大孔树脂纯化黑果腺肋花楸多酚的工艺优化

以黑果腺肋花楸为原料,采用大孔树脂纯化黑果腺肋花楸中多酚类物质。通过对比6 种大孔树脂对黑果腺肋花楸多酚吸附-解吸效果,筛选出XAD-7大孔树脂作为最佳纯化材料,并通过单因素试验确定XAD-7大孔树脂纯化黑果腺肋花楸多酚的静态吸附-解吸最佳工艺条件为：吸附时间4 h、解吸时间2 h、上样液质量浓度3.6 mg/mL、上样液pH 4、乙醇体积分数95%、乙醇溶液pH 7;其对黑果腺肋花楸多酚动态吸附-解吸最佳工艺条件为：上样流速2 mL/min、上样量560 mL、蒸馏水洗脱用量350 mL、洗脱流速2 mL/min、洗脱体积300 mL。在此条件下,黑果腺肋花楸多酚纯度由11.62%提高到64.37%,表明XAD-7大孔树脂对于黑果腺肋花楸多酚具有较好的纯化效果。     

薏苡仁肽纯化的初步研究

研究了由蛋白酶酶解薏苡仁得到多肽,然后通过对DA201-C、XAD-1600、XAD7HP三种树脂在静态吸附过程中对薏苡仁酶解产物的吸附率随时间的变化规律进行测定,可知最大吸附率分别达到46·06%、36·93%、16·93%。在树脂的动态吸附过程中以1BV/h上样时的纯化效果最好,吸附率达到97·6%。因此,可以确定以DA201-C大孔树脂纯化薏苡仁酶解产物的效果最佳。最佳动态解吸条件:上样液pH为5,上样流速1BV/h,75%乙醇作为解吸液。然后利用HPLC测定树脂纯化后薏仁肽的相对分子质量分布,确定了纯化后的薏苡仁肽的分子量分布在278·61～943·32之间。     

大孔树脂吸附桦褐孔菌多糖色素的机理及工艺优化

为探究大孔树脂吸附桦褐孔菌多糖色素动力学与热力学特征及最佳工艺条件,本实验通过水提醇沉、Sevag法除蛋白、透析制备桦褐孔菌多糖,采用静态吸附实验筛选色素吸附率及多糖保留率评分最高的大孔树脂,研究其吸附动力学与热力学特性,并优化该大孔树脂在动态吸附桦褐孔菌多糖色素中的径高比、吸附时间、上样量以及洗脱流速,确定最佳工艺条件。结果表明,实验筛选的17个不同型号大孔树脂中,大孔树脂HPD-500最为适宜,其吸附色素的过程符合准二级动力学模型,反应过程中受颗粒内扩散与液膜扩散的影响;并且吸附过程符合热力学Freundlich模型,为多分子层吸附,其中吸附焓变>0为吸热反应,吉布斯自由能<0为自发反应,吸附熵变>0为熵增反应。HPD-500吸附色素的最佳条件为径高比1:10,吸附时间1 h,上样量10 mg,洗脱流速1.5 mL/min。在此条件下,桦褐孔菌的色素吸附率为83.15%,多糖保留率为78.89%,多糖纯度由20.40%提升至56.52%。HPD-500大孔树脂具有吸附桦褐孔菌多糖中色素、提高多糖纯度的能力,本文为桦褐孔菌资源高效利用提供了理论及实验基础。     

大孔树脂纯化脂溶性玉米黄色素

为探究脂溶性玉米黄色素的纯化方法,从NKA-9、XAD-7HP、D101、DA-201和聚酰胺吸附树脂5种层析树脂中选出DA201大孔吸附树脂,研究其对脂溶性玉米黄色素静态和动态吸附解吸性能,结果表明:DA201大孔树脂对脂溶性玉米黄色素的吸附4 h后达到平衡,饱和吸附量为0.0891 mg/g干树脂,最佳解吸剂为无水乙醇。玉米黄色素粗提浓缩液以2.5 mL/min流速上柱,吸附平衡后,以无水乙醇进行动态等度洗脱,研究其动力学过程。HPLC分析表明,动态纯化后玉米黄色素的质量分数从53.14%提高到86.64%。     

XAD-7型大孔树脂纯化黑果腺肋花楸多酚条件优化

对XAD-7型大孔吸附树脂纯化黑果腺肋花楸多酚的条件进行研究。以没食子酸为标准品,采用Folin-Phenol法测定黑果腺肋花楸多酚的含量,通过静态和动态吸附-解吸试验,考察了上样液浓度和pH值、上样流速、上样量、洗脱剂体积分数和pH值、洗脱流速、洗脱体积等因素对多酚吸附率和解吸率的影响。结果表明:XAD-7型大孔树脂静态吸附黑果腺肋花楸多酚的工艺条件为:上样液质量浓度2.67 mg/mL,上样液pH值4.0,吸附时间2 h;静态解吸工艺条件为:洗脱剂乙醇体积分数95%,pH值7.0,解吸时间1 h。黑果腺肋花楸多酚的动态吸附-解吸工艺条件为:上样量430 mL,上样流速1 mL/min,洗脱体积210 mL,洗脱流速1 mL/min。通过动态吸附-解吸后,黑果腺肋花楸多酚粗提物的纯度由9.56%提高到74.26%,表明XAD-7型大孔树脂法是纯化黑果腺肋花楸多酚的有效方法。     

大孔树脂纯化喀什小檗花色苷

研究XAD-7HP大孔树脂分离纯化喀什小檗花色苷的纯化工艺条件。通过树脂筛选和单因素实验确定适宜工艺参数:吸附时间是4h,体积分数60%乙醇溶液为洗脱液,解析时间100min,上样液pH值2.0,吸附温度为30℃,上样质量浓度为750mg/L,洗脱流速为1.0mL/min,。该工艺生产的花色苷产品为紫黑色粉末,色价和花色苷含量比纯化前分别提高了2.21倍和3.15倍。     

红枣三萜酸大孔吸附树脂纯化特性及其抗氧化活性研究

对红枣三萜酸的大孔吸附树脂纯化特性和抗氧化活性进行了研究。通过比较D101、AB-8、X-5三种大孔吸附树脂对红枣三萜酸的静态吸附和解吸特性,确定出D101大孔吸附树脂为最佳纯化树脂,进一步研究了D101大孔吸附树脂对红枣三萜酸的吸附等温线、动力学特征,并通过动态吸附解吸实验确定了最佳纯化条件。结果表明:D101大孔吸附树脂对红枣三萜酸具有良好的吸附和解吸性能,且其吸附过程符合准二级速率方程,吸附过程由多种扩散过程控制,其中薄膜扩散为主要扩散方式,吸附量随温度的升高而增大,吸附等温线方程符合Freundlich模型。D101大孔吸附树脂纯化红枣三萜酸的工艺条件为:上样体积7 BV,上样p H为7,洗脱剂为95%乙醇,洗脱剂p H为11,洗脱剂体积为5 BV。在此条件下得到的红枣三萜酸纯度由49%提高至78%。抗氧化活性实验结果表明红枣三萜酸经纯化后清除ABTS~+·与·OH的能力均有提高,而清除DPPH·的能力有所降低。     

大孔树脂回收花椒水溶性呈味物质的研究

用不同大孔树脂吸附花椒水性呈味物质,采用紫外分光光度法测定大孔树脂对花椒水性呈味物质的吸附量,选出效果最佳的大孔树脂;利用不同浓度的酒精对吸附饱和的大孔树脂进行洗脱,选出洗脱效果最佳的酒精浓度。研究结果显示:四种大孔树脂吸附能力的顺序为:XAD-16XAD-4HP3500,其中XHD-16大孔树脂的吸附效果最好,每克树脂可吸附13.33g花椒中的水溶性呈味物质;60%的酒精洗脱效果最佳。每克树脂需用9.33mL60%酒精洗脱。通过对花椒水溶性呈味物质吸附能力最佳的XAD-16再生寿命的研究,结果如下:经过45次周期使用后,树脂的吸附量基本无变化,再生寿命长。     

花生壳总黄酮的大孔树脂吸附动力学研究

以花生壳为原料，采用乙醇提取花生壳中的总黄酮，并用大孔树脂吸附花生壳总黄酮。研究了吸附过程中温度对吸附量的影响，并绘制静态吸附动力学曲线，根据静态平衡吸附量分别绘制颗粒内扩散、准一级吸附和准二级吸附的3种动力学拟合曲线，并计算3种动力学模型参数。结果表明：温度对大孔树脂吸附花生壳总黄酮的吸附量具有显著性的影响，该过程是一个吸热过程；吸附速率受到液膜扩散和颗粒内扩散共同控制；确定了大孔树脂吸附花生壳总黄酮的准一级吸附动力学模型公式，并通过Arrhenius方程计算得到吸附过程的活化能Ea为7.96 kJ/mol，该过程是一个物理过程。     

应用大孔树脂纯化花生壳总黄酮

研究大孔树脂纯化花生壳总黄酮的工艺条件,对大孔树脂的种类及其静态吸附、解吸附条件进行初步探讨。通过静态吸附和解吸附的比较,从7种不同型号的大孔吸附树脂中选出AB-8、DM301、NKA-9三种树脂进行静态吸附解吸动力学,发现NKA-9的吸附解吸效果较为稳定,其吸附解吸平衡时间分别为5h和2h。通过单因素试验,NKA-9的最佳吸附条件为35℃、样液pH7.5,样液中花生壳总黄酮初始浓度(0.112±0.02)mg/ml;最佳解吸条件为体积分数90%乙醇作为解吸液、解吸液用量15ml/g湿树脂、解吸液pH8.5。     

Macroporous resin purification behavior of phenolics and rosmarinic acid from Rabdosia serra (MAXIM.) HARA leaf

In the present study, the performance and separation characteristics of two macroporous resins for the purification of phenolics from Rabdosia serra were evaluated. Both HP-20 and XAD-7HP resins were effective for phenolics enrichment, with insignificant difference of adsorption/desorption behaviors, according to their chemical and physical properties. The pseudo-second-order kinetics model was the most favorable for illustrating the whole exothermic adsorption process, which was affected by the mutual effects of boundary layer diffusion and intraparticle diffusion kinetics. After treatment with gradient elution on resin columns, phenolics (from 16.66% to 67.87% by HP-20 and to 58.81% by XAD-7HP), antioxidants (3–4 times more than original) and rosmarinic acid (from 10.14% to 67.26% by HP-20 and to 63.16% by XAD-7HP) were enriched in 30% ethanol fractions. The production of highly concentrated phenolics and rosmarinic acid might expand the application of Rabdosia serra as a bioactive agent for both the food industry and pharmacy.     

大孔吸附树脂对石榴皮多酚的分离纯化

石榴皮中多酚含量丰富,具有抗氧化、抗衰老、抗癌防癌、抗菌、润肤美容、降血压和预防心脑血管疾病等多种生理和药理活性。在食品、医药和日用化学品等领域显示出巨大的应用价值。从XAD-16、XAD-1180、XAD-7HP、D101、DM-11、DM130、SP-700、SP-850、X-5、AB-8和H-103大孔吸附树脂中通过静态实验筛选出SP-700树脂,详细研究了其对石榴皮总单宁的静态与动态吸附和解吸性能。结果表明,SP-700树脂对石榴皮多酚的饱和吸附量为70.52mg/g(干树脂),吸附等温线符合Freundlich方程,为多分子层吸附,饱和吸附时间为5h,适宜解吸剂为体积分数70%的乙醇溶液,测定20、25、30、35℃下吸附等温线,表明最适宜的吸附温度是25℃,此时最大吸附量达到96.71mg/g(干树脂);以5mg/mL质量浓度的石榴皮提取液上柱,流速为4～4.5BV/h时,树脂的多酚穿透吸附容量65.72mg/g(干树脂),3.5BV体积分数70%的乙醇溶液可将吸附于柱上的石榴皮多酚完全洗脱。以该条件纯化石榴皮多酚提取物时,纯化样的收率为26.5g/100g(干石榴皮),多酚质量分数从48%提高到...     

ADSORPTION CHARACTERISTICS OF CROCIN IN THE EXTRACT OF GARDENIA FRUITS (GARDENIA JASMINOIDES ELLIS) ON MACROPOROUS RESINS

To study resin adsorptions and investigate the differences between processes in crude extracts and microfiltrates, the adsorption characteristics of crocin in the extract of Gardenia jasminoides Ellis on 10 macroporous styrene-divinylbenzene (SDVB) resins were investigated. Ground gardenia fruit was extracted with water and the crude extract was partially purified by microfiltration. The crude extract and microfiltrate were mixed with the 10 resins until the adsorption of crocin reached equilibrium on resins. The adsorption followed the pseudo-second-order kinetics closely, but the data also fitted the first-order and intraparticle diffusion models. Furthermore, the Freundlich isotherm was found suitable for describing the equilibrate adsorption data. XAD-1180, HP20, HPD-100A and AB-8 stood out as the best performing resins in terms of their adsorptive capacities and selectivities for crocin. The thermodynamics of the adsorption process was shown to be spontaneous and exothermal in nature, and controlled by physical rather than chemical mechanisms. Adsorption with SDVB resins in conjunction with microfiltration was found to be an efficient process for the purification of crocin in gardenia extract.

PRACTICAL APPLICATIONS

Macroporous resins have been industrially applied in the recovery and purification of some products from plant extracts. However, there is a lack of understanding of the adsorption process and many of the applications are based on empirical data rather than on predicable models. Therefore, the development of reliable mathematical models that can accurately describe and predicate experimental data of adsorption would be extremely helpful in understanding the adsorption process as well as optimizing the design of adsorption systems.     

大孔吸附树脂吸附分离高活性玉米抗氧化肽

采用大孔吸附树脂对玉米抗氧化肽进行分离,通过单因素试验得出XAD-7HP树脂为最适树脂,在此基础上,研究不同pH值条件下的静态吸附能力和不同解吸剂的静态解吸能力等实验,确定玉米抗氧化肽吸附分离的基本参数为pH7.0、解吸剂体积分数70%。通过动态吸附分离实验得出,该树脂可以达到分离纯化玉米抗氧化肽的目的,而且分离后的玉米肽的抗氧化活性比原液提高了1倍。     

The use of different adsorbents for selective removal of compounds from olive residue oil miscella

The selective removal of several impurities from a solution of crude olive residue oil in n-hexane (miscella) using batch adsorption by different materials, used separately or in sequence, was investigated. The following adsorbents were tested: activated diatomaceous earths, powdered activated carbon and synthetic neutral resins ("Amberlite XAD-4, XAD-7, XAD-16). The adsorption efficiency of every group of compounds depended on the adsorbent and the ratio (amount of adsorbent/amount of oil) used. The activated earths and carbon were very much more effective in the adsorption of the compounds from the miscella than the resins. Results were similar for every resin tested. An effective removal of green pigments (chlorophylls and pheophytins) and carotenoids was achieved with every adsorbent tested. With respect to the adsorption of conjugated hydroperoxides (HP), a removal of 50-60% was attained with activated carbon and earths, in contrast to a 20% removal by the resins. For the final oxidation products (FOP), a 60% removal was observed with powdered carbon, 20-30% with earths and 20% with resins. A removal of 20% of free fatty acids (FFA) by activated earths or powdered carbon and 40% by the resins was observed. When the adsorbents were used in sequence (carbon or earths followed by XAD-7 resin), the resin was able to adsorb the remaining FFA, HP and FOP.     

大孔吸附树脂法精制金花茶皂甙的工艺研究

研究大孔吸附树脂法精制金花茶皂甙的工艺条件。比较了聚酰胺、AB-8、XAD-1600和XAD-164种树脂对金花茶皂甙的静态吸附及解吸性能,筛选出最佳吸附剂,并对其吸附动力学特征及解吸条件进行研究。结果表明,XAD-16型树脂的吸附与解吸效果最佳,优化出的最佳柱分离条件为:上样液浓度24.42mg/mL,pH4.88,上样流速1.20BV/h,洗脱过程用1.25BV的蒸馏水除杂后依次用1.75BV30%(v:v),2BV60%(v:v)的乙醇溶液阶段洗脱,精制得2个皂甙组分S2、S3,测定纯度分别为89.48%、70.61%,得率分别为38.94%、30.07%。经颜色反应,两者均为三萜类皂甙。     

基于组合色谱技术的蓝莓果实中花色苷元制备

首先采用液液萃取及大孔树脂层析技术研究花色苷的制备方法,萃取剂为乙酸乙脂,大孔树脂为Amberlite XAD-7HP,在此基础上制得花色苷粗提液。花色苷经酸水解、浓缩后,采用固相萃取技术（C18小柱）对花色苷元进行除酸、除糖处理,制得了纯度为70.2%的花色苷元混合物。最后采用半制备型高效液相色谱技术实现4 种主要花色苷元单体的分离,分别为飞燕草素（纯度98.2%）、矢车菊素（纯度96.3%）、牵牛花素（纯度92.6%）、锦葵色素（纯度90.5%）。本研究可为花色苷元的规模化制备及后期功能活性研究提供技术参考和依据。     

大孔树脂吸附法纯化紫薯花色苷的研究

目的研究大孔吸附树脂吸附法纯化紫薯花色苷成分。方法采用大孔吸附树脂静态和动态吸附解吸实验,结合花色苷p H示差法检测技术,分别考察了D101、AB-8、XDA-7、HPD-722、HPD-750、HPD-450、XDA-6、NKA-II、NKA9和S-8 10种吸附树脂对紫薯花色苷的吸附和洗脱性能,探讨大孔树脂柱层析纯化工艺。结果 XDA-7大孔吸附树脂对紫薯花色苷的吸附和洗脱性能较好。吸附过程中上样液浓度为450 mg/L,样液p H为4.0,上样速率为1 BV/h,树脂的饱和吸附容量为10.2 mg/g;洗脱液为60%乙醇溶液,洗脱速率为2BV/h时,洗脱解析率在94%以上,纯化效果较好。结论 XDA-7大孔吸附树脂可用于紫薯花色苷的纯化应用,该纯化分离工艺简单快速,适合紫薯类花色苷的纯化制备。