天然产物的超临界流体萃取

本文叙述了超临界流体萃取的基本原理、过程和近来在天然产物研究与开发方面的进展。     

Effects of pressure and temperature of supercritical carbon dioxide on the extraction of triacylglycerols from plant tissue

The rate of extraction of triacylglycerols with supercritical carbon dioxide can be greatly enhanced by raising the pressure of the fluid to 600 bar, or higher, and its temperature to 60°C, or higher. Both the amount of carbon dioxide and the time required for complete extraction are reduced at such high pressures and temperatures.     

芫荽子的超临界CO2流体萃取研究

本文用超临界ＣＯ２流体技术对芫荽子的萃取进行了研究,探讨了原料粒度、温度、压力、流体密度对萃取效率的影响,并对其中挥发油的选择性萃取作了初步探索。     

干姜化学成分分析

利用气 质分析比较了干姜超临界提取物质及挥发油的化学组成 ,并用高效液相对干姜超临界提取物中的 6 姜醇进行了含量测定     

超临界CO_2萃取去除蛋黄粉中胆固醇和甘油三酯的研究

采用超临界 CO2 萃取 ,对去除蛋黄粉中胆固醇和甘油三酯进行了研究 .市购鲜鸡蛋去壳、分别收集湿蛋白和蛋黄 ,在 4 5℃下分别真空干燥 ,得蛋白粉和蛋黄粉 .取蛋黄粉装入高压釜中 ,进行超临界 CO2 循环萃取 .通过正交试验得最佳工艺条件是 :A萃取压力为 31 .5MPa,B萃取温度 4 0℃ ,C被萃取蛋黄粉重 30 0 g,D萃取时间 3h.所得蛋黄粉中胆固醇和甘油三酯等中性脂的残留量质量分数仅为 0 .0 1 9% .与不含此类脂质的蛋白粉混合 ,制成几乎不含胆固醇和甘油三酯的高级绿色保健营养食品鸡蛋粉 .     

Combining supercritical fluid extraction of soil herbicides with enzyme immunoassay analysis

Supercritical fluid extraction (SFE) of soil herbicides followed by enzyme immunoassay analysis (EIA) is explained in a step-by-step process. Extracted herbicides, include 2,4-D, simazine, atrazine, and alachlor. The herbicide, trifluralin was not successfully analyzed by EIA because of crossreacting metabolites. Problems with SFE, including uneven packing of cells, leaks, uneven flow and clogging, can largely be eliminated as the method parameters are optimized. It was necessary to add modifiers including methanol or acetone to the SF CO₂ to increase the solubility of the analytes. Detection limits of 2.5 ng/g soil for atrazine and alachlor and 15 ng/g soil for simazine and 2,4-D without concentration of the sample were achieved. Recoveries above 80% and relative standard deviations (RSDs) less than 15% for 2,4-D simazine, atrazine and alachlor were achieved. Atrazine and alachlor recoveries were above 90% with RSDs below 10%. Forty soil samples could be extracted and analyzed in an 8-h day.     

地鳖虫活性物质的超临界CO_2萃取及其药效

应用超临界流体萃取技术萃取地鳖虫Eupolyphaga sinensisWalker活性物质,采用三因素三水平正交试验方案,考察压力、温度、时间等参数对萃取地鳖虫活性物质萃取量的影响。同时,对萃取产物与水提物进行药效比较。结果表明,在试验设计范围内,萃取压力18 MPa、温度55℃、时间90 min为最佳工艺参数组合,地鳖虫活性物质萃取量最大能达到62.50 mg/g,影响萃取量三因素主次关系为压力>温度>时间。地鳖虫超临界萃取产物对镇痛、消炎和抗凝血有较好的效果,相对于水提物有更好的发展潜力。     

Some Properties of Endo-polygalacturonase from Trichosporon penicillatum SNO-3

Some properties of the endo-polygalacturonase from Trichosporon penicillatum were investigated. The enzyme showed the highest activity around pH 5.0 and was stable at this pH up to 50°C. The enzyme catalyzed the hydrolysis of galacturonic acid oligomers as well as its polymer. The pentamer was degraded to a trimer and a dimer, the tetramer to a trimer and a monomer, and the trimer to a dimer and a monomer, respectively, whereas the dimer was not degraded. The kinetic constant V_max and Km values changed with the substrate chain-length; the Km values tended to decrease, whereas the V_max values tended to increase with increasing chain-length of the substrate. The amino acid residue participating in the active site of the enzyme was studied and it was found to be histidine.     

Supercritical fluid extraction of naringin from the peel of Citrus paradisi

The highest yield (14.4 g/kg) of naringin, the major flavonoid from the peel of Citrus paradisi L., that could be achieved by supercritical fluid extraction was obtained using supercritical carbon dioxide modified with 15% ethanol and fresh (rather than dried) peels at 95 bar and 58.6 degrees C. This yield is higher than that attained by the conventional technique of maceration, and close to those obtained by reflux and Soxhlet methods. Furthermore, supercritical fluid extraction consumes less solvent and provides a shorter extraction time than conventional extraction methods.     

Screening of Red Algae Filaments As a Potential Alternative Source of Eicosapentaenoic Acid

Lipids were extracted by a supercritical fluid extraction method from 10 species of filamentous red algae obtained from culture collections and their fatty acid compositions were determined. The fatty acid profiles of the 10 species were similar. The major fatty acids were 16:0, 20:4ω6 and 20:5ω3 (eicosapentaenoic acid, EPA), which amounted to over 70% of the total fatty acids. The highest EPA content (29.8 mg/L), as a percentage of total fatty acids, was produced by Liagora boergesenii filaments, which has good potential for EPA mass production in pilot plants.     

Simultaneous Measurement of Fluoroquinolones in Eggs by a Combination of Supercritical Fluid Extraction and High Pressure Liquid Chromatography

Simultaneous detection of the fluoroquinolone antibiotics ciprofloxacin, enrofloxacin, ofloxacin, and norfloxacin in eggs by a combination of supercritical fluid extraction (SFE) and high pressure liquid chromatography (HPLC) was studied. Lipid matrices that have been considered to result in poor extraction and isolation of fluoroquinolones in eggs were removed first by SFE with supercritical CO₂ alone, and then the fluoroquinolones were extracted by SFE with supercritical CO₂ containing 20% (v/v) methanol for HPLC analysis. A time-course study of the extraction of lipid matrices of eggs suggested that the SFE method successfully removed the matrices within 20 min. When the fluoroquinolones added to control eggs were extracted by SFE, the extraction efficiency was similar to that by the solvent extraction method, giving the recovery percentages from 83 to 96% in a 40 min-extraction time. The fluoroquinolones extracted from eggs by SFE were analyzed simultaneously by HPLC equipped with a fluorescence detector with detection sensitivity at about 10 ppb for the detection limit. The standard calibration profiles of fluoroquinolones showed linear responses to HPLC, showing more than 0.995 for the mean r ² value. This is the first report of the simultaneous measurement of fluoroquinolones in eggs by a combination of SFE and HPLC. Using the SFE method allowed us to avoid extensive sample preparation such as solvent extraction and chromatographic cleanup that are basically required in extraction of fluoroquinolones.     

糖茶藨种子脂肪酸含量分析

用超临界萃取技术对产于青藏高原上的糖茶蔗种子中脂肪酸进行萃取,其萃取率为12％。用毛细管气相色谱对萃取的脂肪酸进行了分离和分析。结果表明不饱和脂肪酸的质量分数在90％以上。其中α-亚麻酸（α-linolenic acid）为27.4％,У-亚麻酸（У-linolenic acia）为2．70％。亚油酸（1inoleic acid）40．0%,油酸（oleic acid）21．0％。     

中药现代化与超临界流体萃取的应用

论述了超临界流体萃取技术在中药开发及产业化中应用的优越性,萃取能力强、提取率高、有效成分高度富集;操作温度低,有铲成分不被破坏;提取时间快、生产周期短,操作参数容易控制,有效成分及产品质量稳定,超临界ＣＯ２具有灭菌作用;应用于药物分析,是一种高效的分析手段,能客观地反应３中药有交成分的起初含量;该不仅工艺上优越,质量标准容易控制,其萃取药药理、临床效果能够保主或更好;流程简单、操作方便,节省劳动力     

石油菜挥发油和超临界流体萃取物化学成分的GC-MS分析

首次利用水蒸气蒸馏法和超临界流体萃取法(SFE)对石油菜地上部位进行提取,分别获得挥发油和SFE萃取物,采用气相色谱-质谱联用技术(GC-MS)结合计算机数据库检索对这两种提取物的化学成分进行了分析鉴定,采用峰面积归一化法测定了其中各个化学成分的相对含量。从挥发油中共分离出39个色谱峰,鉴定了其中28个化学成分,已鉴定出的成分的相对含量总和占化合物检出总量的91.90%,化合物类型均为萜类。从SFE萃取物中共分离出136个色谱峰,鉴定了其中65个化学成分,已鉴定出的成分的相对含量总和占化合物检出总量的58.17%,化合物类型包括萜类、芳香族类和脂肪族类。挥发油和SFE萃取物均含有α-蒎烯、石竹烯和桉油烯醇,其他成分则存在较大差异。     

超临界CO_2萃取冬虫夏草子座挥发性成分的GC-MS研究

报道冬虫夏草挥发性成分的组成,为其进一步的研究工作奠定基础。采用超临界CO2萃取法从冬虫夏草子座中提取挥发性成分,气相色谱-质谱联用技术对其化学成分进行分析。超临界流体萃取物共鉴定了39种组分,占总馏出组分的86.6%以上,占色谱总馏出峰面积的98.56%以上。已鉴定组分中,含量最高的为油酸,相对含量25.6%;其次为亚油酸,相对含量22.67%;再次为棕榈酸11.86%。超临界CO2萃取法能更真实、全面的反映药材中的化学成分,适合于珍稀中药材相关组分的测定。     

超临界CO2萃取烟叶中茄尼醇的工艺研究

采用超临界二氧化碳萃取烟叶中的茄尼醇,考察了萃取过程温度、压力、二氧化碳流量、萃取方式、夹带剂种类及其用量对萃取过程的影响。采用四因素三水平的正交设计,以茄尼醇的提取率为指标,对萃取条件进行了优化。并建立了能较准确测定烟叶中游离茄尼醇含量的方法,采用高效液相色谱对萃取产物进行了分析。以探索提高提取率的方法,为其工业化生产提供参考。结果表明：最佳萃取工艺条件为：甲醇为夹带剂,萃取温度45℃,萃取压力25 MPa,CO₂流量15 kg·h^-1。在最佳工艺条件下茄尼醇的提取率为：92.1%。     

超临界流体萃取——高效液相色谱法测定百合中秋水仙碱

分别用超临界二氧化碳流体和有机溶剂萃取百合中的秋水仙碱,然后用高效液相色谱法直接测定萃取物中秋水仙碱的含量,从而测得百合中秋水仙碱的含量。超临界流体萃取的条件是：用乙醇作提携剂,萃取压力为18MPa,萃取温度为40℃,高效液相色谱测定条件为：ODS柱,甲醇：磷酸二氢钾溶液作流动相,检测波长为220nm,此法快速,简便,准确,可应用于秋水仙碱原料,制剂及其它植物中秋水仙碱含量的测定。     

梧桐子超临界CO2流体萃取物脂溶性成分的GC-MS分析

采用超临界流体孳取法（SFE）和气相色谱-质谱联用技术（GC／MS）对梧桐子中脂溶性化学成分进行分析,并用NIST质谱数据库对其进行分析和鉴定。共分离鉴定出10种物质．大部分为不饱和脂肪酸类和酯类,占色谱总流出峰面积的83．37％。     

超临界二氧化碳萃取亚麻籽油的研究

采用半连续流程以亚麻籽（含水率5％,含油率47％）为原料,超临界CO2为溶剂萃取亚麻籽油。探讨了操作压力,温度,时间,CO2流量及亚麻籽破碎情况对萃取的影响。用国家标准分析了不同萃取条件下得到的亚麻籽油,用GC－MS分析了亚麻籽油的组成,亚麻酸是主要成分,超临界萃取得到的亚麻籽油可作为高质量的保健食用油。     

Extraction of squalene from yeast by supercritical carbon dioxide

Squalene produced under anaerobic conditions, by a strain of Torulaspora delbrueckii was extracted from the biomass using supercritical carbon dioxide. Minimum use of solvent, lower time of isolation and a higher selectivity of extraction merit use of supercritical fluid extraction (SFE) technique over solvent extraction of squalene, as optimized and reported previously. A maximum squalene yield of 11.12 g g^–1 (dry weight) of yeast cells was obtained at a temperature of 60 °C and pressure of 250–255 bar at a constant flow rate of 0.2l min^–1 of carbon dioxide. Lyophilization prior to SFE increased the squalene yield to 430.52 g g^–1 dry weight of yeast cells, an amount that is far greater than that obtained by (2:1) chloroform–methanol solvent extraction.