湖北延胡索中延胡索乙素含量测定方法研究

采用微波辅助提取办法提取湖北产延胡索药材中的延胡索乙素,用高效液相色谱法对延胡索乙素的含量进行分析。使用Zorbax-C18反相柱,以V甲醇-V磷酸(55∶45)为流动相,控制流速1 m L·min-1,采用紫外可变波长检测器,检测波长为280nm,方法的线性关系良好,相关系数r=0.9999。     

巴马汀合成延胡索乙素的制备工艺

介绍巴马汀合成延胡索乙素的制备方法，通过活性镍催化加氢还原法制得该产品，收率在８６％以上。     

提取黄藤中巴马汀制备延胡索乙素的研究

用硫酸溶液从黄藤中提取巴马汀,用大孔树脂富集,使用正交试验优选出还原巴马汀制备延胡索乙素的工艺。在还原的正交试验中,还原剂和催化剂用量是影响产率的主要因素。巴马汀还原条件(乙醇浓度为80%、还原剂∶巴马汀=3∶1、催化剂∶巴马汀=1.5∶1)下制备延胡索乙素,粗产率可达88%~90%。碱性氧化铝分离后,产物与延胡索乙素对照品的PLC、熔点、紫外光谱的测定结果以及产物的核磁共振波谱结果表明,所得产物为延胡索乙素。     

RP-HPLC法测定不同产地延胡索中延胡索乙素含量

用RP-HPLC法测定了对不同产地延胡索中延胡索乙素的含量。测定使用Kromasil C18色谱柱(200 mm×4.6 mm,5μm),以甲醇-0.1%磷酸溶液(用三乙胺调至pH 6.09)(V∶V,55∶45)为流动相,流速为1.0 mL/min,检测波长为280 nm。该方法的线性范围是22.0~352.0μg/mL,平均回收率98.6%,RSD=0.4%(n=9)。该法可用于质量控制。     

高效液相色谱法测定延胡索中延胡索乙素含量

采用高效液相二极管阵列检测法测定延胡索提取物中延胡索乙素含量。采用ZORBAX XDB-C18色谱柱(4.60 mm×250 mm,5μm),以0.1%磷酸水溶液和甲醇为流动相,流速1.0 mL/min,柱温30℃,检测器温度30℃,检测波长280 nm。精密度和稳定性良好,延胡索乙素质量浓度为5~700 mg·L~(-1),标准物质峰面积与质量浓度线性关系良好(r0.999 5);加标回收率为98%~102%,相对标准偏差为0.94%~1.31%。     

HPLC测定丹黄祛瘀胶囊中延胡索乙素的含量

建立了丹黄祛瘀胶囊中延胡索乙素的含量测定方法。采用Agilent C18柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸(三乙胺调pH值至6.0)(60∶40),柱温30℃,流速1.0 mL/min,检测波长280 nm。结果显示:延胡索乙素在0.0408～0.2448μg线性关系良好(r=0.9994);平均回收率为98.6%,and RSD=1.1%(n=6),该方法可用于丹黄祛瘀胶囊的质量控制。     

延胡索挥发油提取方法研究

比较研究延胡索挥发油的常规提取方法并对其进行成分分析。采用索式提取法、加热回流法及超声提取法提取延胡索样品中挥发油成分,使用GC-MS进行分析检测。研究结果表明:加热回流法最为适合延胡索挥发油提取。此外,三种方法提取出来的挥发油成分和含量上均有差异,说明提取方法不同会对延胡索挥发油组分构成及含量造成影响。     

延胡索挥发油提取方法研究

比较研究延胡索挥发油的常规提取方法并对其进行成分分析。采用索式提取法、加热回流法及超声提取法提取延胡索样品中挥发油成分,使用GC-MS进行分析检测。研究结果表明:加热回流法最为适合延胡索挥发油提取。此外,三种方法提取出来的挥发油成分和含量上均有差异,说明提取方法不同会对延胡索挥发油组分构成及含量造成影响。     

高效液相色谱法测定止痛养胃软胶囊中延胡索乙素的含量

测定止痛胃软胶囊中延索乙素的含量,可用高效液相色谱法。选用甲醇—磷酸缓冲溶液(40∶60)为流动相,测定波长280nm。结果:延胡索乙素浓度在0.02140～1.37mg/mL范围内,与峰面积线性关系良好,y=(8.390×106)x+7.505×103(r=0.9997)。结论:该法操作简便、快捷、特异性强,可用于控制止痛养胃软胶囊的质量。     

酸水超声提取-液液萃取-HPLC测定延胡索中乙素的含量

建立了酸水超声提取-液液萃取-反相高效液相色谱法分析延胡索乙素含量的方法。考察了酸液浓度、酸液浸泡时间、料液比、超声时间、pH值、不同萃取溶剂等因素对延胡索乙素提取的影响。使用反相C18柱分离萃取液,流动相为甲醇-pH 6.0的0.1%磷酸缓冲溶液(6∶4),流速1.0 mL/min,检测波长为280 nm。在优化的色谱条件下,延胡索乙素的线性范围为5～200μg/mL,相关系数R2=0.9995,回收率为90.2%～100.1%。所建立的方法简便、准确、重现性好,可用于样品中延胡索乙素的测定。     

黄连中小檗碱的超声波提取工艺

以黄连为原料,研究小檗碱的超声波提取工艺。确定最佳工艺条件为:以乙醇为提取溶剂,超声时间30min、温度50℃、乙醇浓度80%和超声波提取两次。在此条件下,对超声波法提取小檗碱与传统乙醇浸提法进行比较,结果表明,超声波法提取工艺比传统乙醇浸提法小檗碱产量提高了42%。     

不同溶剂对丁二烯工艺的影响

文中对丁二烯抽提不同溶剂的物性特点进行了分析，并研究了这些特点对工艺流程的影响。     

苯乙烯抽提工艺萃取精馏最佳剂油比的探索

对苯乙烯抽提工艺的预分馏单元、选择性加氢单元、萃取精馏单元、溶剂回收单元进行了流程模拟,得到与实际运行工况基本吻合的工艺参数。通过对萃取精馏塔中溶剂进料量的改变,研究C8抽余油苯乙烯质量分数的变化趋势,找出萃取精馏塔的最佳剂油比为6.84。     

Experimental investigation and simulation of gas-liquid-liquid reactive extraction process for the production of hydrogen peroxide

The gas-liquid-liquid reactive extraction system for the production of hydrogen peroxide via anthraquinone route was investigated. The oxidation of the hydrogenated anthraquinone working solution by oxygen and the extraction of hydrogen peroxide from the working solution with deionized water were carried out simultaneously in a sieve plate column of 50 mm in diameter. The effects of the superficial velocity of oxygen on the conversion of 2-ethylanthrahydroquinone and the extraction efficiency of hydrogen peroxide were investigated, separately. The results showed that the oxidation and the extraction do not hamper each other, on the contrary, the presence of gas in the column can promote the transfer of hydrogen peroxide from the organic phase to the aqueous phase, therefore, the conversion of 2-ethylanthrahydroquinone and the extraction efficiency of hydrogen peroxide increased with the increase of gas superficial velocity. In addition, a mathematical model for the simulation of the gas-liquid-liquid reactive extraction process was developed. The predicted values were compared with the experimental data at different conditions and the agreement was found to be quite satisfactory for the production of hydrogen peroxide in a sieve plate column.     

A novel process for extraction of tea oil from Camellia oleifera seed kernels by combination of microwave puffing and aqueous enzymatic oil extraction

The objective of this study was to extract the oil from Camellia oleifera seed kernels by aqueous enzymatic oil extraction (AEOE). We describe a novel process for extraction of tea oil preceded by tea saponin extraction from C. oleifera seed kernels. The extraction efficiency obtained with microwave‐assisted extraction (MAE) is very high, which the recovery yield is up to 83% in 30 s and the saponins in camellia seed kernels can be completely removed by the second MAE. Moreover, an important step in the process development has been the pretreatment by microwave puffing of camellia seed kernel residues followed by AEOE increased oil extraction yield from 53% to 95%, which will is comparable to hexane oil extraction yields from plant materials.     

白花蛇舌草中总黄酮微波辅助提取工艺研究

研究了白花蛇舌草中总黄酮的微波辅助提取工艺,在单因素实验基础上,采用正交实验对提取工艺进行了优化。确定出最佳提取条件为：液料比20∶1mL/g、φ（乙醇）=80%、微波时间120s、微波功率400W、微波温度70℃,在此条件下,总黄酮的提取率达3.46%。     

An alternative sequential extraction process for maximal utilization of bioactive components from Korean red ginseng

Two types of sequential extraction process (SEP) for the recovery of bioactive components from Korean red ginseng were examined. As a SEP (normal SEP, nSEP), Korean red ginseng was sequentially treated using hot water and n-hexane for the successive extraction of water-soluble and lipid-soluble components. Also by changing the sequential order of solvents, an alternative SEP (reverse SEP, rSEP) in which n-hexane extraction was followed by hot water extraction, was proposed. Regardless of the sequential order of solvents, the recovery yield of acidic polysaccharide (AP) and crude saponin (CS) showed no significant change. On the other hand, in the rSEP, the lipid-soluble fraction was obtained from red ginseng with an enhanced recovery yield, four times higher than that in nSEP. Additionally, from dose-response assays to assess the effects of lipid-soluble components on the proliferation of human hepatoma (HepG2) and breast (MCF-7) cancer cell lines, it was found that hexane extract of red ginseng (HER) in rSEP has higher efficacy than the hexane extract of red ginseng marc (HERM) obtained in nSEP. This strongly suggested that rSEP would be a more attractive industrial process in terms of the efficacy of lipid-soluble extract as well as the recovery yield.     

A model to predict physical properties for light lubricating oils and its application to the extraction process by furfural

In the lubricating oil manufacturing process, the aromatic content of vacuum distillates is reduced by solvent extraction, frequently with furfural. In this work, a method based on average pseudo-components properties is developed to calculate physical properties (density, refractive index and sulfur content) of hydrocarbon mixtures. Obtained values were compared to those calculated by other methods reported in the literature, obtaining similar results. In order to simulate the extraction operation, a model based on a reduced number of pseudo-components and the NRTL model is reported for the system furfural+SPD lubricating oil. Thereafter, the extraction operation was simulated by using such model and Aspen Plus^® commercial software. Good agreement was found between predicted and experimental values of yield, furfural content, composition and physical properties for raffinates and extracts.     

Temperature and solvent effects on polyphenol extraction process from chestnut tree wood

Polyphenols are a group of chemical substances found in plants, characterized by the presence of more than one phenol unit or building block per molecule. Polyphenols are generally divided into hydrolysable tannins (gallic acid esters of glucose and other sugars) and phenylpropanoids, such as lignins, flavonoids, and condensed tannins.They are widely found in natural products, nowadays they are extensively used in food and beverage industry and in pharmaceutical and nutraceutical industry for their positive effects on human health.In conventional processes polyphenols are extracted from vegetable material using water as solvent in a temperature range from 40 to 90 °C.The aim of this work is to characterize chestnut tree wood in terms of total extractable polyphenols and assess the temperature and solvent type effects on the polyphenol extraction process. To this end, experimental data on equilibrium distribution of polyphenols between solid and liquid phases for different temperatures (ranging from 60 to 80 °C) and different solvent solutions (water and ethanol-water solutions) are reported. The obtained results have been correlated by means of Freundlich isotherm.Experimental data are also reported about the batch extraction kinetics of polyphenols from solid phase and analysed by a mathematical model to estimate the polyphenol diffusion coefficient inside the chestnut wood particles and the mass transfer coefficient in the liquid phase.