大孔树脂分离纯化大麻果胶中的总黄酮

目的 研究不同型号大孔吸附树脂纯化大麻科植物汉麻果胶中总黄酮的工艺条件及参数.方法 以总黄酮静态饱和吸附量、静态洗脱率为考察指标,对8种大孔吸附树脂的吸附工艺条件进行筛选.结果 D-101树脂具有最佳的吸附及洗脱参数,其最佳工艺为:上样浓度0.6 g生药/ml,以10倍去离子水、10倍70%乙醇依次进行洗脱,流速为2 ...     

大孔吸附树脂分离纯化鲜地黄叶中梓醇的初步研究

目的：选择合适的大孔吸附树脂对鲜地黄叶中梓醇进行富集纯化。方法：以高效液相为检测手段,梓醇含量为检测指标。采用吸附和解吸试验考察了12种大孔吸附树脂对梓醇的吸附解吸性能,筛选出H103树脂进行了分离纯化研究。结果：H103树脂对梓醇具有很好的吸附解吸性能,其纯化条件为上样液浓度1mg/ml,上样体积2BV,上样吸附速度1～2BV/h,洗脱速度1～3BV/h,10%乙醇洗脱8BV。结论：采用H103树脂分离纯化鲜地黄叶中梓醇,可简化步骤,降低成本,方法简单可行。     

大孔树脂纯化艾叶总黄酮的研究

目的研究不同型号大孔树脂纯化艾叶总黄酮的工艺条件及参数。方法以静态饱和吸附量、洗脱量、静态洗脱率为考察指标,比较了5种大孔树脂,以总黄酮的转移率和含量为指标对树脂吸附工艺条件进行了筛选。结果所比较的5种大孔吸附树脂中,AB-8树脂具有最佳的吸附及洗脱参数,其最佳工艺为：上样液浓度为4．42mg·mL^-1,上样液pH值为4．0,用70％乙醇以3mL/min速度洗脱。总黄酮转移率约为82％,其含量约为64％。结论AB-8树脂综合性能较好,适合于艾叶中总黄酮的分离纯化。     

大孔树脂分离治伤灵口服液中芍药苷的研究

目的 研究D101大孔树脂对治伤灵口服液中芍药苷的吸附性能及分离纯化的工艺参数。方法采用HPLC法测定芍药苷含量,通过考察pH值对吸附的影响、吸附容量、洗脱剂选择及其用量等因素对芍药苷分离纯化的影响,确定工艺参数。结果D101大孔树脂对芍药苷的适宜交换吸附条件为pH=4,最大上柱量以芍药苷计为3．661mg·g^-1树脂,水洗除去杂质,洗脱剂为40％乙醇溶液,用量为8个柱体积（BV）。结论D101大孔树脂能提高芍药苷纯度,为芍药苷含量测定提供保证。     

延胡索乙素的制备工艺及药理作用研究进展

延胡索乙素广泛存在于天然植物元胡（延胡索）、千金藤、黄叶地不容、黄藤、夏天无等。提取纯化工艺有：有机溶剂提取酸碱处理萃取法，有机溶剂提取酸碱处理柱层析分离法，超临界二氧化碳萃取法，大孔树脂吸附法，阳离子树脂交 换法，有机溶剂提取结晶法。半合成主要是还原法。其主要特点是利用生物碱的酸溶碱沉的性质,然后萃取出总碱再柱层析 分离得到产品。延胡索乙素的药理作用主要有：镇痛麻醉作用;抗心律失常、降血压、对心肌保护作用;对脑缺血再灌注损伤 的保护作用;对血小板聚集性的抑制作用;抗溃疡病，抑制胃酸分泌;抗肿瘤作用;对成瘾药物的戒断作用等。关于募药理作 用还需继续加强研究。     

HPLC法测定夏天无中原阿片碱延胡索乙素和巴马亭

目的建立测定夏天无药材中的原阿片碱,延胡索乙素和巴马亭的HPLC方法。方法采用反相高效液相色谱法测定夏天无药材中原阿片碱、延胡索乙素、巴马亭的含量。应用Diamonsil C18色谱柱,流动相为乙腈-0．2％冰醋酸（21：79,三乙胺调节pH4．5）,检测波长282啪。结果3种生物碱的线性范围分别为1．896～75．84、1．97—78．8、1．346—67．32μg·mL^-1;平均回收率分别为101．29％、100．77％、100．54％,RSD均〈1．5％。结论反相高效液相色谱法专属性强,操作简单,结果准确,重复性好,可用于夏天无药材中的多种生物碱的的同时测定。     

丹参中丹酚酸B纯化工艺研究

摘要：目的对丹参药材中丹酚酸B的提取工艺进行研究，比较两种大孔树脂的吸附能力和洗脱能力。方法以丹酚酸B为考察指标，用反相高效液相色谱法考察了丹参药材在6倍量水时的最佳提取时间以及丹参提取液在两种大孔树脂吸附工艺中的最大吸附量和最佳洗脱条件。结果丹参水煮提取时间以40min时，丹酚酸B含量最大。AB-8型大孔树脂最大吸附量是16．8mg·g^-1，最佳洗脱浓度是50％的乙醇，最佳洗脱体积是4BV；1400型树脂的最大吸附量是17．2mg·g^-1，最佳洗脱浓度是60％的乙醇，最佳洗脱体积是5BV。结论利用大孔树脂精制丹参水溶性成分，在有效地保留丹酚酸B等有效成分的同时，可有效减少丹参提取物中非酚酸类及杂质的含量，有利于提高制剂载药量。为丹参水溶性成分新制剂的工业化生产应用确定基础。     

大孔树脂吸附法分离丹酚酸

目的筛选大孔树脂吸附法分离丹酚酸的最佳条件。方法采用动态吸附-解吸方法,用HPLC法测定丹酚酸B的含量对工艺进行评价。结果采用ZTC-1型大孔吸附树脂,上柱量按每毫升树脂吸附7.95mg丹酚酸B计算,以4倍柱体积水洗脱;收集30%乙醇洗脱液,约为6倍柱体积。总丹酚酸得率为7.9%,含丹酚酸B为77.8%。结论该法简单可行,分离效果好,可为工业生产提供参考数据。     

大孔吸附树脂分离纯化何首乌有效成分二苯乙烯苷的研究

目的研究不同型号大孔吸附树脂纯化何首乌中二苯乙烯苷的工艺条件及参数。方法以静态饱和吸附量、洗脱量、静态洗脱率为考察指标,比较了7种大孔树脂,并对HPD500树脂的动态比上柱量、比吸附量、比洗脱量进行了考察,以二苯乙烯苷转移率和纯度为指标对树脂吸附工艺条件进行了筛选。结果所比较的7种树脂中,HPD500型树脂具有最佳的吸附及洗脱参数,其动态饱和吸附量达到151.7mg·g-1干树脂,其最佳工艺为以6倍柱体积去离子水、4倍柱体积10%乙醇、6倍柱体积60%乙醇依次洗脱,二苯乙烯苷转移率为95%,其纯度为75.3%。结论HPD500树脂吸附性能较好,适合于何首乌中二苯乙烯苷的纯化。     

大孔吸附树脂对半枝莲中黄酮类成分的分离研究

目的以半枝莲中黄酮类成分为分离对象,进行大孔树脂分离工艺优化和分离研究。方法采用溶剂提取法对半枝莲中有效成分进行提取,以其总黄酮的含量为指标,比较4种不同种类大孔树脂(D1400,HPD-100,D101,NKA-2)的吸附性能。并选择吸附性能最优的大孔树脂分离半枝莲中的黄酮类组分,结合HPLC进行分析检测。结果采用70%乙醇水溶液提取(药材溶剂比为1∶8),得到理想的出膏率11.67%(g/g)。UV法测定结果表明,半枝莲提取物中黄酮类成分含量较高18.34%(mg/g)。D101树脂对总黄酮的吸附率最高52.9%(mg/mg)。结论半枝莲中黄酮类成分含量较高,采用D101型大孔树脂分离能够达到理想的吸附效果,总黄酮成分主要集中在大孔树脂分离的20%乙醇水溶液洗脱组分中。     

Removal of the 2.2.2 cryptand (kryptofix 2.2.2™) from 18FDG by cation exchange

The 2.2.2 cryptand [4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo-(8.8.8)-hexacosane] was trapped efficiently on Dowex AG50W-X8 (100–200 mesh) cation exchange resin. The concentration of the 2.2.2 cryptand in water with 0.1–2% methanol, or in 1 N HCl, was decreased by a factor of >4000 using 1 mL (1.7 mequiv.) of AG50W-X8 and a flow rate of approx. 2 mL/min. K⁺, Cs⁺, Ag⁺ and Ba²⁺ forms were about equal in their ability to remove the 2.2.2 cryptand. A disposable cartridge containing 1 mL of hydrogen form resin was inserted into our automated ¹⁸FDG system so that the hydrolysate (in 2 cm³ of 1 N HCl) would pass through the cartridge before final purification. No cryptand was detected in the final product as determined by TLC with idoplantinate visualization. The detection limit was 2.5 μg/mL. Less than 3% of the total starting radioactivity was retained by the cation column. Quality assurance tests including apyrogenicity, sterility, radiochemical purity, carbohydrate composition and pH were not compromised by the incorporation of the cryptand removal cartridge.     

A simplified procedure for fluorine-18 production using a nuclear reactor

Several target compounds and different purification procedures are compared for reactor production of [¹⁸F]fluoride by means of the ⁶Li(n,α)³H; ¹⁶O(t,n)¹⁸F reaction sequence. Best results are obtained using moist Li₂CO₃ as target, followed by aqueous dissolution using a cation exchange resin and purification by adsorption on a small alumina column with dilute ammonium hydroxide as eluent.     

住友CLC模块在线优化合成^13N-NH3· H2O的研究

目的 确定住友HM-10回旋加速器相关参数,小步优化住友CLC模块,合成显像良好的^13N-NH3· H2O.方法 优化住友HM-10回旋加速器的束流大小、轰靶时间和靶水中乙醇去自由基含量,提高化学反应效率.用阳离子交换柱（CM柱）吸附靶水和小步优化纯化流程得到高化学纯度的^13N-NH3·H2O,并实现一根CM柱上多次吸附纯化（3次左右）.结果 用30 μA束流轰击10 mmol/L乙醇11 min,合成^13N-NH3·H2O 27批次,产量为925 MBq左右,放化纯度和化学纯度均大于99％,注射大狗后心肌灌注显像良好.结论 经过回旋加速器锂靶反应条件的优化和住友CLC纯化模块的小步改进能得到产量稳定、显像良好的^13N-NH3· H2O,能够满足实验及临床要求.     

A column-switching LC/MS/ESI method for detecting tetrodotoxin and Aconitum alkaloids in serum

A liquid chromatography-mass spectrometry-electrospray ionization (LC/MS/ESI) method coupled with a column-switching technique has been developed for the determination of tetrodotoxin (TTX) and Aconitum alkaloids and their metabolites, such as aconitine, mesaconitine, hypaconitine, jesaconitine, benzoylaconine, benzoylmesaconine, benzoylhypaconine and 14-anisoylaconine, in serum. An on-column column-switching technique was employed to analyze TTX and Aconitum alkaloids and their metabolites without pretreatment of the serum. Combination of a multimode column with reversed phases and cation exchange for TTX, and use of a multimode column with reversed phases and a hydrophobic polymer column for Aconitum alkaloids and their metabolites provided successful separation and MS determination in ESI positive mode. A 100 microl serum sample was directly injected into a precolumn. For TTX monitored at m/z 320.1 in the selected ion monitoring mode, the calibration curve was linear within the range 0.1-100 ng/ml and the limit of detection was 0.1 ng/ml. For aconitine, mesaconitine, hypaconitine and jesaconitine, linear calibration curves were obtained up to 500 ng/ml and the limit of detection ranged from 0.2 to 1 ng/ml. For benzoylaconine, benzoylmesaconine, benzoylhypaconine and 14-anisoylaconine, linear calibration curves were obtained up to 500 ng/ml and the limit of detection ranged from 2 to 50 ng/ml. Recoveries from serum samples were within the range 78-119% for all the compounds studied.     

Production of actinium-225 for alpha particle mediated radioimmunotherapy.

The initial clinical trials for treatment of acute myeloid leukemia have demonstrated the effectiveness of the alpha emitter (213)Bi in killing cancer cells. Bismuth-213 is obtained from a radionuclide generator system from decay of 10-days (225)Ac parent. Recent pre-clinical studies have also shown the potential application of both (213)Bi, and the (225)Ac parent radionuclide in a variety of cancer systems and targeted radiotherapy. This paper describes our five years of experience in production of (225)Ac in partial support of the on-going clinical trials. A four-step chemical process, consisting of both anion and cation exchange chromatography, is utilized for routine separation of carrier-free (225)Ac from a mixture of (228)Th, (229)Th and (232)Th. The separation of Ra and Ac from Th is achieved using the marcoporous anion exchange resin MP1 in 8M HNO(3) media. Two sequential MP1/NO(3) columns provide a separation factor of approximately 10(6) for Ra and Ac from Th. The separation of Ac from Ra is accomplished on a low cross-linking cation exchange resin AG50-X4 using 1.2M HNO(3) as eluant. Two sequential AG50/NO(3) columns provide a separation factor of approximately 10(2) for Ac from Ra. A 60-day processing schedule has been adopted in order to reduce the processing cost and to provide the highest levels of (225)Ac possible. Over an 8-week campaign, a total of approximately 100 mCi of (225)Ac (approximately 80% of the theoretical yield) is shipped in 5-6 batches, with the first batch typically consisting of approximately 50 mCi. After the initial separation and purification of Ac, the Ra pool is re-processed on a bi-weekly schedule or as needed to provide smaller batches of (225)Ac. The averaged radioisotopic purity of the (225)Ac was 99.6 +/- 0.7% with a (225)Ra content of < or =0.6%, and an average (229)Th content of (4(-4)(+5)) x 10(-5)%.     

Sensitive determination of pentazocine in human tissues by high-performance liquid chromatography

The authors developed a simple, reliable and sensitive method for the determination of pentazocine in human solid tissues using high-performance liquid chromatography, combined with a three-step liquid-liquid extraction procedure. Levallorphan tartrate served as the internal standard. The extract was evaporated to dryness and dissolved in the mobile phase of acetonitrile/10 mM phosphate buffer (pH 4.0). The eluent was pumped at a flow rate of 0.4 ml/min through a Spherisorb Ph (2.1 mm I.D. x 150 mm) column. A fluorescence detector with excitation at 247 nm and emission at 320 nm was used. The lower limit of detection was about 0.5 ng/g. The calibration curve was linear over the concentration ranges from 1 to 500 ng/g in each tissue examined and could be determined up to at least 10.0 microg/g by means of reduction of injected volumes. Using this method, the concentrations of pentazocine could be determined in the tissues of an autopsied individual for toxicological evaluation.     

不同型号大孔树脂对分蘖葱头总黄酮吸附的研究

目的 研究不同型号大孔吸附树脂分离纯化分蘖葱头总黄酮的工艺条件和参数,优选分离纯化分蘖葱头总黄酮的大孔吸附树脂。方法 比较了9种大孔树脂对分蘖葱头总黄酮的吸附性能,以分蘖葱头中的代表成分槲皮素为考察指标,对大孔树脂纯化分蘖葱头的工艺进行筛选。结果 AB-8树脂对分蘖葱头总黄酮的吸附性能最好,达到静态交换容量为36．05mg·g^-1干树脂,吸附率为97．29％,动态吸附量为5．07mg·g^-1干树脂,吸附率为83．3％,解吸率为76．9％。结论 AB-8树脂吸附分蘖葱头总黄酮的纯化方法可取,具有良好的应用前景。