吸附层析分离麻黄生物碱的过程优化

研究了用吸附层析取代现有的二甲苯萃取麻黄生物碱的工艺,重点考察了洗脱剂和操作条件对产品纯度和回收率的影响,发现在树脂吸附后的洗脱中,0．08M草酸的洗脱率最高,达99．3％,纯化倍数大于20;在操作条件中,进料量、pH和料液在层析柱中的停留时间影响最大：进料量增大导致纯度和收率的下降,树脂的动态吸附容量为27．5mg／mL树脂;停留时间在20rain时纯度较高,而洗脱率随停留时间减少却略有下降;pH=10时吸附性能较好。     

石蒜中总生物碱提取条件研究

通过研究用酸性醇溶液提取石蒜生物碱的方法和条件,结果表明,提取石蒜生物碱较佳的工艺条件是:提取液pH值1,提取时间为2h,提取液乙醇浓度为50%。     

黄连副产物中生物碱含量测定及提取工艺研究

目的:用HPLC对黄连生产副产物的生物碱含量进行测定,探究黄连生物碱在叶柄和须根中的分布。选择副产物生物碱的最佳提取工艺回收利用生物碱。方法:采用HPLC法建立黄连生物碱的含量测定方法,结合HPLC指纹图谱对黄连生产副产物进行生物碱含量测定。采用单因素试验法,分别对提取酸度、料液比和提取次数进行试验,分析并选取最佳提取条件。结果:黄连生产副产物中黄连生物碱的含量非常可观,其中黄连须含有大量的黄连生物碱,值得进一步开发利用。提取条件为:H2SO4浓度1.5%;料液比1∶15;提取时间1 h。结论:从黄连生物碱含量、资源的综合及可持续利用角度考虑,黄连生产副产物有很好的商业利用前景。     

正交试验法优化吴茱萸总碱的微波提取

以紫外-可见分光光度法为检测手段,研究了乙醇-水混合溶剂中吴茱萸总生物碱的微波提取条件,试验中分别以微波功率、萃取时间和萃取溶剂的用量、浓度及酸度等为因素,设计了五因素四水平的正交试验,考察了它们对总生物碱成分提取率的影响。结果表明,最佳提取条件为：在700W微波功率下,用浓度70％、酸度pH=2的乙醇-水混合溶剂25mL／g,提取6min,此条件下总生物碱的提取率可达0．4898％。     

微波辅助提取荷叶生物碱条件的优化

对荷叶中主要生理活性物质生物碱的提取条件进行了初步研究,以稀盐酸水为溶剂结合微波照射浸渍提取,获得了较优化的提取工艺,即用pH2.5 HCl、微波辅助处理2.5 min、固液比1:40、提取温度90℃、提取时间3 h,可得荷叶生物碱量172.63μg.g-1。     

苦参总生物碱提取工艺优化及杀蚜虫活性研究

目的：研究苦参总生物碱的提取工艺及杀虫生物活性。方法：以总生物碱含量为指标考察乙醇冷浸、乙醇渗漉、乙醇回流三种提取方法的提取效率差异,同时用正交设计对乙醇回流工艺条件进行优化,并以蚕豆蚜虫为供试靶标,探讨苦参总生物碱的杀虫生物活性。结果：乙醇回流提取效果较好,液料比、乙醇浓度、提取次数对提取效果均有影响,其最佳提取条件为：液料比12：1,乙醇浓度为60％,提取次数3次;苦参总生物碱对蚕豆蚜虫有一定的杀虫活性,其中氯仿直接提取物对蚜虫杀虫活性最好,随着总生物碱浓度降低,杀虫活性有下降。     

亳芍总生物碱提取及抑菌活性的研究

为了探讨亳芍总生物碱提取条件及其抑菌活性,在前期研究基础上,通过单因素和正交实验对亳芍总生物碱的提取条件进行了研究。采用滤纸片法对亳芍总生物碱提取物对大肠杆菌、金色葡萄球菌酵母菌及黑曲霉菌的体外抑菌活性进行初步测定。结果表明,亳芍总生物碱最佳提取条件为:乙醇浓度为60%,提取时间为3 h,提取温度为60℃,料液比为1∶20。此条件下,测得亳芍总生物碱的含量为0.58‰,提取的总生物碱对大肠杆菌、金色葡萄球菌及酵母菌、黑曲霉菌均有抑制作用,但抑菌效果不同,抑菌作用顺序为:金色葡萄球酵母菌黑曲霉菌菌大肠杆菌。     

苦参总生物碱提取工艺优化及杀蚜虫活性研究

目的研究苦参总生物碱的提取工艺及杀虫生物活性.方法以总生物碱含量为指标考察乙醇冷浸、乙醇渗漉、乙醇回流三种提取方法的提取效率差异,同时用正交设计对乙醇回流工艺条件进行优化,并以蚕豆蚜虫为供试靶标,探讨苦参总生物碱的杀虫生物活性.结果乙醇回流提取效果较好,液料比、乙醇浓度、提取次数对提取效果均有影响,其最佳提取条件为液料比121,乙醇浓度为60%,提取次数3次;苦参总生物碱对蚕豆蚜虫有一定的杀虫活性,其中氯仿直接提取物对蚜虫杀虫活性最好,随着总生物碱浓度降低,杀虫活性有下降.     

微生物方法生产麻黄碱和伪麻黄碱的研究

麻黄碱和伪麻黄碱是药用植物麻黄的主要生物碱类次生代谢产物,具有重要的药用价值.中国是世界上惟一通过天然植物提取麻黄碱的国家,该文简述了近年来利用微生物半转化、微生物直接转化和重组微生物制备麻黄碱的研究进展,对各自存在的问题进行了讨论,展望了微生物在麻黄碱和伪麻黄碱生物合成中的应用前景.     

亳芍总生物碱提取及抑菌活性的研究北大核心CSCD

为了探讨亳芍总生物碱提取条件及其抑菌活性,在前期研究基础上,通过单因素和正交实验对亳芍总生物碱的提取条件进行了研究。采用滤纸片法对亳芍总生物碱提取物对大肠杆菌、金色葡萄球菌酵母菌及黑曲霉菌的体外抑菌活性进行初步测定。结果表明,亳芍总生物碱最佳提取条件为:乙醇浓度为60%,提取时间为3 h,提取温度为60℃,料液比为1∶20。此条件下,测得亳芍总生物碱的含量为0.58‰,提取的总生物碱对大肠杆菌、金色葡萄球菌及酵母菌、黑曲霉菌均有抑制作用,但抑菌效果不同,抑菌作用顺序为:金色葡萄球>酵母菌>黑曲霉菌菌>大肠杆菌。     

茼蒿总黄酮提取及对羟自由基清除作用

采用超声波乙醇浸提法从茼蒿中提取黄酮类物质,对所提取的黄酮类物质进行验证,并用分光光度法测定含量,用茼蒿总黄酮对羟自由基清除作用进行试验。测得样品中总黄酮的含量C=0.169 0 mg/mL,回收率为101.3%,其纯度和产率均较高。该方法采用全物理过程,无任何污染,是提取茼蒿黄酮类物质的有效途径。茼蒿总黄酮提取液对Fenton体系产生的.OH自由基有很好的清除作用。     

Optimizing the Production of Antioxidant and Antibacterial Alkaloids from Macleaya cordata by Subcritical Water Extraction Technology

In this work, the subcritical water extraction technology was used to extract alkaloids from Macleaya cordata, and the effects of extraction temperature and time on its yield were investigated to find the best extraction conditions. Moreover, the antioxidant capacity and antibacterial activity of Macleaya cordata extract were studied. Furthermore, through the single-factor method, it was found that properly increasing the extraction temperature and prolonging the extraction time was conducive to increasing alkaloid yield. Still, a considerable amount of alkaloids might be decomposed by heat, resulting in a decrease in their yield. The results showed that the optimal extraction temperature of alkaloids from Macleaya cordata with subcritical water is 190 °C, the time is 45 min, and the corresponding maximum yield is 35.19±0.12 mg/g (sanguinarine equivalent in raw materials). In addition, the antioxidation and bacteriostasis abilities of subcritical water extract are better than those of traditional hot water extract, indicating that it is a feasible method to extract alkaloids from Macleaya cordata with subcritical water.     

Extraction behavior of caffeine and EGCG from green and black tea

A dipping method was developed to extract the catechins (EGCG) and alkaloids (caffeine) from green tea (Korea) and black tea (Sri Lanka). The effects of the solvent composition (water vs. ethanol), extraction time, temperatures, and solvent pH on the amount of catechins (EGCG) and alkaloids (caffeine) extracted from green and black tea were investigated. Reversedphase high-performance liquid chromatography (RP-HPLC) was used to analyze the catechins (EGCG) and alkaloids (caffeine) extracted. The content of EGCG and caffeine in green tea extracts was in the range of 2.04∼0.30 and 10.22∼0.85 mg/g, respectively. The amount of EGCG and caffeine in black tea extracts was in the range of 0.32∼0.24 and 5.26∼1.01 mg/g, respectively. The amount of caffeine extracted from green and black tea was greater than the amount of EGCG. Pure water is the best solvent for extracting EGCG and caffeine from green tea. The amount of caffeine extracted from green and black tea increased as the temperature, extraction time, and hydrogen ion concentration of the solvent increased. Although the amount of EGCG extracted from green tea increased as the temperature increased, the amount of EGCG extracted from black tea was not affected by temperature. The extraction of EGCG from both green and black tea was not affected by the hydrogen ion concentration of the solvent.     

Supercritical carbon dioxide extraction of colchicine and related alkaloids from seeds of Colchicum autumnale L

A method for the extraction of the alkaloids colchicine, 3-demethylcolchicine and colchicoside from seeds of Colchicum autumnale by supercritical carbon dioxide has been established. Several parameters such as pressure, temperature, percentage of modifier and extraction time have been examined. Two extraction steps with constant carbon dioxide density (0.90 g/mL) and flux (1.5 mL/min) were required to extract the alkaloids in 110 min using 3% methanol as modifier. The quantitative determination of the alkaloids was performed by HPLC; the percentages of recovery were higher than 98% for the three alkaloids. This extraction procedure was compared with a conventional method involving maceration and sonication, and the same levels of alkaloids were obtained in each case. The supercritical carbon dioxide method is, however, very efficient, more rapid and more environmentally friendly than conventional methods.     

超声波协同复合酶法提取姬松茸多糖

研究了超声波协同复合酶法提取姬松茸多糖的最佳工艺条件。采用均匀设计法分别考察不同时间、pH值、温度、酶浓度、固液比对纤维素酶、果胶酶以及木瓜蛋白酶酶解反应的影响,并研究三种酶联合使用时的加酶方式以及超声波协同提取时的最佳条件。结果表明,超声波协同复合酶法可显著提高姬松茸多糖的提取率,其最佳提取条件为：超声波作用20min,分步加酶法（先加果胶酶：pH值3．8、温度50℃、时间90min、加酶量7000U／g、固液比1：45;然后加纤维素酶：pH值3．6、温度75℃、时间120min、加酶量150U／g、固液比1：45;最后加木瓜蛋白酶：pH值3．6、温度75℃、时间120min、加酶量20000U／g、固液比1：45）,多糖提取率达到14．51％。     

Extraction and composition of three naturally occurring anti-cancer alkaloids in Camptotheca acuminata seed and leaf extracts

Naturally occurring camptothecins (CPT) are important sources of chemotherapeutic agents for clinical treatment of cancer. Extraction of CPT from Camptotheca acuminata trees remains to be a cost-effective way in the supply equation compared with a total synthesis. This study conducted a series of experiments to determine efficient solvent for the maximal extraction of CPT and its two derivatives, hydroxycamptothecin (HCPT) and methoxycamptothecin, from seeds and leaves of C. acuminata. Methanol as an extraction solvent demonstrated in seeds a significantly higher recovery of these three alkaloids than dichloromethane and acetone. Methanol concentrations at 70% in water resulted in maximum extraction of all the three alkaloids regardless of the type of plant materials. However, other strengths of methanol, lower or higher, either decreased the extracting power or showed no improvement in the extraction. Seed extract contained all the three alkaloids whereas leaf extract was absent of HCPT. A stable ratio of the three alkaloids was discovered but it was dependent upon seed or leaf extract of C. acuminata, which with various compositions can be produced. Ecological and medicinal implications of the leaf and seed extract characterized with different chemical compositions are discussed.     

伊乐藻生物碱的GC-MS分析及其对铜绿微囊藻的化感作用

藻类暴发性生长是水体富营养化带来的环境问题之一,利用植物化感作用抑制藻类生长作为一种新型的生物抑藻技术在近年来开始受到研究者的重视,并取得了一定的研究成果。文章采用GC-MS联用技术鉴定出伊乐藻中的9种生物碱成分,还研究了其总生物碱对铜绿微囊藻的化感作用。结果发现添加总生物碱的处理组中铜绿微囊藻生物量均受到了抑制,在总生物碱的浓度为62.0mg/L时,3d后铜绿微囊藻的抑制率为44.0%,表明伊乐藻总生物碱对铜绿微囊藻的生物量增长具有明显的抑制作用。该结论为通过沉水植物恢复富营养化水体提供了重要依据。       

甘肃棘豆草中苦马豆素的提取分离工艺比较研究

以甘肃棘豆草为试验材料,通过工业酒精热回流提取、水提取和酸水提取3种工艺提取其中的总生物碱,总生物碱经硅胶柱层析分离后减压升华得到,并比较了3种工艺对甘肃棘豆中总生物碱得率和苦马豆素得率的差异。结果表明,3种工艺总生物碱平均得率和苦马豆素平均得率依次分别为7.91、6.79、6.22 mg/g和18.61、12.22、6.23μg/g,由此确定工业酒精热回流为提取苦马豆素的最佳提取分离工艺。     

生川乌中生物碱成分含量随煎煮时间变化的研究

本文研究乌头中生物碱成分的含量随煎煮时间变化的趋势,为考查乌头类中药的毒性,提供定量指标.按不同时间水煎提取样品;分别采用容量法、比色法和薄层扫描法测定总生物碱、双酯性生物碱和乌头碱的含量.生川乌醇水双提总生物碱含量最高,水提样品中以煎煮4 h较高;生川乌醇水双提酯性生物碱含量最高,水提样品中以煎煮2 h为最高,比双提酯性生物碱含量低;生川乌醇水双提乌头碱含量最高,水提样品中以煎煮2h为最高,比双提乌头碱含量低.为乌头类中药的毒性研究提供了详细的参考指标.     

Determination of Aconitum alkaloids in blood and urine samples: II. Capillary liquid chromatographic–frit fast atom bombardment mass spectrometric analysis

Determination of fourteen alkaloids, toxic Aconitum alkaloids, aconitine, mesaconitine, jesaconitine, hypaconitine and deoxyaconitine, and their hydrolysis products, benzoylaconines and aconines, have been established using capillary liquid chromatography (LC) fast atom bombardment mass spectrometry (FAB-MS) with a frit interface. Protonated molecular ions were observed as base peaks in the FAB-MS for these fourteen alkaloids. All the alkaloids were simultaneously quantified with linear gradient LC elution by solvent mixture of acetonitrile and 0.3% trifluoroacetic acid using selected ion monitoring of the protonated molecular ions. The calibration curves of these alkaloids were linear in injection amounts ranging from 5 to 500 pg, and their detection limits were 1 pg per injection (S/N=3). Solid-phase extraction using Sep-Pak Plus PS-1 was also investigated to clean-up and concentrate alkaloids in blood and urine samples, and showed satisfactory recoveries. This capillary LC–frit-FAB-MS method enables determination of low levels of Aconitum alkaloids in blood and urine samples, coupled with solid-phase extraction.