α-生育酚在超临界 CO_2 中溶解度神经网络模型的建立

生育酚有很高的生理活性 ,油脂生产中得到的脱臭馏出物含有丰富的天然生育酚。作为萃取生育酚的基础 ,该文对甲酯化油脂脱馏出物中 α-生育酚在超临界 CO2 中的溶解度进行了测试 ,并用 Chrastil分子缔合模型和RBF神经网络模型对溶解数据进行了拟合。Chrastil分子缔合模型的相对误差为 2 5 .36 %。对于 RBF神经网络模型 ,经过网络学习和训练 ,训练集平均误差仅为 0 .32 % ,测试集误差为 6 .48% ,效果比较理想     

α-生育酚在超临界CO2中溶解度神经网络模型的建立

生育酚有很高的生理活性，油脂生产中得到的脱臭馏出物含有丰富的天然生育酚。作为萃取生育酚的基础，该文对甲酯化油脂脱馏出物中α-生育酚在超临界CO₂中的溶解度进行了测试，并用Chrastil分子缔合模型和RBF神经网络模型对溶解数据进行了拟合。Chrastil分子缔合模型的相对误差为25.36%。对于RBF神经网络模型，经过网络学习和训练，训练集平均误差仅为0.32%，测试集误差为6.48%，效果比较理想。     

豆油脱臭馏出物中α-生育酚在超临界CO2中溶解度的研究

生育酚有很高的生理活性,油脂生产中得到的脱臭馏出物含有丰富的天然生育酚。作为萃取生育酚的基础,该文研究了油脂脱臭馏出物中α-生育酚（α-T）在超临界CO₂中的溶解度。研究结果表明：1）酯化处理能明显提高α-T的溶解度;2）α-T溶解度随系统压力的升高而升高;3）未酯化的原料中α-T的溶解度随温度的提高而提高;酯化过的原料中α-T的溶解度随温度的提高,先降低、随后上升。从α-T与脂肪酸之间氢键缔合关系、溶质之间的协同作用和操作参数等方面对上述结果的形成进行了分析。     

超临界CO2萃取烘烤花生中挥发性物质的研究

采用超临界CO2技术萃取烘烤花生中挥发性物质,用固相微萃取-气相色谱质谱联用(SPME-GC-MS)技术鉴定萃取物的风味组分,并将样品偏差值和感官评价相结合,评价萃取物香气协调性变化,综合进行萃取条件的优化,以建立一种烘烤花生风味物质的提取方法.结果显示,萃取压力25MPa,萃取温度55℃,萃取时间120min;超临界CO2萃取能萃取出烘烤花生中近85％的挥发性风味组分,该条件下超临界CO2萃取物风味轮廓感官上与烘烤花生原始风味接近.采用样品偏差值可以定量评价超临界萃取烘烤花生中风味物质香气协调性的变化.     

超临界CO_2法制备褪黑素脂质体的工艺优化

为了优化褪黑素脂质体的生产工艺、提高包封率以及褪黑素的生物利用度,采用响应面法优化超临界CO2制备褪黑素脂质体的工艺参数。在单因素试验基础上以共溶剂浓度、超临界时间、超临界压力为影响因素,脂质体的包埋率为响应值,运用分析法建立了二次多项式数学模型,并分析模型的有效性及各因素间的交互作用。最终响应面法优化的工艺参数为:乙醇浓度为7.5%,超临界温度为50℃,超临界时间为35 min,此时包埋率可高达83.2%。采用超临界二氧化碳法制备褪黑素脂质体具有工艺简单、重现性好,且脂质体包封率高、颗粒粒径小、稳定性较高等优点,为今后的实际生产提供了理论基础和科学依据。     

基于TDLAS的储粮二氧化碳激光检测系统研制

储粮过程由微生物及害虫等组成的生物场与温度和湿度等构成的非生物场所造成的影响会降低粮食品质,影响粮食安全。储粮中二氧化碳浓度反应粮库生物场状况,是储粮生物场监测的重要指标。为实现储粮二氧化碳浓度高精度检测,该研究基于可调谐半导体激光吸收光谱(Tunable Diode Laser Absorption Spectroscopy,TDLAS)技术高灵敏度和快速响应的特点研制了一套储粮二氧化碳浓度现场检测系统,并建立了二氧化碳激光光谱分析与数据处理方法。基于便携式要求,系统采用紧凑型设计,集二氧化碳浓度、温度及湿度检测功能于一体,同时实现弱信号调理、二氧化碳浓度计算及生成多参数云图、水势图显示等功能。整机尺寸338 mm×251 mm×88 mm,室温条件下功耗小于1.3 W。试验结果显示：该检测系统能够长时间稳定工作,人机交互功能鲁棒性较好,对储粮二氧化碳浓度检测的响应时间小于20 s,线性误差小于1.2%,检测重复性为0.4%,检测精度为10mg/m³,检测范围为0～20 000 mg/m³,温度的检测范围为-40～120℃,湿度检测范围为0...     

亚临界丙烷萃取米糠油及其微量活性组分动力学模型

为了揭示亚临界流体萃取米糠油及其微量活性组分的动力学规律,该文以亚临界丙烷为萃取介质,研究了米糠油、γ-谷维素及α-生育酚等活性组分在不同萃取温度和时间的萃取率,并基于 Baümler 模型对目标物的萃取率进行模型拟合,建立相应的动力学模型并验证。结果表明,亚临界萃取过程中目标物的相对萃取率随时间增长递增,且在初始阶段（洗涤过程）的增长速率快于第二阶段（扩散过程）的增长速率;同时,升高萃取温度可同时提高目标产物的扩散系数和相对萃取率;基于Baümler模型可较好拟合亚临界丙烷萃取米糠油、γ-谷维素和α-生育酚的动力学过程（R2>0.95）,所得动力学模型具有较好的预测准确性。由Arrhenius方程可计算出米糠油、α-生育酚和γ-谷维素的亚临界萃取反应活化能,其中米糠油的活化能最低（5.23 kJ/mol）,α-生育酚次之（7.05 kJ/mol）,γ-谷维素最高（9.11 kJ/mol）,表明γ-谷维素最难萃取且对温度依赖程度最高;根据拟合所得动力学模型,对米糠油提取率进行预测,结果表明,该模型对米糠油萃取率的预测准确率达95.8%,而对γ-谷维素和α-生育酚萃取率的预测准确度稍低,分别达94.7%和94.4%,对三者均具有很好的预测准确性。总之,基于 Baümler 模型可以较好地建立米糠油及其有益伴随物的亚临界萃取动力学模型,从而较为准确的预测米糠油及其微量活性组分的萃取率,对米糠油的亚临界萃取工艺具有一定的理论指导意义。     

初烤烟叶中烟碱和新植二烯的提取工艺研究

为探究云南烟油的成分以及烟碱和新植二烯的提取工艺,本试验以云南典型初烤烟叶为原料,通过超临界CO2萃取、超声辅助萃取、索式回流萃取和溶剂萃取4种方法提取初烤烟叶中烟碱和新植二烯,采用气相色谱-质谱(GC-MS)分析萃取物组成,比较不同萃取方法和萃取溶剂下,烟叶萃取物得率及所得萃取物中烟碱和新植二烯的相对含量.结果 表明...     

超临界二氧化碳萃取蒜汁中大蒜油的研究

利用超临界二氧化碳对蒜汁中大蒜油的萃取进行了研究,结果表明：萃取釜中添加填料可以大大提高萃取速度;一次压榨汁大蒜素含量高,萃取速度快,但通过延长萃取时间,两次压榨汁可以得到较高的萃取率;超临界CO₂萃取蒜汁中大蒜油的最佳萃取条件为萃取压力15 MPa,萃取温度40℃,CO₂流量11 kg/h。该方法得到的大蒜油成分与从破碎大蒜固体中萃取得到的大蒜油成分基本相同,大蒜素含量在40%以上。     

适宜提取方法提高美藤果油提取率及油品质

为了提高美藤果油的提取率以及油的品质,该文以美藤果为原料,比较了水酶法、超临界CO2萃取法、超声波辅助有机溶剂萃取法和低温冷榨法这4种不同的提取方法对美藤果油提取率和油品质的影响;并采用气相色谱-质谱联用法（gas chromatograph-mass spectrometer-computer, GC-MS）和高效液相色谱法（high performance liquid chromatography, HPLC）测定美藤果油的营养组成,以及以1,1-二苯基-2-三硝基苯肼（1,1-Diphenyl-2-picrylhydrazyl radical 2,2-Diphenyl-1-(2,4,6-trinitrophenyl) hydrazyl,DPPH?自由基）清除率为指标比较了美藤果油与其他植物油的体外抗氧化活性。结果表明：4种提取方法中,水酶法和超声波辅助有机溶剂提取法油脂提取率较高,分别为95.1%和92.7%,其次为超临界萃取法,为86.44%。但超临界CO2萃取法提取出的油脂综合理化指标优于其他３种提取方法,其中水酶法提取出的油不溶性杂质、酸价、过氧化值和黄色值都低于超声波辅助有机溶剂萃取法和低温冷榨法,但感官品质最差。综合考虑得出：超临界萃取法为美藤果油较佳的提取方法。此方法提取的美藤果油中富含不饱和脂肪酸和生育酚、多酚等活性成分,不饱和脂肪酸质量分数高达92.37%,总生育酚和总多酚质量分数分别为59.2 mg/(100 g)、10.2 mg/(100 g),但不含有维生素A;美藤果油对DPPH·自由基的半数抑制率IC50为1.148 mg/mL,明显低于橄榄油、茶油、亚麻籽油和紫苏油（P<0.01）,说明美藤果油体外抗氧化能力较强。研究结果可为美藤果油进一步开发提供参考。     

不同干燥方法对罗非鱼片品质和微观结构的影响

为了解不同干燥方法对罗非鱼片干燥后品质和微观结构的影响,采用热风干燥、真空冷冻干燥、超临界CO2干燥等3种方法对罗非鱼片进行干燥,研究其对营养成分、微生物、感官特征、复水性能、质构特征、微观结构等的影响。结果表明:与热风干燥和真空冷冻干燥相比,超临界CO2干燥的鱼片,粗蛋白含量高,脂肪含量较低;且在杀灭微生物方面有着显著的优势;但其鱼片的收缩率和复水特性稍差于真空冷冻干燥,而其感官、质构和微观结构等品质均与真空冷冻干燥的相当,而所有品质都明显优于热风干燥;结合经济性等综合考虑,罗非鱼片应用超临界CO2干燥是可行的。研究结果可为罗非鱼片干燥技术的选择提供参考。     

Supercritical CO(2) and subcritical propane extraction of pungent paprika and quantification of carotenoids, tocopherols, and capsaicinoids.

Ground paprika (Capsicum annuum L.) was extracted with supercritical carbon dioxide (SC-CO(2)) and subcritical propane at different conditions of pressure and temperature to estimate the yield and variation in carotenoid, tocopherol, and capsaicinoid contents and composition. The yield of paprika extract was found to be affected by the extraction conditions with SC-CO(2) but fairly constant at different conditions with subcritical propane. The maximum yields of oleoresin were 7.9 and 8.1% of ground paprika by SC-CO(2) and subcritical propane, respectively. The quantitative distribution of carotenoids, tocopherols, and capsaicinoids between paprika extract and powder was influenced by extraction conditions. SC-CO(2) was inefficient in the extraction of diesters of xanthophylls even at 400 bar and 55 degrees C, whereas tocopherols and capsaicinoids were easy to extract at these conditions. Under mild conditions subcritical propane was superior to SC-CO(2) in the extraction of carotenoids and tocopherols but less efficient in the extraction of capsaicinoids.     

超临界CO2干燥罗非鱼片的传质模型和数值模拟

为了探讨超临界CO2干燥罗非鱼的机理,该文基于微分床的质量守恒定律建立了超临界CO2干燥罗非鱼片的传质数学模型,通过Matlab软件对其干燥过程进行了数值模拟,分析了干燥室内超临界CO2中的溶质质量分数和罗非鱼片中的溶质质量分数随干燥时间和干燥床高度变化的规律,揭示溶质在超临界CO2干燥过程中的传质模式。结果表明:在超临界CO2干燥罗非鱼片的过程中,溶质传质主要以对流扩散为主,而以轴向扩散为辅;数值模拟的结果与试验值拟合良好(R2=0.97),相对偏差的绝对值在10%以内,说明建立的传质数学模型能较好的模拟超临界CO2干燥罗非鱼片的过程。研究结果可为超临界CO2干制罗非鱼片的工业化生产的过程控制提供参考。     

Designed polar cosolvent-modified supercritical CO2 removing caffeine from and retaining catechins in green tea powder using response surface methodology

This study examines cosolvent-modified supercritical carbon dioxide (SC-CO2) to remove caffeine from and to retain catechins in green tea powder. The response surface method was adopted to determine the optimal operation conditions in terms of the extraction efficiencies and concentration factors of caffeine and catechins during the extractions. When SC-CO2 was used at 333 K and 300 bar, 91.5% of the caffeine was removed and 80.8% of catechins were retained in the tea: 3600 g of carbon dioxide was used in the extraction of 4 g of tea soaked with 1 g of water. Under the same extraction conditions, 10 g of water was added to <800 g of carbon dioxide in an extraction that completely removed caffeine (that is, the caffeine extraction efficiency was 100%). The optimal result as predicted by three-factor response surface methodology and supported by experimental data was that in 1.5 h of extraction, 640 g of carbon dioxide at 323 K and 275 bar with the addition of 6 g of water extracted 71.9% of the caffeine while leaving 67.8% of the catechins in 8 g of tea. Experimental data indicated that supercritical carbon dioxide decaffeination increased the concentrations of caffeine in the SC-CO2 extracts at 353 K.     

Supercritical fluid extraction and high-performance liquid chromatographic determination of phloroglucinols in St. John's Wort (Hypericum perforatum L.)

A small-scale supercritical fluid extraction (SFE) method was developed for the selective extraction of phloroglucinols from St. John's wort (SJW) leaf/flower mixtures using supercritical carbon dioxide (CO(2)). The extraction efficiency was investigated as influenced by pressure, temperature, time, and modifier. The optimized condition of SFE was carried out at 3.80 x 10(4) kpa (5500 psi) and 50 degrees C. Samples were held in static extraction for 10 min, followed by a dynamic extraction for 90 min at the flow rate of 1 mL/min. A simple and sensitive HPLC method was developed for the analysis of hyperforin and adhyperforin, the major phloroglucinols, in the SFE extract of SJW.     

Extraction of azadirachtin A from neem seed kernels by supercritical fluid and its evaluation by HPLC and LC/MS

A new supercritical extraction methodology was applied to extract azadirachtin A (AZA-A) from neem seed kernels. Supercritical and liquid carbon dioxide (CO(2)) were used as extractive agents in a three-separation-stage supercritical pilot plant. Subcritical conditions were tested too. Comparisons were carried out by calculating the efficiency of the pilot plant with respect to the milligrams per kilogram of seeds (ms/mo) of AZA-A extracted. The most convenient extraction was gained using an ms/mo ratio of 119 rather than 64. For supercritical extraction, a separation of cuticular waxes from oil was set up in the pilot plant. HPLC and electrospray mass spectroscopy were used to monitor the yield of AZA-A extraction.     

Supercritical fluid extraction of all-trans-lycopene from tomato

A procedure is proposed for the supercritical fluid extraction of all-trans-lycopene from tomato using carbon dioxide at 40 degrees C without modifier. The present method minimizes the risk of degradation via isomerization and oxidation of health-promoting ingredients, such as lycopene. The effect of different experimental variables on the solvating power of the supercritical fluid was evaluated in terms of both the selectivity achievable in the process and the yield of the extraction of all-trans-lycopene. Satisfactory separations of the all-trans-lycopene isomers from the cis counterparts were achieved using a C(30) column. The obtained extract contained 88% all-trans-lycopene and 12% cis-lycopene.     

Valorization of Brazilian vetiver (Vetiveria zizanioides (L.) Nash ex Small) oil

The valorization of extracts from Brazilian vetiver (Vetiveria zizanioides (L.) Nash ex Small) roots was studied. This study took into account the extraction method, the chemical composition of the extracts, their sensorial characteristics, and the possibility of chemical transformations of the product. The performed extraction methods were hydrodistillation and extraction with supercritical carbon dioxide. Some pretreatment methods were tested on the vetiver roots and evaluated in terms of extraction yield, process time, chemical composition, and sensorial properties. Supercritical carbon dioxide extraction resulted in high yield (3.2%) in significantly less time than the other methods. The chemical compositions of the extracts obtained by the different methods were also compared to those of commercial vetiver oils from other sources, showing that Brazilian samples had a greater acid amount. An extraction in basic medium from Brazilian vetiver oil was done to remove its main acid (zizanoic acid), which was chemically transformed into an alcohol (khusimol) of desirable sensorial properties. Sensory evaluation indicated that the Brazilian volatile oil without acid could be used in perfumery and the extract obtained with supercritical carbon dioxide could have application in food.     

Comparison of eucalyptus camaldulensis Dehn. oils from Mozambique as obtained by hydrodistillation and supercritical carbon dioxide extraction

Leaf oils of E. camaldulensis Dehn. from Mozambique obtained by hydrodistillation and by supercritical carbon dioxide extraction under different conditions were compared with regard to their major components. The oil obtained by hydrodistillation showed high concentrations of 1,8-cineole (43%), alpha-pinene (5.5%), beta-pinene (3.4%), p-cymene (5.2%), terpinen-4-ol (3.1%), and globulol (4.1%). The extracts obtained by supercritical carbon dioxide extraction have lower amounts of 1,8-cineole, alpha-pinene, beta-pinene, and terpinen-4-ol, but have higher amounts of allo-aromadendrene and globulol. At the same time, distilled oil of E. radiata was extracted from an inert matrix (Celite) and the extract showed a higher content of 1,8-cineole at 80 bar and 60 degrees C than the feed, suggesting that a multiple-stage supercritical carbon dioxide extraction of the E. camaldulensis studied can produce an oil close to the market requirements set by the European pharmacopoeias.     

Supercritical fluid extraction of the pesticides carbosulfan and imidacloprid from process dust waste

Large amounts of contaminated process dust remain from the procedure of pesticide treatments applied to seed pellets. A pilot study in analytical-scale supercritical fluid extraction (SFE) was performed to determine the possibility of using supercritical carbon dioxide for the extraction of the nonpolar insecticide carbosulfan and the more polar insecticide imidacloprid present in contaminated dust waste, at concentrations of up to 20% (w/w). The effects of various experimental conditions, such as temperature, flow rate, and addition of modifier, on the recovery of the analytes were evaluated by extracting the pesticides both from spiked support material and from real dust samples. It was found that carbosulfan could easily be extracted from the dust waste within 30 min at 138 bar and 40 degrees C with a recovery of 98.9% (RSD = 2.3%, n = 10), compared to values obtained with a validated liquid extraction method. A sufficient removal of the more polar substance imidacloprid required the addition of a modifier, and the results showed a strong dependence of the extraction efficiency on the choice of modifier. Extractions at 276 bar and 80 degrees C with a solvent consisting of supercritical carbon dioxide modified with methanol (5%) gave a recovery of 97.0% (RSD = 3.6%, n = 10) using a 40 min extraction time. The results indicate that it seems to be possible to use process-scale SFE for the decontamination of pesticides from dust waste. The conditions outlined also permit analytical determinations of the two insecticides based on a combination of SFE and liquid chromatography.