大孔吸附树脂分离纯化异甘草素的研究

研究大孔吸附树脂分离纯化异甘草素的工艺条件及参数。通过研究HPD-600、D4020、D101、AB-8、NKA-II、AL-2和NKA-9树脂对异甘草素的吸附和解吸附能力,筛选最佳树脂为AB-8,并研究了其对异甘草素的吸附和解吸附性能,确定了最佳的吸附与解吸附工艺参数,吸附:pH=5,室温,流速1.5BV/h,溶液处理量为5BV;脱附:洗脱剂为70%的乙醇溶液,流速1BV/h,洗脱剂用量4.5BV。异甘草素样品溶液经AB-8树脂吸附与脱附后回收率为76.7%,纯度由2.02%提高到29.1%,提高了14.4倍。实验结果表明,AB-8树脂对异甘草素的吸附量大,脱附容易,可以应用于异甘草素的分离纯化。     

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.     

大孔吸附树脂富集板蓝根中(R,S)-告依春工艺研究

采用静态吸附法考察了D101、AB-8、NKA-2、NKA-9、HPD 100、HPD600等6种大孔吸附树脂对(R,S)-告依春的吸附及解吸性能,筛选出效果最佳的AB-8树脂,并对其进行动态考察.最佳富集条件为:上样液pH 6,生药质量-体积浓度为0.200g/mL,解吸液为2BV量70％乙醇,在优化条件下(R,S)-告依春在浸膏中含量可从0.76％提高到12.48％.结果表明,AB-8型大孔吸附树脂可用来从板蓝根水提取液中富集(R,S)-告依春.     

Optimization of luteolin separation from pigeonpea [Cajanus cajan (L.) Millsp.] leaves by macroporous resins

In the present study, the performance and separation characteristics of eight macroporous resins for the separation of luteolin (LU) from pigeonpea leaves extracts have been evaluated. The adsorption and desorption properties of LU on macroporous resins including AB-8, NKA-9, NKA-2, D3520, D101, H1020, H103 and AL-2 have been compared. AL-2 resin offers the best adsorption and desorption capacity for LU than other resins based on the research results, and its adsorption data at 25 degrees C fit best to the Freundlich isotherm. Dynamic adsorption and desorption experiments have been carried out with the column packed by AL-2 resin to optimize the separation process of LU from pigeonpea leaves extracts. The optimum parameters for adsorption were sample solution LU concentration 65.5 microg/ml, pH 5, processing volume 3 BV, flow rate 1.5BV/h, temperature 25 degrees C; for desorption were elution solvent ethanol-water (50:50, v/v) 2 BV and followed by ethanol-water (60:40, v/v) 2 BV, and flow rate 1BV/h. After treated with AL-2 resin, the LU content in the product was increased 19.8-fold from 0.129% to 2.55%, with a recovery yield of 78.54%. The results showed that AL-2 resin revealed a good ability to separate LU. Therefore, we conclude that results in this study may provide scientific references for the large-scale LU production from pigeonpea or other plants extracts.     

大孔吸附树脂分离纯化金银花中黄酮类物质的研究

比较了AB-8、S-8、NKA-9和D-101 4种大孔吸附树脂对金银花提取液中黄酮类物质的吸附及解吸附性能.在静态吸附试验基础上,筛选出效果较好的D-101树脂进行动态试验研究,结果表明,D-101树脂在30℃下对金银花黄酮类物质的静态吸附-动态解吸较优的工艺参数为:上样液pH值2.46,解吸液为95%乙醇,解吸液的流速为3mL/min,pH值11,4.5BV解吸液即可完全洗脱被树脂吸附的黄酮类物质,其解吸率高达98.00%.在试验研究范围内,树脂吸附金银花黄酮是自发性放热过程,并且符合Langmuir方程,此外树脂对黄酮的吸附动力学可用Pseudo-second-order模型较好地拟合,其表观吸附速率常数为Kso℃=3.43×10-2g/(mg·min).     

Preparative separation and enrichment of four taxoids from Taxus chinensis needles extracts by macroporous resin column chromatography

An environment‐friendly method was established for the preparative separation and enrichment of four taxoids, namely 10‐deacetylbaccatin III (10‐DAB III), 7‐xylosyl‐10‐deacetyltaxol (7‐xyl‐10‐DAT), cephalomannine and paclitaxel from Taxus chinensis needles extracts. Characteristics of seven widely used macroporous resins for four taxoids were compared, AB‐8 resin offered better adsorption and desorption capacities than others. AB‐8 resin column chromatography was used to study the desorption process for four taxoids. The optimum parameters for desorption were 30% ethanol 5 RV for removing impurities, following 15 RV for 10‐DAB III, after the desorption of impurities with 35% ethanol 10 RV, 45% ethanol 30 RV for 7‐xyl‐10‐DAT, then 65% ethanol 10 RV for cephalomannine and paclitaxel, the flow rate was 6 RV/h. After separation on AB‐8 resin column chromatography, the contents of 10‐DAB III, 7‐xyl‐10‐DAT, cephalomannine and paclitaxel in the product reached 4.58, 13.17, 1.36 and 3.08%, respectively, which were 7.63‐, 3.68‐, 6.18‐ and 6.55‐fold to those in T. chinensis needles extracts. The recovery yields were 94.96, 77.32, 88.09 and 95.25%. In general, the AB‐8 resin column chromatography has the advantages of lower cost, high efficiency and simple procedure. Therefore, it may provide scientific references for the preparative separation and enrichment of taxoids from other T. species.     

Enrichment and purification of deoxyschizandrin and γ-schizandrin from the extract of Schisandra chinensis fruit by macroporous resins

In present study, the performance and separation characteristics of 21 macroporous resins for the enrichment and purification of deoxyschizandrin and γ-schizandrin, the two major lignans from Schisandra chinensis extracts, were evaluated. According to our results, HPD5000, which adsorbs by the molecular tiers model, was the best macroporous resin, offering higher adsorption and desorption capacities and higher adsorption speed for deoxyschizandrin and γ-schizandrin than other resins. Columns packed with HPD5000 resin were used to perform dynamic adsorption and desorption tests to optimize the technical parameters of the separation process. The results showed that the best adsorption time is 4 h, the rate of adsorption is 0.85 mL/min (4 BV/h) and the rate of desorption is 0.43 mL/min (2 BV/h). After elution with 90% ethanol, the purity of deoxy-schizandrin increased 12.62-fold from 0.37% to 4.67%, the purity of γ-schizandrin increased 15.8-fold from 0.65% to 10.27%, and the recovery rate was more than 80%.     

Enrichment and purification of madecassoside and asiaticoside from Centella asiatica extracts with macroporous resins

In present study, the performance and separation characteristics of five macroporous resins for the enrichment and purification of asiaticoside and madecassoside from Centella asiatica extracts have been evaluated. The adsorption and desorption properties of total triterpene saponins (80% purity) on macroporous resins including HPD100, HPD300, X-5, AB-8 and D101 have been compared. According to our results, HPD100 offered higher adsorption and desorption capacities and higher adsorption speed for asiaticoside and madecassoside than other resins. Column packed with HPD100 resin was used to perform dynamic adsorption and desorption tests to optimize the separation process of asiaticoside and madecassoside from C. asiatica extracts. After the treatment with gradient elution on HPD100 resin, the content of madecassoside in the product increased from 3.9 to 39.7%, and the recovery yield was 70.4%; for asiaticoside the content increased from 2.0 to 21.5%, and the recovery yield was 72.0%. The results showed that HPD100 resin revealed a good ability to separate madecassoside and asiaticoside, and the method can be referenced for the separation of other triterpene saponins from herbal raw materials.     

大孔吸附树脂分离纯化金银花绿原酸研究

以金银花粗提物为原料,比较了NKA-2、D1400、聚酰胺、HP2MGL、ADS-21、D101及AB-8 7种大孔吸附树脂对金银花绿原酸静态吸附与解吸的效果,并通过单因子实验、正交试验与验证实验,优化了树脂分离纯化金银花绿原酸的工艺技术参数.结果表明,NKA-2树脂吸附效果最好,静态饱和吸附量可达212.17 mg/...     

大孔树脂分离纯化丹酚酸的研究

比较了D301R、D392、D380大孔阴离子交换树脂和X-5.AB-8、NKA-9、SP825大孔吸附树脂对丹参水溶性成分的吸附和解吸能力,筛选出效果较好的SP825进行分离纯化丹酚酸的研究.实验表明,大孔吸附树脂SP825能分离出纯度为95.32%的丹参素,在梯度洗脱条件下可得到以丹参素(水洗脱)和丹酚酸B(乙醇洗脱)为主的产品.在最佳吸附与解吸工艺参数下,丹参素、紫草酸、迷迭香酸、丹酚酸A和丹酚酸B的收率分别为:36.92%、80.39%、82.45%、43.07%和41.03%.     

大孔吸附树脂提取青蒿素的研究

探讨了大孔吸附树脂提取青蒿素的方法。以青蒿素的吸附量,青蒿素含量,青蒿素收率和提取率为考察指标,确定大孔吸附树脂提取青蒿素的工艺条件。研究结果表明,ADS-17树脂对青蒿素的吸附量大,解吸容易,可用于提取黄花蒿中青蒿素的工业化生产,其工艺条件为:青蒿素最大吸附量为112.30mg/g,吸附流速为2BV/h,洗脱剂为90%乙醇,解吸流速为2BV/h,青蒿素含量大于99%,收率高达0.3%,提取率高达75%以上。     

Separation and purification of flavonoid from Taxus remainder extracts free of taxoids using polystyrene and polyamide resin

An efficient separation process of flavonoid from Taxus wallichiana var. mairei remainder extracts free of taxoids was developed in this study. AB‐8 macroporous resin and polyamide resin offered the fine adsorption capacity, and its adsorption rate at 30°C fitted well to the Langmuir and Freundich isotherms. Resin dynamic adsorption and desorption experiments were conducted to optimize the separation process of total flavonoids from T. wallichiana var. mairei remainder extracts free of taxoids. The optimum parameters for adsorption by AB‐8 resin were as follows: (1) the concentration of flavonoids in a sample solution of 5.61 mg/mL with a processing volume of 2 bed volume (BV) (60 mL); (2) for desorption, ethanol–water (80:20, v/v), with 6 BV as an eluent at a flow rate of 2 BV/h. After a one‐run treatment with AB‐8 resin, the content of flavonoids was increased 5.10‐fold from 4.05 to 20.65%. The optimum parameters for adsorption by polyamide resin were as follows: processing volume of 2 BV (30 mL); for desorption, ethanol–water (70:30, v/v), with 8 BV as an eluent at a flow rate of 2 BV/h. After one‐run treatment with polyamide resin, the content of total flavonoids increased from 20.65 to 65.21%. The method will provide a potential approach for large‐scale separation and purification of flavonoid for its wide pharmaceutical use.     

大孔吸附树脂分离纯化荔枝核黄酮类化合物的研究

比较了D101、D3520、NKAII、AB-8、X-5、HPD-100、HPD-300、HPD-600等8种大孔吸附树脂对荔枝核中抗乙肝活性成分黄酮类化合物的吸附及解吸性能,筛选出效果较好的HPD-300树脂进行分离纯化实验研究。实验表明,HPD-300树脂能够有效地吸附和解吸荔枝核黄酮类化合物,并确定了最佳的吸附和解吸工艺参数。采用最佳的工艺条件分离纯化荔枝核黄酮类化合物,黄酮类化合物的含量由31%提高到82%。     

Separation of injectable salidroside by column chromatography of macroporous resins for treating myocardial ischemia

The objective of the present study is to develop a method for large-scale separating and purifying salidroside from rhodiola kirilowii roots and for preparing injectable medicinal ingredient.Crude extract of salidroside was prepared by water-ethanol system,and purified by column chromatography of macroporous resins.Static adsorption and desorption studies were performed on six kinds of macroporous resins,and SP825 resin was chosen,followed by optimizing process parameters.The optimum sample volume,feed concentration,ratio of diameter to height,and feeding flow rate were 1.5 bed volumes(BV),15 mg/mL,1:10 and 1 BV/h,respectively.Dynamic desorption was performed consecutively with 8 BV of distilled water,3 BV of 5% ethanol and 8 BV of 10% ethanol at a flow rate of 2 BV/h.After three cycles in separating 3.5 tons of rhodiola kirilowii roots,salidroside purity was increased from 3.4% in the crude extract to 93.6% in purified salidroside product.This study provides a novel method to separate salidroside for injectable use.     

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.     

大孔树脂对茄尼醇吸附行为的研究

从6种大孔树脂中筛选出用于茄尼醇分离较好的树脂NKA,并进一步研究了其对茄尼醇吸附行为,结果表明,吸附等温线服从Langmuir方程和Freundlich方程,且吸附过程表现为优惠吸附.在温度为283～313K,吸附量为15～35mg/g的条件下,吸附焓变为-16.20～16.57kJ/mol,自由能变为.3.142～3.459kJ/mol,吸附熵变为-47.43～41.17J/mol.K.NKA树脂对茄尼醇吸附速率较快,吸附过程符合一级吸附动力学方程,吸附过程主要受液膜扩散控制.     

大孔吸附树脂分离提取多杀菌素

采用大孔吸附树脂法分离提取多杀菌素.从11种大孔吸附树脂中筛选出DM11进行了静态、动态吸附性能实验,并考察了不同吸附、解吸条件的影响.结果表明,DM11的静态吸附容量为25.63mg/g(wet resin),其吸附等温线符合Langmuir吸附等温式.采用丙酮做洗脱剂,洗脱率为97.5%,动态吸附最佳吸附pH为9.5,吸附流速为6BV/h,穿透吸附容量为21.2mg/ml(wet resin),洗脱流速1.5BV/h.     

Simultaneous determination of main taxoids in Taxus needles extracts by solid-phase extraction-high-performance liquid chromatography with pentafluorophenyl column

A simple and accurate RP-HPLC method with pentafluorophenyl (PFP) column was developed for the simultaneous determination of six taxoids, i.e. paclitaxel, 10-deacetylbaccatin III (10-DAB III), 7-xylosyl-10-deacetyltaxol (7-xyl-10-DAT), 10-deacetyltaxol (10-DAT), cephalomannine and 7-epi-10-deacetyltaxol (7-epi-10-DAT), in the extracts from the needles of three Taxus species. The mobile phase consisted of acetonitrile (A) and water (B), and the extracts were separated using gradient elution program: 30% A at the first 7 min, and then ramped to 42% A at 8 min, held until 38 min. The developed method was validated with satisfactory precision (RSD < 2.61%), repeatability (RSD < 2.92%) and recovery (95.19-104.47%). The above taxoids in the extracts of Taxus cuspidata, T. chinensis and T. media were analyzed with the developed RP-HPLC method, and the results showed that the contents of different taxoids in three mentioned species were distinct. Maximal amounts of 10-DAB III, 7-xyl-10-DAT and 7-epi-10-DAT appeared in T. chinensis, while T. media possessed the highest content of 10-DAT, cephalomannine and paclitaxel. The developed method is accurate and efficient. It can be reliably used in the improved determination of taxoids for the quality control of Taxus species.     

新乡红豆杉中多种紫杉烷类化合物的反相高效液相色谱分析

采用反相高效液相色谱法(RP-HPLC)研究了新乡种植红豆杉树皮中的多种紫杉烷类化合物.结果表明,新乡种植红豆杉树皮中的10-去乙酰巴卡丁Ⅲ、巴卡丁Ⅲ、7-木糖-10-去乙酰基三尖杉宁碱、7-木糖-10-去乙酰基紫杉醇、7-木糖-10-去乙酰基紫杉醇C、10-去乙酰基紫杉醇、三尖杉宁碱和紫杉醇的平均含量(质量分数,n=...     

Regioselective protection of 10-deacetylbaccatin Ⅲ and semi-synthesis of paclitaxel

Semi-synthesis of paclitaxel was achieved in four steps from 10-deacetylbaccatin HI （10-DAB HI）. The key steps are the regioselective protection at the hydroxyl group at C-7 of 10-DAB HI, using 1,1′-thiocarbonyldiimidazole as a selective reagent, and the deprotection of the protected paclitaxel with a mixture of p-toluenesulfonic acid and 0.1 mol/L aqueous hydrochloride.