红花中羟基红花黄色素A的纯化工艺研究

对羟基红花黄色素A纯化进行了工艺研究。采用恒温水提法对红花进行浸提,X-5型吸附树脂分离,采用Sephadex LH-20柱层析对纯化工艺中的条件进行筛选,运用紫外分光光度计测定羟基红花黄色素A的含量。结果显示:纯化的最佳工艺条件为上样量为2%的柱体积,流速为1.0 mL/min,洗脱液浓度为50%的乙醇,径高比为1∶8。采用紫外可见分光光度法测得羟基红花黄色素A的含量为86.4%。此方法具有操作方便,纯度较高的优点。     

Nimbin分离纯化方法的研究

首次成功探索了一条快速、经济、有效的分离纯化nimbin的精制流程,即一次硅胶柱层析—→二次Florisil柱层析—→甲醇结晶的分离精制流程,同时考察了梯度洗脱、不同洗脱速度、不同收集方法对nimbin纯度和回收率的影响,得到纯度为96.072%的nimbin纯化合物。     

连续中压硅胶柱层析纯化法夫酵母虾青素

采用连续中压硅胶柱层析纯化虾青素,原料为含量高于20%的法夫酵母虾青素。连续中压柱层析分离工艺条件为:不锈钢中压层析柱装填120～160μm层析硅胶,以石油醚∶1,2-二氯乙烷∶丙酮(体积比)为5∶2.5∶1作洗脱剂,负载量为1∶7,可以得到纯度大于97%的虾青素产品,平均回收率大于60%。回收的洗脱液经校正后可重复使用。使用后的层析柱以丙酮为再生液再生,石油醚为平衡液平衡,平衡后的层析柱可重复使用多次。利用该工艺方法纯化虾青素,与传统方法相比溶剂用量少、层析填料价格低、生产周期短、分离效果好,易于实现连续工业化清洁生产。     

一种高纯度羊毛脂胆固醇制备方法的研究

研究了以95%以上纯度的羊毛脂胆固醇为原料,通过熔融结晶提纯的方法得到高纯度羊毛脂胆固醇,包括熔融结晶、发汗和溶解结晶三个步骤。本次研究考察了该工艺各步骤的纯化条件,并对各步纯化条件进行了筛选和优化。结果表明,粗品只需经过一次熔融结晶、发汗、溶解结晶就可得到含量99%以上纯度的高纯度羊毛脂胆固醇,总收率达到60%以上。该方法与现有高纯度羊毛脂胆固醇生产方法相比,工艺简单、毒性低、产品纯度及收率均较高,具有工业化生产前景。     

总丹参酮中丹参酮ⅡA的提取分离

目的:以丹参酮ⅡA含量为跟踪指标,建立一个适合工厂化生产的丹参酮ⅡA分离纯化工艺。方法:先对提取溶剂、提取方法、提取溶剂用量和提取时间进行比较筛选,再利用硅胶柱层析进行分离纯化。结果:先用60倍的甲醇超声提取2.5h,再进过硅胶柱层析,以氯仿:石油醚(4∶1)为洗脱剂的提取纯化方法为最佳的工厂化生产工艺。结论:该工艺不仅提取率高,收率较高、成本低、合理,而且简便、实用。     

硅胶柱层析法分离生姜精油中的β-水芹烯

利用硅胶柱层析对生姜精油中的β-水芹烯进行分离研究,采用紫外分光光度法(UV)、气相色谱-质谱联用(GC-MS)和高效液相色谱(HPLC)对分离样品进行分析,结果表明,柱层析适宜条件为:正己烷为洗脱剂,m(生姜精油)∶m(硅胶)=1∶50,洗脱剂流速为2.0 mL/min。在该条件下,经过两次硅胶柱层析,可得到β-水芹烯的峰面积百分数为95.18%的样品。     

苦豆子生物碱单体的分离纯化工艺研究

在对苦豆子的酸水浸提液进行了超滤和脱色预分离的基础上,采用不同的有机溶剂萃取和硅胶柱层析对其中主要的生物碱进行分离纯化及条件优化.结果表明合适的生物碱萃取富集条件是用氯仿为溶剂,Ph=10.5.该氯仿萃取液用硅胶柱层析分离,洗脱剂为氯仿-甲醇-氨水(5:0.4:0.01,V/V/V),洗脱速度1柱床体积·h-1,得到峰1～峰3.峰1和峰2中的化合物经丙酮结晶和重结晶分别得到纯度99%以上的氧化槐果碱和氧化苦参碱;峰3对应的组分再经硅胶柱层析,洗脱剂为丙酮-甲醇(10:1,V/V),洗脱速度1柱床体积·h-1,得到峰4～峰6,峰4中的化合物经石油醚结晶和重结晶,可以得到纯度95.8%的槐定碱.采用了HPLC-MS,IR,熔点测定和薄层色谱等方法进行上述生物碱单体的定性定量及分子结构确定. 本研究为深度开发苦豆子生物碱资源和为制备医药工业所需的高纯度生物碱原料提供了依据.     

树脂吸附法从发酵液中提取红霉素的工艺研究

针对传统红霉素生产工艺中存在的问题,提出了膜过滤、吸附、杂质洗涤、红霉素洗脱、洗脱液成盐及树脂再生等步骤组成的红霉素提取新工艺过程。以红霉素发酵液为原料,研究和优化了各单元操作的工艺条件和实际效果。采用孔径为50 nm的无机陶瓷膜对红霉素发酵液进行预处理,过程的平均脱色率为54.0%,平均脱蛋白率为67.5%,红霉素平均收率为92.5%。采用大孔树脂吸附技术对滤液中的有效成分进行浓缩、富集,过程收率为92.6%,结晶后所得红霉素硫氰酸盐的纯度相比原有工艺提高2.31%。筛选出体积分数50%丙酮和50%0.40mol/L NaOH溶液组成的混合溶液对使用后的树脂进行再生,再生后树脂的饱和吸附量不低于新鲜树脂饱和吸附量的80%。     

以分子筛为脱水剂精制DMF

本文研究了以分子筛为脱水剂精制DMF的工艺条件，结果表明：能将含水量0.1-0.3%DMF一次脱水达到含水量0.03%以下，解决了我国DMF水份超标的难题。本工艺设备简单、再生条件温和、操作费用低、成本低。分子筛可使用1000次上。     

达卡他韦二盐酸盐晶型A结晶工艺研究

目的:开发抗丙肝药达卡他韦二盐酸盐晶型A的放大制备方法。方法:运用溶液结晶法研究了达卡他韦二盐酸盐晶型A的结晶工艺,包括溶剂的选择、结晶起始温度、熟化时间和结晶终点温度等因素。结果:选定水作为结晶溶剂,结晶起始温度为60℃,60℃熟化时间为6～8小时,终点结晶温度为20～25℃,获得最终产品。100克放大验证结果表明,使用本研究确定的工艺路线,可将晶型A成功放大到100克。结论:建立了达卡他韦二盐酸盐晶型A的放大制备方法,该方法操作简单,所用结晶溶剂为纯水,绿色环保无污染,可放大性好,适合工业化生产。     

Purification of wedelolactone from Eclipta alba and evaluation of antioxidant activity

A hybrid chromatography-crystallization process to purify wedelolactone obtained from Eclipta alba was developed. The crude extract was obtained by microwave-assistant extraction and purified by silica gel column chromatography in which dichloromethane–methanol–acetic acid solution was used as the eluent. Dilution crystallization was employed to perform the final purification. To optimize the processing parameters, single factor analysis and response surface methodology were employed. The results indicated that the purification yield and purity of wedelolactone could reach 77.66% and 99.46%, respectively. Antioxidant assays showed that the products had strong antioxidant and free radical scavenging activity which was close to oligomeric proantho cyanidins.     

Purification of cholesterol from lanolin by column chromatography

采用柱层析法分离羊毛脂中的胆固醇,以胆固醇与杂质羊毛甾醇的分离度为判定依据来筛选吸附剂及优化层析工艺,同时对吸附剂进行了再生考察。实验表明,当以200～300目粗孔硅胶为吸附剂、丙酮/正己烷混合溶剂（体积比4∶96）为流动相、35 ℃下胆固醇上载量为2.4%（质量分数）时,胆固醇的分离效果较好,所得胆固醇含量可达84.36%,收率为85.67%。另外选用丙酮/正己烷混合溶剂（体积比50∶50）对吸附剂进行再生处理,硅胶经7次使用再生循环,分离效果未降低。     

Purification process for cod liver oil polyunsaturated fatty acids

The polyunsaturated fatty acids (PUFA) eicosapentaenoic acid (EPA, 20∶5n−3) and docosahexaenoic acid (DHA, 22∶6n−3), which have several pharmaceutical properties, have been purified from cod liver oil. The process consisted of four main steps: (i) saponification of the oil, (ii) use of urea inclusion adducts method to obtain PUFA, (iii) PUFA methylation, and (iv) argentation silica gel column chromatography of the methylated PUFA. Argentation silica gel chromatography yielded highly pure DHA in the process (100% purity, 64% yiild). For EPA, the recovery in the combined process was 29.6%, and the final purity was 90.6%, owing to the simultaneous elution of other polyunsaturated fatty esters. The recovery in the urea inclusion method was strongly enhanced by application of orbital agitation during the crystallization process, in which EPA yield increased from 60–70% without agitation to 90–97% at 800 rpm; stearidonic acid (18∶4n−3) yield ranged from 60–75% without agitation to 87–95% at 800 rpm, and DHA yield varied from 53–73% without agitation to 85–99% at 800 rpm     

应用薄层色谱对牛磺酸生产工艺进行流程诊断

以硅胶Ｇ为固定相,以正丁醇－冰醋酸－乙醇－水体系为流动相,研究了薄层色谱对工业合成牛磺酸及其中间产物２ 氨基乙基硫酸酯、反应原料乙醇胺的分离效果。实验结果表明,当流动相组成为正丁醇∶冰醋酸∶乙醇∶水＝８∶２∶１∶１（体积比）时,分离效果较佳。并应用该方法对牛磺酸生产工艺进行了流程诊断,分析了原料、酯化反应产物、还原反应产物、粗结晶产品和牛磺酸产品的组成。结果表明,酯化反应、还原反应、粗结晶和结晶精制各步收率分别为８９．５７％、７６．９５％、９３．６１％和９３．１２％,中间产物２ 氨基乙基硫酸酯在还原步骤发生可逆反应是导致牛磺酸收率较低的根本原因。     

Recovery of Sinapic Acid from the Waste Effluent of Mustard Protein Isolation by Ion Exchange Chromatography

Sinapic acid present in the waste stream of yellow mustard protein isolation was purified by strong base Dowex (1 × 8, Cl^?) ion exchange chromatography. The ratio of loading volume to resin bed volume was 19:1. Approximately 80 % of sinapic acid was adsorbed. The column was washed with two bed volumes of water to remove remaining undesirable components. Approximately 75 % of sinapic acid adsorbed by the resins in the column was eluted by ten bed volumes of a solution containing 0.9 M acetic acid and methanol (4:6, v/v). Up to 15 adsorption and regeneration cycles resulted in only a slight, 3–5 %, reduction in ion exchange capacity, indicating that this is a viable approach to the recovery and purification of sinapic acid. The recovery of this valuable nutraceutical ingredient improves the economic viability of an integrated extraction process for this Canadian oilseed crop.     

Biological regeneration of nitrate-loaded anion-exchange resins by denitrifying bacteria

For regeneration of nitrate-loaded anion-exchange resins large quantities of salt are needed while the voluminous concentrated brine, produced during regeneration, is difficult to dispose of. These problems can be avoided by using denitrifying bacteria in the regeneration process of the resins. Experiments showed that resins could be regenerated by a denitrifying sludge suspension containing 7 g dm^?3 NaCl. However, the process proceeded slowly compared with conventional regeneration. After 24 h of regeneration the resin still contained 18% nitrate, relative to the total capacity. The breakthrough curve of a biologically regenerated ion-exchange resin was characterized by nitrate leakage whereas nitrate breakthrough started sooner, resulting in a nitrate capacity which was only 72% as compared with a conventionally regenerated ion-exchange column.     

柱色谱法纯化马铃薯叶中的茄尼醇

通过柱色谱法从马铃薯叶的提取物中分离提纯了茄尼醇,并以RP-HPLC法测定了茄尼醇的质量分数。采用硅胶对茄尼醇进行吸附纯化,以茄尼醇的实测收率、质量分数为考察指标,通过对硅胶颗粒、洗脱剂流速、洗脱剂组分配比进行考察,确定了茄尼醇的柱色谱优化条件。结果表明,以200~300目硅胶为填料,流动相流速为2.0 mL/m in,洗脱剂以石油醚、V(石油醚)∶V(乙酸乙酯)=20∶1、15∶1、9∶1进行梯度洗脱,茄尼醇的质量分数达到85.37%,重结晶后达到97.47%。     

Design and operation of a modified silica gel column chromatography

Liquid–solid chromatography (LSC) is the oldest of the various liquid chromatography methods. Despite the fact that high-performance liquid chromatography (HPLC) operation leads to better separation and analysis, classical column chromatography and thin-layer chromatography (TLC) are still widely practiced because of their convenience. In this study, a modified silica gel column chromatography was designed with the objective of reducing the amount of solvent required to achieve the same degree of separation as the classical silica gel column chromatography. The separation of squalene and fatty acid steryl esters (FASEs) from non-polar lipid fraction (NPLF) of soybean oil deodorizer distillate (SODD) was employed as a model system to test the effectiveness of this new design. Modified silica gel column chromatography process is feasible from economic point of view compare to classical silica gel column chromatography because it significantly reduces the amount of solvent and time required to achieve the same degree of separation. By employing modified silica gel column chromatography to obtain the squalene-rich fraction, the mobile phase volume and elution time required as fractions of those needed in classical silica gel column chromatography are 1/73 and 1/18, respectively. To obtain the FASEs-rich fraction, the corresponding mobile phase volume and elution time are 1/221 and 1/23, respectively of those needed in classical silica gel column chromatography.     

头孢氨苄连续结晶研究及应用

头孢氨苄的传统生产方法多为间歇结晶,存在效率低、能耗高等弊端。为节约能耗、提高生产效率、缩短工时、降低成本,针对头孢氨苄等电点结晶的特点,本文设计了两级连续结晶工艺。采用单因素法系统研究了头孢氨苄水溶液初始浓度、停留时间、搅拌速率、结晶终点pH、晶种策略等因素对头孢氨苄连续结晶过程产品的收率、晶习及粒度分布的影响。单因素实验结果显示头孢氨苄水溶液质量分数为14%、最佳停留时间为12min、结晶终点pH控制在4.8附近、晶种添加量为5%时其产品收率、粒度分布均达到了理想的效果。该工艺能将结晶过程的过饱和度有效地控制在介稳区内,避免了爆发成核。与间歇结晶相比,两级连续结晶工艺的工时缩短30%。产品晶习完整,粒度分布均匀,收率可以达到96%。目前该工艺已成功实现单条生产线规模为500t/a的产业化应用。