大孔吸附树脂分离纯化蛹虫草固体培养基中虫草素工艺

比较D101、AB-8、HPD-100、HPD-400、HPD-500、HPD-722、DM130七种大孔吸附树脂对蛹虫草固体培养基中虫草素的吸附与解吸性能,筛选出HPD-100树脂为最佳树脂,并确定HPD-100树脂吸附分离最佳工艺条件：上样液质量浓度0.6mg/mL、上样流速3BV/h、上样体积6BV;解吸剂为体积分数25%乙醇溶液、解吸流速2BV/h、解吸体积4BV。根据此工艺条件,蛹虫草固体培养基粗提物经HPD-100树脂纯化后,虫草素产品纯度可达14.1%,较粗提物产品提高了8倍多。     

大孔树脂法纯化陕产重楼总皂苷工艺研究

研究陕产重楼中总皂苷利用大孔吸附树脂纯化的最优工艺。应用7种大孔吸附树脂吸附重楼中的总皂苷进行静态实验,筛选得到最佳树脂;通过动态实验确定最佳树脂对重楼总皂苷的纯化的最优工艺参数。结果表明,HPD-400A树脂纯化重楼总皂苷的效果最优,最优工艺条件为上样液质量浓度5mg/mL,上样量8BV,流速3BV/h,解吸流速2BV/h,解吸剂体积分数75%的乙醇,洗脱剂用量4BV,按此工艺条件制备的重楼总皂苷的含量为62.68%;Freundlich等温吸附模型可更好的描述树脂对重楼总皂苷的吸附,采用HPD-400A树脂分离纯化陕产重楼中的总皂苷效果较好。     

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。     

大孔吸附树脂纯化八角枫根中水杨苷工艺

研究大孔树脂纯化八角枫根中水杨苷的最佳工艺条件。以水杨苷的吸附率和解吸附率为评价指标,筛选树脂种类,并优化吸附和洗脱条件。8种大孔吸附树脂中,HPD-826型大孔树脂对水杨苷具有较好的吸附分离性能,最佳的纯化工艺条件为上样液质量浓度45.12μg/mL、最大上样量6.5BV、径高比1:8、洗脱流速3BV/h,先用4BV的水洗柱除去水溶性杂质,再用5BV体积分数30%乙醇溶液洗脱。经HPD-826型大孔树脂处理后的水杨苷回收率可达78%左右,HPD-826大孔树脂对水杨苷纯化的综合性能较好,工艺稳定、可行,适合于工业化生产。     

马兰头总黄酮的大孔树脂纯化工艺优化

目的利用大孔树脂来纯化马兰头中粗黄酮,并确定纯化黄酮的最佳工艺。方法以黄酮回收率为指标,在单因素实验的基础上运用Box-Behnken响应面法(response surface methodology,RSM)设计三因素三水平实验以获得最佳纯化条件。结果 HPD-600大孔吸附树脂纯化马兰头粗提液的最佳工艺条件为:上样浓度0.93 mg/mL、上样pH为3.00、洗脱剂体积分数为84.17%、吸附速率1 BV/h,洗脱速率1 BV/h,此条件下马兰头总黄酮的质量分数由纯化前的4.11%提高到纯化后的50.80%。结论利用HPD-600型大孔树脂可以较好地纯化马兰头中的总黄酮。     

大孔吸附树脂法纯化槐米总黄酮的研究

对大孔吸附树脂纯化槐米总黄酮的工艺进行了研究.方法是采用优选树脂纯化槐米总黄酮,以分光光度法测定槐米总黄酮含量.结果表明AB-8树脂吸附与纯化槐米总黄酮的效果较好,其工艺参数为:原液上样质量浓度为2.802mg/mL,最大吸附量为30.8mg/g,吸附速度为1 BV/h,上样2次,吸附时间为1 h,洗脱剂为45%乙醇,用量为3BV,洗脱速度为4BV/h,且树脂可重复使用3次.     

明日叶总黄酮的纯化工艺研究

采用静态-动态吸附与解析相结合的方法,从12种树脂中筛选出纯化明日叶总黄酮最佳的树脂并对其纯化工艺条件进行探讨。结果表明:HPD-600大孔树脂对明日叶总黄酮有较好的吸附、解析效果。最佳纯化条件为:上柱液中总黄酮质量浓度控制在2 mg/m L~3 mg/m L之间,以3 BV/h的流速过柱,树脂达吸附饱和的上样量为2.7 BV;洗脱条件为:用蒸馏水冲洗至无色后,改用4 BV,50%乙醇以2 BV/h流速进行洗脱。经HPD-600树脂纯化后,明日叶总黄酮的纯度由14.46%提升至46.96%,提升近3.2倍。     

辣椒精中辣椒碱类化合物的纯化方法

辣椒中辣椒红素提取后产生大量的副产物辣椒精,为提高辣椒资源的综合利用,本研究以辣椒精为原料,采用低浓度乙醇萃取-离子交换树脂纯化-重结晶联用的方法制备辣椒碱类化合物。研究采用正交实验设计对低浓度乙醇萃取法的工艺进行优化,采用单因素实验方法对D201树脂纯化法和重结晶法的工艺进行优化,最后采用气-质联用法(GC-MS)对纯化效果进行评价。研究表明低浓度乙醇萃取的最佳工艺为:乙醇浓度50%、料液比1∶30、萃取时间20min;D201树脂纯化的最佳工艺为上样液浓度8.45mg/m L、上样量4倍柱体积(BV)、上样速度1.5BV/h,解吸液浓度70%乙醇、解吸液p H4、解吸速度3BV/h,解吸液用量20.5BV,得辣椒碱类化合物的解吸率为70.72%;重结晶的最佳工艺为结晶溶剂水、结晶p H11.32、结晶温度20℃。GC-MS分析结果表明,纯化后晶体中的辣椒碱类化合物含量约为原料中的2.11倍,其中辣椒碱的相对含量为62.00%、二氢辣椒碱的相对含量为34.84%。该纯化工艺获得了较好的纯化效果,并有效降低了辣椒碱类化合物的制备成本、提高产品的安全性。     

大孔树脂对木瓜酒单宁的吸附性能研究

以木瓜酒中单宁含量为指标,通过静态吸附试验从5种大孔树脂中筛选出HPD-100树脂,其吸附容量为每克干树脂吸附72.15 mg单宁.考察HPD-100树脂的吸附、解吸效果及其影响因素.结果表明,吸附最佳条件为pH6 0,静态吸附4h;动态吸附流速为2.0 BV/h,吸附体积达到5 BV时为吸附终点,吸附率为89.5％.静态解吸附最佳条件为洗脱液pH 7.0,洗脱时间6h,洗脱乙醇浓度75％;动态解吸附流速为1.0BV/h,解吸附体积达到1.6 BV时为解吸附终点,解吸附率为68.6％.HPD-100大孔吸附树脂对木瓜酒单宁具有良好富集作用,适于木瓜酒涩味的去除或单宁的分离纯化.     

利用大孔树脂吸附纯化头花蓼总多酚工艺的研究

采用Folin-Ciocalteu比色法测定多酚含量,研究10种大孔树脂对头花蓼总多酚的吸附和解吸效果,筛选出适合分离纯化头花蓼总多酚的树脂,并以总多酚的吸附率和解吸率为指标对HPD-722纯化头花蓼总多酚的工艺进行了研究。结果表明:HPD-722为纯化头花蓼总多酚的最佳树脂。确定其最佳工艺条件为:上样浓度控制在2.0~4.5 mg/mL,上样流速2BV/h,用体积为7.5BV的50%乙醇溶液集中洗脱。纯化后总多酚的含量可达到59.02%。     

茶叶中有效成分综合提取的研究

以绿茶为原料，采用ZJL大孔离了交换树脂和ZJX大孔吸附树脂从茶叶的浸提液中提取茶氨酸、咖啡因、茶多酚和茶多糖。通过对树脂的静态、动态吸附性能的实验研究，确定了咖啡因、茶氨酸、茶多酚及茶多糖联合分离提取的工艺。研究结果表明：该工艺能有效的从茶叶中提取咖啡因、茶氨酸和茶多酚，提取的咖啡因纯度达83．23％，提取率为1．9％，茶氨酸纯度达85．43％，提取率为0．94％，提取的茶多酚纯度达95．62％，提取率为12．35％，且茶多酚中的咖啡因含量低于0．7％，茶多糖的纯度达51％，提取率为1．1％。     

大豆异黄酮精制工艺研究

试验比较10种不同型号大孔树脂对大豆异黄酮吸附性质和不同溶剂萃取大豆异黄酮效果,确定HPD-600树脂吸附纯化大豆异黄酮最佳工艺条件如下:上样液浓度0.15mg/mL、上样液pH值4～5、上样量4.5BV、吸附流速1.0ml/min、静态吸附250min,用80%乙醇作为解吸剂,解吸流速为0.5ml/min,3.0BV解吸剂即可解吸完全。得到大豆异黄酮粗品含量为20.11%,比粗提物纯度提高7.18倍;同时得出丙酮沸点回流萃取可得到含量为42.91%大豆异黄酮产品,纯度比含量为20.11%原料提高2.13倍;乙酸乙酯和丙酮组合沸点回流萃取,可得到含量为70.36%大豆异黄酮产品,纯度比含量为42.91%原料提高1.64倍。     

荷移光度法测定茶及茶饮料中茶氨酸含量

通过实验得到了适宜茶氨酸测定的荷移剂--四氯苯醌,并对四氯苯醌荷移光度法测定茶氨酸的条件进行探讨。最佳测定条件为：茶氨酸水溶液与四氯苯醌乙醇溶液反应,温度50℃,pH8～9,时间50min,能得到n茶氨酸:n四氯苯醌=2:1 的紫红色荷移络合物,其稳定常数K(293K)= 3.9 × 103,Gibbs 自由能ΔrGm(293K)= － 20.14 kJ/mol;在工作波长λ=331nm 处,表观摩尔吸光系数ε = 1.98 × 104 L/mol·cm,在5 × 10-6～9 × 10-5 mol/L 内符合比尔定律,线性方程为A=0.028 × 10-6C － 0.02 (r=0.9958)。该法对市售的茶叶和茶饮料中茶氨酸含量测定的结果与HPLC法一致,回收率在98.7%～102.6% 内,RSD 为1.2%～4.2%。此方法操作容易掌握,灵敏度高,结果较为满意,但样品的预处理稍繁琐。     

Changes in theanine and caffeine contents of black tea with different rolling methods and processing stages

Theanine is a specific amino acid in tea, which has positive effects on health. Theanine contents of different grade Turkish teas, variations in the theanine content during tea processing, and the effects of different rolling processes on theanine content were determined. Theanine content of Turkish tea varying between 0.32 and 0.43 % has been reported for the first time by this study. Theanine content decreased in all processing steps from 10.0–3.42 to 7.73–3.97 mg g^?1 dw in Orthodox and Cay-Kur methods, respectively. In both methods, the highest theanine loss (almost 50 %) was observed in the withering step, which was followed by drying step. Caffeine content of Turkish tea was determined varying between 1.8 and 2.2 %. While the caffeine content increased in the withering step, it decreased in other steps. The correlation between theanine and caffeine contents was evaluated. A high correlation (R ² = 0.87) between the caffeine and theanine contents was found in teas classified by Cay-Kur method, and caffeine/theanine ratio was found to be around 5.3 in general.     

Column-chromatographic extraction and separation of polyphenols, caffeine and theanine from green tea

A highly efficient column-chromatographic extraction (CCE) followed by sequential adsorption to extract and separate bioactive compounds from green tea was developed. Tea powder was loaded into columns with 4-fold solvents and eluted through a cyclic CCE. High-quality tea extracts with greater than 90% extraction efficiencies of polyphenols, epigallocatechin-3-gallate, caffeine, theanine and polysaccharides were obtained with 4-fold water circulated five times among different columns at 70 °C. Similar results, except for low polysaccharide extraction (35.5%), were obtained with 4-fold 30% ethanol circulated three times at room temperature. The highly concentrated water extraction was directly passed through columns of polyamide, DM130 macroporous and 732 ion exchange resins, resulting in high-purity polyphenols (99%), caffeine (98%) and theanine (98%) after simple purification of the eluates from each column. This method uses simple equipment, minimum solvents and can be used for both quantitative analysis and continuous preparation of high-quality tea extracts and bioactive compounds.     

离子交换树脂分离合成茶氨酸

采用离子交换树脂法取代常规的醇沉法分离、纯化合成的茶氨酸粗品。以732型阳离子交换树脂为分离材料,探讨了上样浓度、洗脱液浓度、pH对茶氨酸分离效果的影响,比较离子交换法和乙醇沉淀法对合成茶氨酸粗品的分离效果。结果表明:上样液中茶氨酸的最佳质量浓度为4mg/mL,最佳洗脱液(氨水)浓度为0.4mol/L,茶氨酸在pH=8～11时被解吸。当茶氨酸纯品进样量为200mg,流速为1mL/min,完全洗脱茶氨酸时,约需0.4mol/L氨水50mL,即需0.25mL0.4mol/L氨水/mg茶氨酸。当产品质量分数相近且≥95%时,离子交换法比乙醇沉淀法的产率高25%以上。使用阳离子交换树脂分离合成茶氨酸,大大提高了产品的纯度和得率。     

罗望子果实黄酮类物质的提取纯化工艺

为了筛选出罗望子果实中黄酮类化合物的最佳分离纯化工艺,本文了采用正交设计试验筛选罗望子果实中黄酮类化合物的提取的最佳工艺.结果表明罗望子果实中黄酮类化合物最佳提取工艺为:使用75%乙醇溶液按1:30的料水比进行加热,在80℃恒温下2h回流提取,重复2次.罗望子果实中粗黄酮的进一步的精制方法为醇沉法和Diaion HP-...     

Effects of aqueous brewing solution pH on the extraction of the major green tea constituents

The pH of the aqueous brewing solution was maintained at values ranging from 1 to 9 during the green tea extraction and the effects on the tea's extracted constituents were studied. The epistructured catechins were stable under acidic conditions but epimerized or degraded at pH ≥ 6. The extractable solids contained more epistructured catechins at pHs 3–5 but more non-epistructured catechins at pHs 6–7. More tea cream was obtained at pH 1 but the concentration of catechins, caffeine and theanine was low in this fraction. Therefore, to maximize the extraction of the epistructured catechins and to minimize their epimerization and degradation and to maximize the extraction of caffeine and theanine, the results suggest that the pH should be maintained between 3 and 5.3 during the aqueous brewing process.     

Microwave-assisted extraction of chlorogenic acids from green coffee beans

Microwave-assisted extraction (MAE) has been considered as a potential alternative to conventional solvent extraction for the isolation of phenolic compounds from plants. Aqueous and alcoholic extracts of green coffee bean obtained by MAE were quantitatively analysed for total yield of extracts, chlorogenic acids, caffeine and total polyphenol content. The extracts were also evaluated for radical-scavenging activity, using 1,1-diphenyl-β-picrylhydrazyl radical. Under optimum conditions of time (5 min), temperature (50 °C) and wattage (800 W), the maximum chlorogenic acids and caffeine could be extracted with water as solvent. The extracts contained chlorogenic acids and caffeine in the ranges of 31–62% and 22–40%, respectively. The yields of MAE under optimum conditions were higher than those from the conventional solvent extraction at 5 min and 50 °C and the extracts showed radical-scavenging activity of >75%, even at the concentration of 25 ppm. The MAE process can thus be predicted and controlled for industrial application.     

离子交换吸附分离茶氨酸的研究

本实验以目前工业上生产茶多酚后的废茶水为原料,通过超滤、脱色等预处理后,通过离子交换树脂对茶氨酸进行吸附分离,探索从其中分离制备茶氨酸的工艺。选用001×7阳离子交换树脂,分析了影响茶氨酸交换容量的因素,并对树脂吸附茶氨酸的动力学进行了研究。通过响应面分析法确定固定床离子交换工艺中合适的吸附工艺条件为:pH值为3.4,上样液浓度为3.0mg/ml,上样流速为1.7柱床体积/h。最后确定洗脱工艺条件,用pH11.3的氨水洗脱后得到茶氨酸含量为58%,离子交换过程中茶氨酸的回收率为82%。