废次烟叶中浸膏提取纯化茄尼醇的柱分离条件的研究

通过对上样量、填料高度、流速等因子的考察,研究在常温常压条件下柱层析分离方法提纯精制茄尼醇粗品的优化方法.结果显示:装柱量为30g,茄尼醇粗品上样量1.0g,流速为0.6mL/min为最佳柱分离条件的硅胶柱层析的分离效果较好,可以得到纯度95%以上的茄尼醇.     

柱层析法纯化烯丙基硅烷

以四烯丙基硅炕（G0）为核心制备了第一代（G1）和第二代烯丙基硅烷（G2）．产物以正己烷-乙酸乙酯V（正己烷）：V（乙酸乙酯）=20：1为流动相,采用一次硅胶柱层析法,用薄层层析（TLC）检测,成功脱除杂质,目标产物收率为67．6％（G1）和64．8％（G2）．经核磁共振、热质量分析等表征提纯产物,表明目标产物结构完整．     

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%。     

硅胶柱层析法提纯大豆磷脂酰胆碱的研究

探讨了以大豆浓缩磷脂为原料,应用柱层析法提纯大豆磷脂酰胆碱(PC)的工艺过程.用TLC法考察了水、异丙醇与正己烷的体积配比,确定流动相适宜配比为正己烷:异丙醇:水(1:1:0.175,v/v/v).通过对固定相、流动相和上载量的考察,得到了柱层析最佳工艺条件:在空塔流速为0.382 cm·min-1,进样浓度为0.25 g浓缩磷脂·(mL流动相)-1的室温条件下,固定相选用100～200目粗孔2号硅胶,流动相为正己烷:异丙醇:水(1:1:0.16,v/v/v),最适上载量为0.086gPC·(g硅胶)-1.经高效液相色谱法定量分析,产品中磷脂酰胆碱纯度高达85%.     

应用柱层析法纯化Vero细胞乙型脑炎疫苗

浓缩Vero细胞乙脑疫苗经SepharoseCL－6B柱层析可去除大部分杂蛋白，再经SphacrylS－500HR层析可进一步去除比病毒大的杂质及残余小分子量杂蛋白。经两步凝胶过滤层析纯化后，疫苗总蛋白含量减少约99％，抗原比活性提高87～165倍，抗原回收率达30％～50％，残余牛血清和残余细胞DNA均符合WHO有关规程要求，提纯疫苗的效力达到或超过中国地鼠肾灭活乙脑疫苗和日本提纯鼠脑拔苗的参考苗。     

多级错流萃取法从粗品茄尼醇皂化液中提取茄尼醇的研究

采用液液萃取法从茄尼醇皂化液中提取茄尼醇,对茄尼醇皂化液的萃取条件进行研究,探讨了萃取剂的用量、萃取温度、萃取时间及萃取级数对多级错流萃取过程的影响,并进行正交实验.结果表明5.0 g粗品茄尼醇经皂化,加人100 mL萃取剂、温度控制为30℃、萃取时间设汁为45 min、经过三级错流萃取,并脱除萃取溶剂,可得到70%以上的茄尼醇,分配系数为27.58.     

柱层析法纯化基因工程HBsAg中试工艺的研究

由乙肝病毒S基因转化的哺乳动物细胞培养收液，经过Butyl-S-SepharoseFF层析，DEAESepharoseFF层析和Sepharose4FF层析，可获HBsAg纯品。产品检定结果表明，PAGE和SDS-PAGE电泳纯度均合格，小牛血清残余量、细胞DNA残余量和动物免疫效力也均符合规定标准．HBsAg终收率达40％左右．在此工艺中，疏水作用柱层析的纯化效率比较高，可去除绝大部分杂蛋白和细胞DNA。     

柱层析法制备无甲醇酒精

用球状４Ａ（钠Ａ）型分子筛作固定相,以无水乙醇作流动相,采用迎头法洗脱,对无水乙醇中的甲醇进行柱层析,制备了无甲醇乙醇。     

柱层析法制备无甲醇酒精

用球状４Ａ（钠Ａ）型分子筛作固定相,以无水乙醇作流动相,采用迎头法洗脱,对无水乙醇中的甲醇进行柱层析,制备了无甲醇乙醇。     

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。     

硅胶柱层析纯化利普司他汀工艺研究

采用硅胶柱层析法对利普司他汀粗品进行分离纯化,确定最佳纯化工艺条件如下:以120目硅胶为固定相,依次用1 BV 5％ 丙酮-正庚烷、1 BV 10％ 丙酮-正庚烷、7 BV 15％ 丙酮-正庚烷、2 BV 30％ 丙酮-正庚烷梯度洗脱,洗脱流速为0.75 BV·h-1,载样量为3％,收集7 BV 15％ 丙酮-正庚烷的...     

烯虫酯的纯化

通过硅胶柱层析纯化烯虫酯,以V正/V丙=100/1.2正己烷丙酮混合液作淋洗液,使烯虫酯与杂质分离,制得99%以上的烯虫酯,柱层析方法可行、实用。     

硅胶柱层析法分离提纯双基药中的硝化甘油

探讨了以双基药为原料,采用柱层析法分离提纯来获取少量硝化甘油的工艺方法。结果表明,以乙醚为提取溶剂、二氯甲烷为流动相,45~75μm的层析用粗孔硅胶为固定相,空塔流速约为0.764 cm/min的条件下进行层析柱分离提纯,可获取克量级的硝化甘油。经高效液相色谱法分析,所得硝化甘油纯度高,未见杂峰。     

Purification of Stearidonic Acid from Modified Soybean Oil by Argentation Silica Gel Column Chromatography

The objective of this study was to purify stearidonic acid (SDA, 18:4 ω-3) from modified soybean oil containing a mixture of over 20 fatty acids (23% SDA). Interest in obtaining purified fractions of SDA arises from reported health benefits associated with polyunsaturated fatty acids (PUFA), such as cardiovascular disease prevention. In addition, SDA may also provide improved stability characteristics since its unsaturation index is less than longer PUFA, such as eicosapentaenoic acid (EPA, 20:5 ω-3). First, a chemical ethanolysis of modified soybean oil was performed to transform the triacylglycerols into fatty acid ethyl esters (FAEE). Then, the FAEE were fractionated and SDA-EE was purified by argentation silica gel (10% AgNO₃) open column chromatography, which allows selectivity based on degree of unsaturation. Different FAEE sample loads and mobile phases were explored until the best purification of SDA-EE was achieved. The solvents used were hexane and hexane:acetone mixtures (99 and 95%). Under the optimal conditions, a fraction with high SDA-EE purity (96%) was obtained with 77% yield. Besides, it was possible to obtain another fraction enriched in α-linolenic acid-EE (37% purity and 68% yield) and γ-linolenic acid-EE (22% purity and 61% yield). A scaled-up process resulted in 840 mg of final product composed of 97% SDA-EE with 71% yield.     

低压硅胶柱层析分离制备高纯辣椒素

从辣椒素总碱（Capsaicinoids）中提取高纯度的辣椒索及二氢辣椒素单体,建立了分离工艺条件。以TLC实验筛选适当的洗脱流动相,低压硅胶柱层析分离纯化,产物用两相法重结晶,TLC及HPLC监测分离效果及产品纯度。结果表明优选的流动相为混合溶剂石油醚：丙酮=8：2（体积比）,纯化分离得到辣椒素和二氢辣椒索,纯度分别从64％和29％提高到97％和96％。     

柱层析法分离纯化碳酸甘油酯

采用氧化铝柱层析法分离纯化碳酸甘油酯,根据溶剂极性选择甲醇和丙酮混合溶液为洗脱剂,探讨了溶剂组成配比、粗碳酸甘油酯样品与氧化铝重量比和温度对分离效果的影响。由实验得出较佳分离条件为:洗脱剂配比V甲醇︰V丙酮=1︰19,粗碳酸甘油酯样品与氧化铝重量比N=1︰10,常温,此时纯度大于95%的碳酸甘油酯的收率可达92.53%。     

Purification of GLA-Triglycerides from Evening Primrose Oil by Gravimetric Column Chromatography

Gravimetric normal-phase silver ion–silica gel column chromatography has been used for the novel application of purification of GLA-containing triglycerides (GLA-TGs) from evening primrose seed oil (EPO). Gradient elution with increasing polarity enabled separation of valuable TG species containing γ-linolenic acid (GLA, 18:3n-6). Enzymatic hydrolysis revealed the distribution of fatty acids (FAs) in the isolated TG species, with GLA in the sn-2 position in different percentages, depending on the degree of unsaturation. A novelty of this work was the successful use of the procedure to improve the purification of raw GLA species from EPO up to preparative scale, thus enabling use of this methodology for industrial purposes.