大孔树脂吸附分离长春花中的文多灵、长春质碱和长春碱

通过对11种国产大孔树脂对文多灵、长春质碱和长春碱的静态吸附容量和解吸率等指标的考察,筛选出AB-8大孔吸附树脂作为分离长春花生物碱的载体,其对文多灵、长春质碱和长春碱吸附量分别为365.8、254.2、24.8 mg·ml^-1。利用大孔吸附树脂吸附分离长春花3种生物碱的过程为：长春花原料用稀硫酸溶液提取,提取液用氨水调节pH值为8,然后采用AB-8大孔吸附树脂柱吸附,用20%乙醇洗涤除去强极性成分,在30℃下用pH=4的50%乙醇解吸,得单吲哚生物碱文多灵和长春质碱,再用90%乙醇解吸,得双吲哚生物碱长春碱。单吲哚生物碱纯度可达50%以上,长春碱纯度达60%以上。     

苦参碱农药标准品研制

[目的]使用萃取、碱性氧化铝柱层析与重结晶相结合的方法研制苦参碱标准品。[方法]首先采用氨氯法萃取制备苦参总生物碱,然后采用碱性氧化铝柱层析法,对苦参总生物碱进行分离纯化,使苦参碱含量达到92%以上,最后结合重结晶方法进行纯化。[结果]苦参碱标准品含量98.16%。[结论]使用氨氯法萃取、碱性氧化铝柱层析与重结晶相结合的方法制得苦参碱标准品,其含量大于市售苦参碱标准品含量,符合标准品要求。     

负压空化强化提取长春花中生物碱的工艺参数优化

采用负压空化法对长春花中的生物碱进行提取研究,以长春花中3种主要生物碱长春碱、文多灵和长春质碱的提取率评价提取效果,考察了提取溶剂、pH值、酸性调节物,提取时间、料液比和提取次数等因素对提取效果的影响.结果表明:以pH值为1.5的硫酸50%甲醇溶液作为提取溶剂,料液比1:10,空化提取25 min,空化提取3次时,提取效果最好;与其它提取方法相比,负压空化法更适合用于含量低但价格昂贵的长春碱的提取,提取率达到0.082‰.     

钯催化的3,3’-螺-2-吲哚酮的合成研究

以Pd（OAc）2为催化剂,三叔丁基膦为配体,以NaOt-Bu为碱,通过2-吲哚酮的分子内芳基化反应,以93%的收率合成得到3,3’-螺碳环-2-吲哚酮化合物。     

UPLC-ESI-Q-TOF-MS~E快速鉴定钩藤中吲哚类生物碱

目的通过超高效液相色谱与飞行时间质谱联用技术(UPLC-ESI-Q-TOF-MS~E)快速鉴定和分析钩藤中吲哚类生物碱成分。方法采用色谱柱:HSS T3(100mm×2.1mm,1.8μm,Waters),流动相采用A为0.1%甲酸水溶液,B为乙腈,梯度洗脱。流速为0.4m L·min~(-1),进样量为4μL,正离子MSE扫描模式检测。结果通过对照品数据对照、元素组成分析和碎片结构分析,并结合相关文献,鉴定了9种吲哚类生物碱分别为a.卡丹宾碱、b.二氢卡丹宾碱、c.异去氢钩藤碱、d.柯诺辛碱、e.去氢钩藤碱、f.钩藤碱、g.缝籽嗪甲醚、h.去氢毛钩藤碱、i.毛钩藤碱,并分析其裂解规律。结论 UPLC-ESI-Q-TOF-MS~E可用于快速鉴定钩藤中吲哚类生物碱,为钩藤饮片的质量控制提供了技术支持。     

1-烷基吲哚-3-乙酸的合成

以吲哚-3-乙腈为原料,经过与卤代烷在碱存在下的N-烷基化和碱水解2步反应分别合成了1-甲基吲哚-3-乙酸(2a)和1-[3-(四氢-2H-吡喃-2-氧基)丙基]-1H-吲哚-3-乙酸(2b),总收率分别为87%和68%,其结构经1H NMR和Ms确证。     

牛心朴子草中生物碱的抑制植物病毒活性研究

牛心朴子草广泛分布于我国西北旱沙荒漠地带,笔者发现其提取物中生物碱部位对危害极大的烟草花叶病毒(TMV)具有很高的抑制活性。生物活性跟踪与色谱分离、结构鉴定确认该生物碱属于菲并吲哚里西啶,活性成份为安托芬(1)和6-羟基-2,3-二甲氧基菲并吲哚里西啶(2)。此外,还分离得到另外三种生物碱。构效关系表明氮上孤电子对和菲环对高的抗病毒活性是必要的。     

吲哚的分离精制技术

住金化学公司鹿岛工厂利用二甘醇对萘塔底油(洗油)与甲基萘进行共沸蒸馏, 共沸残液中 含有13％的吲哚。通过对吲哚分离精制方法的研究, 提高了吲哚的回收纯度, 现介绍如下。1 吲哚的分离精制1.1 吲哚分离精制方法的概况对工业萘塔底油(洗油)进行脱碱处理后, 用二甘醇进行共沸蒸馏, 切去吲哚前馏分和除去 多余的二甘醇, 再精馏制取吲哚。精馏所得的吲哚用水和甲醇进行再结晶, 制取高纯吲哚。1.2 吲哚的浓缩脱碱后, 洗油中的大部分成分在用二甘醇共沸蒸馏时与吲哚分离, 其主要成分的沸点和共 沸温度见表1。洗油用二甘醇进行共沸蒸馏时, 可获得…     

新疆白喉乌头中4种生物碱的分离鉴定及含量测定

采用硅胶柱层析、硅胶柱色谱法等手段对白喉乌头的95%乙醇提取物中的化学成分进行了分离纯化,通过¹HNMR、¹³CNMR对分离得到的4种生物碱的结构进行了鉴定,并采用HPLC法同时测定了其含量。结果表明,从白喉乌头的95%乙醇提取物中共分离得到4个二萜生物碱,分别鉴定为：8-去氧刺乌头碱、异刺乌头碱、高乌甲素、冉乌头碱,其中异刺乌头碱为首次从白喉乌头中分离得到;3批白喉乌头药材中8-去氧刺乌头碱、异刺乌头碱、高乌甲素、冉乌头碱的平均含量分别为0.026 mg·g^-1、0.124 mg·g^-1、1.143 mg·g^-1、0.561 mg·g^-1,其中高乌甲素的含量最高。     

芦竹碱合成新工艺的研究

报道了芦竹碱新的合成方法，由吲哚与甲醛和二甲胺缩合而制得芦竹碱，经重结晶后其含量为98％。收率为95％。     

Structure of the Bis‐Indole Alkaloids Tabernaemontabovine and Tabernaemontavine — A Revision

The structures of the bis‐indole alkaloids tabernaemontabovine ( 1 ) and tabernaemontavine ( 2 ) have been revised on the basis of APT, ¹H‐¹H COSY, gradient‐selected HSQC and gradient‐selected HMBC spectra.     

茄秆中生物总碱提取条件的研究

以茄秆为原料,用索氏提取法进行生物总碱的提取,用酸碱滴定法对提取的生物总碱的含量进行测定。以生物总碱的含量作为指标,进行单因素试验,研究了有机溶剂种类、料液比、提取时间、pH值等因素对茄秆中生物总碱提取的影响。茄秆生物总碱的优化条件为: 60% 乙醇为提取剂,料液比为1:5.5, pH值为3,时间为 3 h,生物总碱平均含量为 1.96%。在优化条件下提取效果稳定、可重复性高。     

双水相萃取分离苦参生物碱

用乙醇、聚乙二醇和Triton X-100与硫酸铵等无机盐构建双水相体系,研究了各体系的形成过程与性质及对氧化苦参碱和苦参碱的萃取性能,发现乙醇/硫酸铵双水相体系稳定、分相快、萃取率高,更适合苦参生物碱的萃取;对其萃取条件的优化结果表明,乙醇和硫酸铵分别为38%(w)和18%(w),体系pH值为7.0,30℃下搅拌萃取15 min,氧化苦参碱与苦参碱的分配系数和萃取率分别为4.46和5.10,96.17%和95.74%. 在苦参的水提取液中直接用该体系萃取分离氧化苦参碱、氧化槐果碱、槐定碱、苦参碱及槐果碱5种生物碱,萃取率为91.03%~94.46%,三级错流总萃取率为97.22%~98.78%;该体系用于苦参生物碱的纯化,可显著减小杂质含量,苦参碱含量可提高1倍以上,其焓变DH0和熵变DS0均大于0,且DG0<0,表明萃取过程为吸热熵增的自发过程.     

正交实验法优选苦豆籽总生物碱的纯化工艺

用紫外分光光度法测定苦豆籽总生物碱的含量,以总生物碱的质量为评价指标,采用单因素实验和正交实验对其纯化工艺进行优化。结果表明,苦豆籽总生物碱的最佳纯化条件为:HCl酸化的pH=4.0,NaOH溶液为碱化剂,碱化pH=9.0,氯仿为苦豆籽总生物碱萃取剂且萃取比例为1∶5。在最佳纯化条件下,总生物碱含量达28.98%,收率为1.73%左右。     

Gewinnung und Entbitterung von Speiseöl und Proteinkonzentrat aus Samen von Lupinus mutabilis

Production and Debittering of Edible Oil and a Protein Concentrate from Seeds of Lupinus mutabilis Lupine oil was produced from seeds of L. mutabilis using an extraction and refining process of soya oil. The refining included a step of debittering by washing with diluted acids. This decreased the alkaloid content from 0.14 % in the raw oil to 5 ppm in the endproduct, a content of rest alkaloids, which can be considered as unobjectionable. The oil alkaloids are not identical with those of the seeds. While in seeds Lupanin is the main alkaloid fraction, in the oil 13-Hydroxylupanin and N-Methyl angustofolin are dominant. The raw oil contained 800 ppm γ-Tocopherol 39 ppm α-Tocopherol. During the refining process the Tocopherol content decreased from about 840 ppm to 530 ppm total Tocopherol in the endproduct. The oil-cake contained about 4 % alkaloids. With aqueous alcohol (70 %?90 % ethanol) was debittered to a protein concentrate, which contained 73% protein and 0.06% rest alkaloids. By changing the pH value of the debittering medium both in the acid (pH 5) and alkaline (pH 9) range the alkaloid extraction could be improved and the loses of protein could be diminished. Qualitatively the alkaloid pattern of the protein concentrate was similar to that of seeds, although the hydroxylupanin fraction increased from 32.7% of total alkaloids before the debittering to 42.3% in the debittered concentrate. This is advantageous because the toxicity of hydroxylupanin is only about 1/10 of that of Lupanin.     

微波辅助提取牡丹雄蕊总生物碱工艺研究

采用微波辅助法提取牡丹雄蕊中的总生物碱。考察了料液比、浸润时间、微波加热提取时间、微波功率、pH值和乙醇浓度等对提取率的影响。结果表明,牡丹雄蕊总生物碱的最佳提取工艺条件为:料液比1∶20,浸润时间24 h,微波加热提取时间15 min,微波功率500 W,pH值3和乙醇浓度80%。在此最佳工艺条件下,牡丹雄蕊中总生物碱提取率为2.16%。     

Lupin protein concentrates by extraction with aqueous alcohols

In order to remove the toxic quinolizidine alkaloids and other nonprotein constituents, hexane-defatted flakes of lupin (Lupinus mutabilis) were extracted under various conditions with ethanol, methanol or their aqueous solutions. Lupin protein concentrates containing more than 70% protein and 0.1–0.2% alkaloids were obtained in high yields by consecutive extractions, countercurrent extraction or semicountercurrent extraction of the defatted lupin flakes with either 80% ethanol or 80% methanol.     

混合溶剂提取催吐萝芙木水溶性生物碱的工艺研究

用混合溶剂提取法研究催吐萝芙木水溶性生物碱的浸提工艺。考察了不同混合溶剂对水溶性生物碱提取率的影响,确定了丙酮-水（v：v=10：1）混合溶剂为适宜溶媒,并通过正交实验,确立了该溶媒提取催吐萝芙木水溶性生物碱的优化条件：8倍量的混合溶剂,提取时间10h,温度40℃,pH=10。在优化后的条件下,采用该混合溶剂对水溶性生物碱提取率为3．22％,是采用乙醇的1．35倍,蒸馏水的1．69倍。     

Separation and Purification of Indole in Model Coal Tar Fraction of 9 Compounds System

Separation and purification of indole present in model coal tar fraction was examined by the combination of extraction to separate indole from the crude model coal tar fraction, distillation to obtain high concentration of indole in the extract, and solute crystallization (SC) to obtain high-purity indole present in indole-enriched distillate. The model fraction was made up of four types of nitrogen heterocyclic compounds (quinoline, iso-quinoline, 4.66% indole, and quinaldine), three types of bicyclic aromatic compounds (1-methylnaphthalene, 2-methylnaphthalene, and dimethylnaphthalene), biphenyl, and phenyl ether. Aqueous solutions of formamide and n-hexane were used as the extraction solvent and the SC solvent, respectively. Through the combination of formamide extraction, distillation, and SC using n-hexane in this work, 99.5% indole was recovered. We confirmed that the combination examined by this work was one of the very useful combinations for the high-purity purification of indole present in the coal tar fraction.