合研制的二氧化碳回流中低压超临界流体萃取设备，解决了关键实验手段，通过应用证明设备可靠，费用低廉，有实用价值。     

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。     

超临界流体技术在萃取中的应用简介

超临界流体萃取技术具有许多传统技术所没有的快速、高效、高选择性、低能耗等优点,特别是超临界流体的特性是它可以代替高毒有机溶剂做反应介质,符合绿色化学的要求。本文综述了超临界流体的特性,介绍了超临界流体萃取的原理,归纳了超临界流体萃取的应用现状,并介绍了超临界流体的其他领域应用概况。     

自制超临界流体萃取仪操作条件的优化及其应用

超临界流体萃取是近年来发展起来的一种新的分离技术。本文使用自己研制的超临界流体萃取仪对吸附有痕量正构烷烃的Ａｌ２Ｏ３进行萃取，对各种操作条件进行优化。并对卢柑皮及生姜样品进行初步的萃取分析。结果证明该仪器设计合理，具有操作简便、高效、自动化程度高的优点，为复杂样品中痕量组分的萃取分析奠定了基础。     

超临界流体萃取在天然药物分析中的应用

按物质的不同性质综述了１９９５年以来超临界流体萃取技术在天然药物分析中的一些进展情况,常见的分析主要包括萜类、生物碱、黄酮类、挥发油及苯丙素类。超临界流体萃取作为一门新型的样品前处理技术,在天然药物的分离分析中展示了其特有的优点。该技术操作温度低,不会引起热敏性的分解变质;使用的有毒溶剂少,从而减少化学药品对药物的污染。     

超临界流体萃取中草药的研究进展

综述了近二十年来超临界流体萃取技术在中草药提取与分离中的研究现状 ,并展望了其应用前景     

衍生-超临界流体萃取金属离子的技术与进展

综述了近年来衍生-超临界流体萃取环境样品和环境模拟样品中金属离子的研究报道,结合作者的研究工作,着重评述了超临界流体萃取不同环境样品、环境模拟样品中金属离子的原理、萃取过程的动力学模型、衍生剂的选择原则、金属螫合物在超临界流体中的溶解度理论、影响萃取效率的因素、金属离子超临界流体萃取应用研究现状与进展等。利用流体与基体改性技术实现了金属离子和金属螯合物的超临界流体萃取,且在萃取体系中加入适量的表面活性剂能显著提高萃取效率。     

天然香料的超临界CO_2流体萃取

对天然产品的需求导致人们对超临界CO2流体萃取的极大兴趣。本文综述了超临界CO2流体萃取在天然香料中的研究和应用进展并讨论了它与传统分离方法相比较时的优点。     

Extraction and isolation of diphenylheptanes and flavonoids from Alpinia officinarum Hance using supercritical fluid extraction followed by supercritical fluid chromatography

In this paper, an off-line combination method of supercritical fluid extraction and supercritical fluid chromatography was developed for the selective extraction and isolation of diphenylheptanes and flavonoids from Alpinia officinarum Hance. The enrichment of target components was successfully achieved using supercritical fluid extraction with the following conditions (8% ethanol as co-solvent at 45°C and 30 MPa for 30 min). Taking full advantage of the complementarity of supercritical fluid chromatography stationary phases, a two-step preparative supercritical fluid chromatography strategy was constructed. The extract was firstly divided into seven fractions on a Diol column (250 × 20 mm internal diameter, 10 μm) within 8 min by gradient elution increasing from 5% to 20% modifier (methanol) at 55 ml/min and 15 MPa. Then the seven fractions were separated by using a 1-AA or a DEA column (250 × 19 mm internal diameter, 5 μm) at 50 ml/min and 13.5 MPa. This two-step strategy showed superior separation ability for structural analogs. As a result, seven compounds, including four diphenylheptanes and three flavonoids with high purity, were successfully obtained. The developed method is also helpful for the extraction and isolation of other structural analogs of traditional Chinese medicines.     

Trends in techniques for the extraction of drugs and pesticides from biological specimens prior to chromatographic separation and detection

The isolation of non-volatile organic poisons from biological specimens is often difficult and time consuming. This paper surveys the isolation of common drugs and pesticides from biological specimens, including serum, blood and tissue, and the effect of experimental variables on the recovery of compounds, with emphasis on recent trends in extraction techniques and new methods under development, particularly those applicable to forensic toxicology. Traditional liquid-liquid extraction techniques are increasingly being replaced by or used in combination with newer extraction techniques such as solid-phase and supercritical fluid extraction. The potential advantages and problems encountered when incorporating these new methodologies in the isolation of drugs and pesticides from biological matrices are discussed. Although early implementation of solid-phase extraction techniques in forensic toxicology has been hampered by a variety of problems, including extract quality, reproducibility and selectivity, improvements in sorbent quality and elution solvents continue to facilitate their replacement of traditional liquid-liquid extraction methods. Future developments in supercritical fluid extraction should allow this technique to develop in an extremely powerful quantitative tool for the isolation of drugs and pesticides either from solid-phase sorbents or from their endogenous matrices.     

Solid-phase extraction with supercritical fluid elution as a sample preparation technique for the ultratrace analysis of flavone in blood plasma.

A new sample preparation technique, solid-phase extraction with supercritical fluid elution, was developed for the selective isolation of ultratrace levels of drugs from plasma. Plasma samples spiked with a drug were applied to octadecylsilane cartridges and the cartridges were then washed, briefly dried and directly fitted into cells for subsequent supercritical fluid elution. The absolute recovery was studied by using a radiolabeled model compound. The extraction selectivity was examined by chromatographing the extracts with a reversed-phase high-performance liquid chromatographic method with ultraviolet detection. The effects of extraction pressure and the length of capillary restrictors on drug recovery were examined in order to determine the optimal conditions for supercritical fluid elution. The performance of the method was compared to that of conventional solid-phase extraction in terms of recovery, selectivity, precision and accuracy of analysis. Flavone was used as the model compound and dog plasma as the biological matrix for these studies.     

超临界流体萃取分离离子液体与有机物及其相平衡的研究

离子液体具有一些优良的物理和化学性质,非常有希望成为传统有机溶剂的替代溶剂.但是如何从过程物流中分离和回收离子液体将是其工业化应用的一个很大挑战.蒸馏、液液萃取和超临界萃取是目前已知的三个可行的方法.其中超临界萃取可应用于离子液体与挥发的或相对不挥发的有机物的分离,而且不存在相间交叉污染.本文从二元体系相平衡、三元体系相平衡、模型化研究和萃取实验结果方面介绍了超临界萃取方法的最新研究进展,在此基础上提出了用超临界丙烷替代超临界二氧化碳作为萃取溶剂的新思路,并探讨了该领域今后的研究方向和工业化前景.     

Supercritical fluid extraction in plant essential and volatile oil analysis

The use of supercritical fluids, especially carbon dioxide, in the extraction of plant volatile components has increased during two last decades due to the expected advantages of the supercritical extraction process. Supercritical fluid extraction (SFE) is a rapid, selective and convenient method for sample preparation prior to the analysis of compounds in the volatile product of plant matrices. Also, SFE is a simple, inexpensive, fast, effective and virtually solvent-free sample pretreatment technique. This review provides a detailed and updated discussion of the developments, modes and applications of SFE in the isolation of essential oils from plant matrices. SFE is usually performed with pure or modified carbon dioxide, which facilitates off-line collection of extracts and on-line coupling with other analytical methods such as gas, liquid and supercritical fluid chromatography. In this review, we showed that a number of factors influence extraction yields, these being solubility of the solute in the fluid, diffusion through the matrix and collection process. Finally, SFE has been compared with conventional extraction methods in terms of selectivity, rapidity, cleanliness and possibility of manipulating the composition of the extract.     

The use of alternative fluids in on-line supercritical fluid extraction – capillary gas chromatography

A key feature differentiating analytical supercritical fluid extraction (SFE) from conventional liquid extraction is the possibility of varying the solvent strength of a supercritical fluid to achieve selective extractions of specific target compounds, or functional classes of compound, from complex matrices. This can be accomplished by using supercritical fluids other than carbon dioxide, for example, sulfur hexafluoride, nitrous oxide, or sulfur hexafluoride-modified carbon dioxide. The use of these fluids will be demonstrated by the characterization of complex environmental and petroleum matrices by directly coupled SFE – capillary GC. On-line SFE-GC involves the decompression of pressurized extraction fluid directly into the heated, unmodified capillary split injection port of the chromatograph. This paper will also show how, by adjustment of the extraction temperature and pressure, SFE selectivity may be further enhanced.     

Comparison of extraction techniques for the isolation of explosives and their degradation products from soil

A comparison of four extraction techniques used for the isolation of 14 explosive compounds (Method 8330-Explosives) from spiked soil samples is described. Soxhlet warm extraction (SWE), pressurized solvent extraction (PSE), microwave assisted extraction (MAE) and supercritical fluid extraction (SFE) were included. The effects of basic extraction conditions – i.e. type of extraction solvent, temperature, pressure, and extraction time – were investigated. The best extraction recovery of the monitored compounds from spiked soil was obtained using pressurized solvent extraction. Recoveries of explosives using the PSE technique were in the range from 65 to 112%. Extraction recoveries by Soxhlet warm extraction and supercritical fluid extraction reached 65–99% and 52–75%, respectively. The lowest extraction recoveries (28–65%) were obtained using microwave assisted extraction. A very low extraction recovery for tetryl was observed in all cases but the best results were achieved by pressurized solvent extraction (58%).     

Application of sequential extraction with supercritical CO(2), subcritical H(2)O,and an H(2)O/CO(2) mixture for estimation of environmentally mobile heavy metal fractions in sediments

Results from use of a new isolation procedure based on sequential extraction with supercritical CO(2), subcritical H(2)O, and an H(2)O/CO(2) mixture in the same supercritical fluid extractor have been compared with results from the BCR-recommended three-step sequential extraction procedure. The new procedure gives more detailed information about environmentally mobile fractions (water-soluble, bicarbonate-forming), and in less time (5-6 h), than the BCR procedure.     

Comparison of supercritical fluid and ultrasound-assisted extraction of carotenoids and chlorophyll a from Dunaliella salina

In the work described here the extraction processes of carotenoids and chlorophylls were analysed using two extraction techniques, namely ultrasound-assisted extraction and supercritical fluid extraction, and the results are compared. The solvents used for the ultrasound-assisted extraction were N,N′-dimethylformamide and methanol and for the supercritical fluid extraction, carbon dioxide. The raw material studied was Dunaliella salina, a microalgae characterized by the high levels of carotenoids present in its cellular structure. The results indicate that the supercritical fluid extraction process is comparable to the ultrasound-assisted extraction when methanol is used as solvent. In addition, the supercritical extraction process is more selective for the recovery of carotenoids than the conventional technique since it leads to higher values for the ratio carotenoids/chlorophylls. Finally, the effects of pressure and temperature on the extraction yields of the supercritical fluid extraction process were studied.