大孔吸附树脂对沙棘叶总黄酮的吸附性能考察

以吸附值(mg/g)和解吸附率(%)为评价指标,通过静态吸附/解吸附分别考察LSA-40、LSA-21、DM-130、HPD450、D101和XDA-1六种大孔吸附树脂对沙棘叶总黄酮的吸附/解吸附性能。通过动态吸附/解吸附优选沙棘叶总黄酮最佳分离工艺条件。结果表明中极性树脂LSA-21在吸附/解吸附方面显示出最佳的综合性能,对沙棘叶总黄酮的静态吸附值/解吸附率分别为131.78mg/g和55.53%,经静态和动态吸附后得到的总黄酮纯度分别为19.4%和20.3%。     

虎尾草黄酮类化学成分研究

对虎尾草药材地上部分用70%乙醇提取后,以大孔吸附树脂、聚酰胺和硅胶等分离材料进行分离和纯化,从中分得10个黄酮类化合物,利用氢谱、碳谱、质谱和颜色反应等手段对其结构进行确认,10个化合物依次为槲皮素(Ⅰ)、山奈酚(Ⅱ)、异鼠李素(Ⅲ)、槲皮素-3-O-β-葡萄糖苷(异槲皮苷)(Ⅳ)、槲皮素-3-O-α-L-鼠李糖苷(槲皮苷)(Ⅴ)、山奈酚-3-O-β-D-葡萄糖苷(Ⅵ)、山奈酚-3-O-β-D-半乳糖苷(Ⅶ)、金丝桃苷(Ⅷ)、异鼠李素-3-O-β-D-芸香糖苷(Ⅸ)和芦丁(Ⅹ),其中化合物Ⅴ、Ⅵ为首次从该植物中分离得到,化合物Ⅲ、Ⅸ为首次从该属植物中分离得到。     

大孔树脂吸附法吸附分离黄酮的研究

研究了D101、LD601、LS-303B、LX-28、LX-38型大孔树脂对黄酮的吸附及分离性能。结果表明,LD601型大孔树脂对黄酮的吸附效果较好,pH 2～4的盐酸溶液中,静态吸附量为5 849.312μg/g,对流速2 mL/min黄酮溶液的吸附率可达96.27%,负载1 500μg黄酮的LD601树脂,用40%乙醇50 mL以3 mL/min流速进行解吸,解吸率可达97.51%。     

沙棘叶黄酮糖苷生物转化黄酮苷元研究

沙棘叶中的黄酮类化合物主要以糖苷形式存在,现采用酶法水解糖苷中的糖基使其变成苷元,提高抗氧化活性.沙棘黄酮糖苷经过α-鼠李糖苷酶(1 IU)、β-葡萄糖苷酶(2 IU)、木聚糖酶(1.5 IU)、纤维素酶(15 IU)、果胶酶(0.5 IU)、α-淀粉酶(2 IU)组成的复合酶预处理后,黄酮糖苷转化率仅为0.23%,再用柚苷酶水解可获得高含量的黄酮苷元,转化率达85%以上,其中槲皮素占总黄酮苷元的23.31%,异鼠李素占35.11%,山奈酚占9.95%.沙棘黄酮苷元不易溶于水而溶于乙醇.     

不同大孔树脂吸附-解吸附喜树黄酮性能的研究

采用静态吸附和解吸方法研究了AB-8、D-101、X-5、H-103、YWD-03五种大孔树脂对喜树叶黄酮的吸附与解吸性能,结果表明,AB-8树脂对喜树叶黄酮的吸附分离综合性能最佳,中性条件下其静态吸附率为85.54%,最大解吸率高达98.75%以上。     

大孔吸附树脂纯化黄花蒿黄酮及其抗氧化活性

该文对大孔吸附树脂纯化黄花蒿黄酮的工艺条件进行了研究与优化,并对纯化后的黄酮进行了抗氧化活性的研究。比较了AB-8,DM-101,DA-201,D-101及SD-401对黄花蒿中黄酮类物质的吸附及解吸附性能,结果显示,D-101的综合效果最佳。通过D-101大孔吸附树脂动态吸附解吸实验,获得较佳的纯化工艺:上样液黄酮质量浓度为1.55 g/L,流速为2 mL/min,上样100 mL后,用蒸馏水洗脱至溶液无色,再用250 mL体积分数70%乙醇以1 mL/min洗脱。在该条件下,黄酮质量分数从20.10%提高到80.32%,洗脱率达91.08%,黄酮回收率为68.25%。黄花蒿黄酮对油脂有明显的抗氧化性作用;黄花蒿黄酮对植物油的抗氧化能力强于柠檬酸和抗坏血酸,对动物油脂的抗氧化能力稍弱于抗坏血酸而略强于柠檬酸。     

大孔树脂吸附分离丹参提取液中丹酚酸B的工艺研究

对国内几种大孔吸附树脂的丹酚酸B吸附性能进行了实验筛选。结果表明。YWD06树脂有较好的吸附和洗脱能力;适宜吸附条件:pH控制在4～5、流速为2BV/h;以70%乙醇为洗脱剂,pH=5、流速为3BV/h时,洗脱效果好。     

HPD-100大孔吸附树脂与聚酰胺吸附黄酮的对比研究

对比研究了HPD-100大孔吸附树脂与聚酰胺吸附树脂对总黄酮的静态和动态吸附性能,考察影响吸附的主要因素。结果表明,Freundlich等温方程较Langmuir等温方程更适宜描述树脂对总黄酮的吸附,聚酰胺树脂的方程拟合更好。黄酮溶液的浓度及流速对HPD-100的吸附影响不大,吸附率均高达90%以上,相同条件下,聚酰胺树脂只有其80%左右。而解吸剂流速对HPD-100解吸的影响则相反,只有聚酰胺树脂的80%左右。两种树脂对于黄酮的吸附解析总过程无明显差异。     

HPD-100大孔吸附树脂与聚酰胺吸附黄酮的对比研究

对比研究了HPD-100大孔吸附树脂与聚酰胺吸附树脂对总黄酮的静态和动态吸附性能,考察影响吸附的主要因素。结果表明,Freundlich等温方程较Langmuir等温方程更适宜描述树脂对总黄酮的吸附,聚酰胺树脂的方程拟合更好。黄酮溶液的浓度及流速对HPD-100的吸附影响不大,吸附率均高达90%以上,相同条件下,聚酰胺树脂只有其80%左右。而解吸剂流速对HPD-100解吸的影响则相反,只有聚酰胺树脂的80%左右。两种树脂对于黄酮的吸附解析总过程无明显差异。     

大孔树脂吸附分离丹参提取液中丹酚酸B的工艺研究

对国内几种大孔吸附树脂的丹酚酸B吸附性能进行了实验筛选。结果表明。YWD06树脂有较好的吸附和洗脱能力;适宜吸附条件：pH值控制在4-5、流速为2BV/h;以70%乙醇为洗脱剂,pH值=5、流速为3BV/h时,洗脱效果好。     

Preparative Separation of Glabridin from Glycyrrhiza glabra L. Extracts with Macroporous Resins

Abstract

In the present study, the performance and adsorption characteristics of five macroporous resins for the separation of glabridin from Glycyrrhiza glabra L. have been evaluated. The adsorption and desorption properties of glabridin on macroporous resins including HPD100, HPD300, HPD800, NKA and H103 were compared. HPD100 resin offered the best adsorption and desorption capacities based on the research results. Both Langmuir and Freundlich isotherms were used to describe the interactions between the solutes and resins at different initial concentrations. Dynamic adsorption and desorption experiments on HPD100 resin packed column were conducted to optimize the separation process of glabridin from licorice extracts. After the treatment with stepwise elution on HPD100 resin, the content of glabridin in the product increased from 0.21% to 32.2% which is 153-fold higher than it in G. glabra L. roots and the recovery yield was 79.7%. The results indicated the good ability of HPD100 resin for separation glabridin and the study may provide scientific references for the large-scale glabridin production from G. glabra L. or other plants extracts.     

对硝基酚在几种树脂上的吸附性能研究

研究了对硝基酚在四种吸附树脂(AM-1、NDA-88、NDA-99、NDA-150)上的静态吸附行为,结果表明,NDA-88、NDA-99、NDA-150三种吸附树脂对对硝基酚的吸附效果比较好。并研究了NDA-99树脂的动态吸附和脱附行为,结果显示,对硝基酚在NDA-99树脂上的吸附量为3.75 mmol/g。该树脂吸附对硝基酚后,容易脱附。用2mol/L NaOH∶C2H5OH(体积比1∶1)作脱附剂,温度328 K,体积为2.5倍树脂体积时,脱附率93%。     

大孔树脂对桃金娘叶总黄酮的静态吸附性能研究

分别研究了X-5和AB-8两种不同树脂对桃金娘叶总黄酮的静态吸附和解吸性能。结果表明,X-5树脂具有较好的吸附和解吸参数,是一种分离纯化桃金娘叶总黄酮较好的树脂,其最佳条件为温度为25℃、吸附时间为6 h、黄酮原液pH=6时,吸附率最大,为66.07%,此时选用95%的乙醇做解吸剂,于30℃温度下解吸12 h时,解吸效果最佳。     

Enrichment and Purification of Syringin, Eleutheroside E and Isofraxidin from Acanthopanax senticosus by Macroporous Resin

In order to screen a suitable resin for the preparative simultaneous separation and purification of syringin, eleutheroside E and isofraxidin from Acanthopanax senticosus, the adsorption and desorption properties of 17 widely used commercial macroporous resins were evaluated. According to our results, HPD100C, which adsorbs by the molecular tiers model, was the best macroporous resin, offering higher adsorption and desorption capacities and higher adsorption speed for syringin, eleutheroside E and isofraxidin than other resins. Dynamic adsorption and desorption tests were carried out to optimize the process parameters. The optimal conditions were as follows: for adsorption, processing volume: 24 BV, flow rate: 2 BV/h; for desorption, ethanol-water solution: 60:40 (v/v), eluent volume: 4 BV, flow rate: 3 BV/h. Under the above conditions, the contents of syringin, eleutheroside E and isofraxidin increased 174-fold, 20-fold and 5-fold and their recoveries were 80.93%, 93.97% and 93.79%, respectively.     

微波法合成硫脲树脂及其吸附性能研究

研究了硫脲、甲醛、对苯二酚的聚合,比较了微波辐射和常规加热对树脂产率的影响,考察了不同条件下树脂对金属离子的吸附情况。用核磁共振和红外光谱对树脂可能含有的官能团进行表征。结果表明:微波辐射与常规加热相比具有反应时间短、产率高的优点。酸性条件下树脂对Ag 的最高吸附量可达2.2mmolg-1,而相同条件下对Ni2 、Cd2 、Co2 等过渡金属离子基本不吸附,体现了该树脂在对金属离子的选择分离方面有较高的应用价值。利用含8%硫脲的1molL-1HNO3溶液洗脱经吸附过的树脂,洗脱率可达95%以上,再生的树脂吸附量仍可达到前一次的98%。     

大孔树脂对贯叶连翘中金丝桃素的静态吸附

考察了18种不同类型的大孔树脂对贯叶连翘中金丝桃素的静态吸附和解吸效果,并对3种效果较好的树脂进行了吸附动力学研究;比较了上样液pH对吸附效果的影响;探讨了NKA-9树脂在25℃等温吸附过程,并应用Langmuir方程进行了拟合。结果表明,弱极性树脂NKA-9对金丝桃素吸附解吸作用最好,到达吸附平衡时间为1h左右,吸附量可达12.45mg/g干树脂。上样液最佳pH=4,上样液pH对树脂的吸附有很大影响。NKA-9树脂对金丝桃素的吸附为单分子吸附,符合Langmuir吸附理论。     

Separation of Monascus pigments from extractive fermentation broth with a high concentration of triton X-100

ABSTRACT

In this study, Monascus pigments were separated from the extractive fermentation broth by the combination of reverse micellar extraction and macroporous resins (MACR) adsorption with the alkalizing S-8 MACR (S-8 ALR). A 95.07% pigment adsorption was achieved together with a relative low Triton X-100 co-adsorption that was only 2.53%. The liquid intraparticle diffusion and film diffusion limit the pigment adsorption rate. A 79.48–84.03% of the pigment could be eluted from the resin using the methanol solution containing a 0.5% (w/v) hydrochloric acid. The S-8 ALR could be recovered for cycle use without a deficit of the adsorption or desorption efficiency.

Abbreviations: ACR—Acidified resin; ALR—Alkalizing resin; HPLC—High performance liquid chromatography; PSM—pigment- surfactant micelle; TEM—Transmission electron microscopy.     

Preparation of high purity squalene from soybean oil deodorizer distillate with the combination of macroporous resin and thin-film evaporation coupling distillation

ABSTRACT

In this study, the combination of macroporous adsorbent resins (MARs) and thin-film evaporation coupling distillation (TFECD) was studied systematically, with aim to obtain high value-added squalene from soybean oil deodorizer distillate (SODD). Five types of resins (X-5, D-101, D4020, DM301, and AB-8) were first used to evaluate the adsorption/desorption properties of squalene. D101 resin exhibited higher adsorption/desorption capacities and desorption ratios for squalene based on static adsorption results among the tested resins. We further investigated the adsorption kinetics, isotherms, and thermodynamics with D101 resin as adsorbent. The adsorption of squalene on D101 was best fitted to pseudo-second-order kinetic model and the Langmuir equation. The dynamic adsorption and desorption indicated that similar results were observed in the static adsorption test. The purity of squalene was increased from 7.5 to 82.5% with the recovery up to 88.5% after separation on D101 column. The resin-refined sample was directly subjected to TFECD purification. Under optimized process parameters, the final product with purity of 98.5% and recovery yield of 76.5% was confirmed by high-performance liquid chromatography (HPLC) analysis. The present study provided an effective method for large-scale production of high purity squalene.