反相高效液相法测定穿心莲药材及其制剂中的穿心莲内酯和脱水穿心莲内酯

 发展了穿心莲药材及其中成药中两种主要成分穿心莲内酯和脱水穿心莲内酯的反相高效液相测定方法。采用甲醇振荡提取法进行样品前处理 ,在以乙腈 水为流动相作梯度洗脱、ODS柱、检测波长为 2 2 5nm的条件下 ,穿心莲内酯和脱水穿心莲内酯在 1 5min内可达到基线分离。两种内酯在 1 0mg/L～ 1 0 0mg/L时其浓度与峰面积成良好的线性关系 ,加标回收率为 96 %～ 1 0 4 %。     

阿尔泰狗哇花总皂苷的提取与纯化

对阿尔泰狗哇花总皂苷的提取与纯化工艺进行了研究.利用正交设计确定了提取温度、乙醇浓度、溶剂用量、时间及次数等提取工艺参数.比较了五种大孔吸附树脂和聚酰胺树脂对阿尔泰狗哇花总皂苷的吸附与脱附性能.结果表明,在优化的提取条件下提取,经AB-8大孔吸附树脂柱层析分离纯化,制得总皂苷产品,其含量比原药材提高约7倍多,进一步完善后可适用于工业化生产.     

大孔吸附树脂提取麦拓莱霉素的工艺研究

研究了用大孔吸附树脂从发酵液中分离提取新型大环内酯类抗生素-麦拓莱霉素的吸附工艺过程，对吸附条件进行了优化，得到了适宜的操作条件．结果表明：NKA树脂为最佳吸附剂：吸附最佳pH值为10．32；吸附流速选择为1ml／min；NaCl的加入对吸附不利，选择NaCl浓度为0．6％左右，本实验条件下，发酵液中的麦拓莱霉素浓度为0．18mg／ml；NKA的吸附量可达33．7mg／g树脂。     

大孔吸附树脂对紫草宁的吸附性的研究及从细胞培养液中提取紫草宁的 …

以配制的紫草宁水溶液为对象，研究了大孔吸附树脂提取水溶液中紫草宁的方法，包括树脂的筛选，紫草宁的浓度，溶液ｐＨ及盐离子浓度对吸附的影响；解吸剂的选择，确定了适宜的吸附和解吸条件。最后，采用真实的细胞培养体系进行间歇的边培养边吸附分离研究，紫草宁产率提高了７６．４％，为今后实现细胞培养与分离相耦合的连续化操作提供充分的准备工作。     

微乳液毛细管电动色谱法快速测定消炎利胆片中的穿心莲内酯和脱水穿心莲内酯

建立了微乳液毛细管电动色谱同时分析消炎利胆片中穿心莲内酯和脱水穿心莲内酯的方法。考察了缓冲溶液的浓度、pH值、十二烷基硫酸钠(SDS)以及助表面活性剂的含量对分离测定的影响。在由乙酸乙酯-SDS-正丁醇-30 mmol/L硼砂缓冲液(pH 9.5)（质量比为0.5∶0.6∶6.0∶92.9）组成的微乳液体系中,两种内酯在6 min内完成分离。该法简便、快速、选择性好,用于实际样品中穿心莲内酯和脱水穿心莲内酯的分析,获得了满意的结果。     

胶束电动毛细管色谱法测定穿心莲中穿心莲内酯和脱水穿心莲内酯

采用胶束电动毛细管色谱法分离测定了中药穿心莲中穿心莲内酯和脱水穿心莲内酯。电泳条件 :以2 0mmol L磷酸缓冲溶液 1 0mmol LSDS(含 5 %甲醇 ,V/V ,pH 6.8)为电泳介质 ,未涂层石英毛细管 (75 μmi.d.× 5 0cm ,有效分离长度 4 2 .2cm)为分离通道 ,压力进样 (2 5 0kPa·s) ,2 0kV恒压电泳 (2 5℃ )分离 ,检测波长 2 4 0nm。在 1 0 .4～93 .5mg/L ,和 1 0 3～ 92 .7mg L范围内 ,对两种内酯分别进行了定量分析。加样回收率穿心莲内酯为 1 0 2 % ,脱水穿心莲内酯为 1 0 2 %。     

两个穿心莲内酯苷的波谱学研究

利用柱色谱对穿心莲地上部分的提取物进行分离,得到3,14-二去氧穿心莲内酯苷和14-去氧穿心莲内酯苷。利用核磁共振氢谱(1H-NMR)、碳谱(13C-NMR)以及双量子滤波相关谱(DQFCOSY)、总相关谱(TOCSY)、异核多量子相干谱(HMQC)、异核多键相关谱(HMBC),解析这两个化合物的结构。确定了1H-NMR的氢信号和13C-NMR的碳信号的归属,并且用NOESY对3,14-二去氧穿心莲内酯苷的立体结构进行了研究。     

PYR树脂对甜菊糖的吸附与洗脱性能研究

系统研究了PYR型树脂对甜菊糖的吸附与洗脱性能，并与目前国内应用于甜菊糖提取分离的某些商品化吸附树脂进行了比较。结果表明，PYR树脂比其它树脂具有更优的性能，其静态吸附容量比AB—8树脂提高25％，且吸附速度快，易于洗脱再生，是一种具有工业化应用前景的新型吸附剂。     

大孔吸附树脂技术应用于复方中成药制备工艺的研究

本文报告了用非极性大孔吸附树脂法从复方中药中提取分离有效成分的研究。结果表明，正确地选择大孔吸附树脂及吸附和解吸条件，可得到高纯度的有效组分，其粘度低，有利于制剂。     

胶束毛细管电泳在线扫集技术同时分离测定穿心莲内酯和脱水穿心莲内酯的研究

采用胶束毛细管电泳在线扫集技术分离测定了中药穿心莲中脱水穿心莲内酯和穿心莲内酯.电泳条件:以20 mmol/L H3BO310 mmol/L NaH2PO4-50mmol/L SDS(含体积分数20%甲醇,pH 2.4)为电泳运行缓冲溶液,未涂层石英毛细管(58 cm×50 μm i.d.,有效长度为41.2 cm)为分离通道,重力进样,进样高度为11 cm,-20 kV恒压,检测波长为246 nm.富集倍数可以达到200倍以上.在5.70～91.20 mg/L,和3.96～31.68 mg/L范围内呈良好的线性关系,对两种内酯分别进行了定量分析.加标平均回收率脱水穿心莲内酯为100.80%,穿心莲内酯为98.06%.     

ADSORPTION OF DINITROPHENOLS ONTO POLYMERIC ADSORBENTS AND ITS MECHANISM

The adsorption of 2,4-dinitrophenol and 2,6-dinitrophenol on non-polar and polar adsorbents was studied.The results showed that the equilibrium adsorption did not comply with the Langmuir equation and was not mono-layer adsorption .It is of interest to notice that the effect of pH on the adsorption of 2,4-or 2,6-dinitrophenol onto ADS-7 and ADS-21 was very small,The result is explained by hydrogen bonding interaction between 2,4-or 2,6-dinitrophenol and the adsorbent ADS-21.The large adsorption capacity of dinitrophenol onto ADS-21,which was about 500mg/g at an equilibrium concentration of 400mg/L,and the small dinitrophenol leakage in the effluent from ADS-21 column presented a good prospect for treatment of wastewater containing dinitrophenol with adsorbent ADS-21.     

ADSORPTION OF DINITROPHENOLS ONTO POLYMERIC ADSORBENTS AND ITS MECHANISM

1 INTRODUCTIONPhenol and many substitUted phenols, such as nitrophenols, chlorophenols and aminophenolset al, are the common organic pollutantS existing in wane water of many chemical plants.Treatment of the wastewater containing phenols is an important project for environmentprotection and has been studied by various methods, such as dialysis ['l, microbial degradation ['1,oxidation l'l, extracting with solvents I4] and adsorption with polymeric adsorbents IS]. Theadsorption method is v…     

Preparative separation of vitexin and isovitexin from pigeonpea extracts with macroporous resins

Vitexin and isovitexin are a pair of isomeric compounds known as the major constituents in pigeonpea leaves and possess various pharmacological activities. In the present study, the preparative separation of vitexin and isovitexin with macroporous resins (Nankai Hecheng S & T, Tianjin, China) was studied. The performance and adsorption characteristics of eight macroporous resins including ADS-5, ADS-7, ADS-8, ADS-11, ADS-17, ADS-21, ADS-31 and ADS-F8 have been evaluated. The research results indicate that ADS-5 resin is most appropriate for the separation of vitexin and isovitexin. Langmuir and Freundlich isotherms were used to describe the interactions between solutes and resin at different temperatures, and the equilibrium experimental data were well fitted to the two isotherms. Column packed with ADS-5 resin was used to perform dynamic adsorption and desorption tests to optimize the separation process. The optimum parameters for adsorption were as follows: the concentration of vitexin and isovitexin in sample solution: 0.22 and 0.40mg/mL, respectively, processing volume: 3 BV, flow rate: 1mL/min, pH 4, temperature: 25 degrees C; for desorption: ethanol-water (40:60, v/v), 5 BV as an eluent, flow rate: 1mL/min. After one run treatment with ADS-5 resin, the contents of vitexin and isovitexin were increased 4.07-fold and 11.52-fold from 0.86%, 1.53% to 3.50% and 17.63%, the recovery yields were 65.03% and 73.99%, respectively. In conclusion, the preparative separation of vitexin and isovitexin can be easily and effectively achieved via adsorption and desorption on ADS-5 resin, and the method can be referenced for the separation of other flavone C-glucosides from herbal materials.     

吸附树脂的色层吸附及其在甜菊甙分离纯化中的应用

研究了ADS－7等吸附树脂对甜菊甙各组分的吸附选择性及色层吸附性能,发现ADS－7吸附树脂不仅在吸附甜菊甙时对各个组分呈现出一定的选择吸附顺序,在水洗时还有一定的选择洗脱顺序,这两个顺序正好相反。利用ADS－7吸对脂的这一色层性能,制备了富含甜度最高、味质最好的Rebaudioside A及几科不含色素的高品质甜菊甙,具有很好的实际应用意义。     

二乙烯苯-异氰酸三烯丙基酯-丙烯腈共聚物大孔树脂对原花青素的吸附

根据原花青素含有疏水性的苯环和酚羟基的特点,设计合成了含有苯环和酰胺基的大孔二乙烯苯-异氰酸三烯丙基酯-丙烯腈(DTA)共聚物吸附树脂,DTA树脂通过疏水作用和氢键吸附原花青素.比较了DTA吸附树脂和3种商品化吸附树脂ADS-5(非极性)、ADS-8(弱极性)和ADS-17(中极性)对原花青素的吸附性能.结果表明,DTA、ADS-8、ADS-17对原花青素的吸附既包含疏水作用又有氢键参与.在合适的单体和致孔剂配比情况下合成的DTA吸附树脂对原花青素有很好的吸附性能.     

Separation of 7-xylosyl-10-deacetyl paclitaxel and 10-deacetylbaccatin III from the remainder extracts free of paclitaxel using macroporous resins

The separation and enrichment of 10-deacetylbaccatin III (10-DAB III) and 7-xylosyl-10-deacetyl paclitaxel were studied on seven macroporous resins with special structures. The performance of 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III on macroporous resins including AB-8, ADS-17, ADS-21, ADS-31, ADS-8, H1020 and NKA-II was compared according to their adsorption and desorption properties. AB-8 provided a much higher adsorption capacity for 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III than other resins, and its adsorption data fitted well to the Langmuir and Freundlich isotherm. According to the adsorption and desorption capacities and the adsorption isotherms, AB-8 demonstrated a remarkable capability for the preparative separation of 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III from the remainder extracts free of paclitaxel. In order to optimize parameters of separation, dynamic adsorption and desorption experiments were carried out on the columns packed with AB-8 resin. The optimal conditions were: the processing volume 15 BV; concentrations of 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III in feed solution 0.0657 mg/mL and 0.1494 mg/mL; flow rate 1 mL/min; temperature 35 degrees C. The gradient elution program was as follows: 30% ethanol for 3 BV, then 80% of ethanol for 6 BV, flow rate 1 mL/min. After the AB-8 resin treatment, the contents of 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III in the product had increased from 0.053% and 0.2% to 3.34% and 1.69%, which were 62.43-fold and 8.54-fold of those in the untreated extracts, respectively, and the recoveries of 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III were 85.85% and 52.78%. The performance achieved good separation and higher recovery of 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III from remainder extracts free of paclitaxel by using AB-8 resin. It is a fast and effective method for the separation and enrichment of 7-xylosyl-10-deacetyl paclitaxel and 10-DAB III.     

Industrial-scale preparation of akebia saponin D by a two-step macroporous resin column separation

A simple and efficient procedure for the industrial preparation of akebia saponin D, one of the bioactive compounds commonly found in the well-known Chinese Medicinal herb Dipsaci Radix, was developed. First, HPD-722 was selected from among 10 kinds of macroporous absorption resins. Following this step, the purity of akebia saponin D was increased about 10 times from 6.27% to 59.41%. In order to achieve a higher purity, ADS-7 was chosen from among five kinds of macroporous absorption resins, and the purity of akebia saponin D was increased from 59.41% to 95.05%. The result indicated HPD-722 and ADS-7 were the most suitable resins to purify akebia saponin D from Dipsaci Radix. Under these conditions, large-scale preparation of akebia saponin D was carried out successfully. The preparation method is simple, efficient, and has been demonstrated to be effective for large scale preparations of akebia saponin D from Dipsaci Radix.     

不同树脂对瓜果腐霉代谢产物中除草活性成分的吸附分析

利用HPD400、HPD500、HPD600、HPD700、HPD850、ADS-17、D101、DM130大孔吸附树脂对瓜果腐霉培养滤液中除草活性成分的吸附情况进行了研究,通过对树脂吸附后的流出液和洗脱液的浓缩物进行HPLC检测分析,确定了其除草活性成分。实验发现,在所选择的8种树脂中以HPD500、HPD850、HPD600、ADS-17对除草活性成分的吸附能力最强,其中以HPD500和HPD600树脂的10%的乙醇洗脱液中除草活性成分含量最高。综合结果表明,以HPD500树脂作为吸附瓜果腐霉培养滤液中除草活性成分的适宜树脂。研究发现,HPD500树脂对除草活性成分吸附和解吸附的最佳条件是:吸附最适温度为20℃,树脂吸附饱和度为33.75mL/g,较适宜吸附流速为2BV/h,较适宜脱附流速为1BV/h,洗脱剂浓度为10%乙醇,洗脱剂用量为2.5BV。     

大孔吸附树脂法去除淫羊藿多糖中蛋白的研究

从4种大孔吸附树脂中筛选出ADS-7, 考察了其对淫羊藿多糖中蛋白的去除作用, 并讨论了pH值、 鞣酸、 上样量等对树脂去蛋白效率的影响. 结果表明, 该方法对淫羊藿粗多糖中的蛋白具有较高的去除效率, 淫羊藿粗多糖中的蛋白含量由1.2%下降到0.035%.     

pH、富里酸和温度对铀酰在ZrP_2O_7上的吸附影响

采用质量滴定法和静态法分别研究了ZrP2O7的零电荷点(pHPZC)和铀酰离子在ZrP2O7上的吸附及解吸行为.铀酰离子在ZrP2O7上的吸附受体系pH、固液比、电解质种类及富里酸(FA)强烈影响,离子强度对铀酰离子在ZrP2O7上吸附的影响较小;随着固液比(m/V)和pH增大,吸附边界向左偏移;磷酸根与硫酸根对吸附有相反的影响;在低pH下,富里酸(FA)促进铀酰离子在ZrP2O7上吸附;柠檬酸根对吸附有非常大的影响;温度升高有利于吸附.采用Langmuir和Freundlich模型对吸附等温线进行拟合研究,表明Freundlich模型可以更好地拟合铀酰离子在ZrP2O7上的吸附.通过对热力学数据如(△H0,△S0和△G0)的计算可知吸附过程是自发和吸热过程.铀酰离子在ZrP2O7上吸附为不可逆吸附.