大孔硼酸基聚苯乙烯树脂分离果葡糖研究

通过偶氮反应将氨基苯硼酸共价连接到聚苯乙烯载体上,制备了硼酸基聚苯乙烯载体.研究了实验条件对载体吸附果糖能力及载体分离柱分离效果的影响,确定了最佳洗脱条件.以长径比为175:1的分离柱,于室温下用pH6.1的二次水以0.16mL/min的流速进行洗脱,成功地将42%的果葡糖分离,果糖纯度达到99%.     

高效液相色谱法测定果低聚糖中的糖含量

以ＹＷＧ－ＮＨ２色谱柱和ＲＩＤ－６Ａ示差折光检测器对果低聚糖进行高效液相色谱法（ＨＰＬＣ）分析，获得了良好的分离效果。结果表明：果低聚糖糖浆中含有３０％～３５％的葡萄糖和５５％～５８％的果低聚糖（包括三糖、四糖和五糖），此外，还含有少量的果糖和蔗糖。ＨＰＬＣ能准确、快速地定性、定量果低聚糖中各组分糖，方法灵敏度高、重现性好，有理想的回收率，单糖和低聚糖的最低检出限在微克级     

高效液相色谱法测定果低聚糖中的糖含量

 以ＹＷＧ－ＮＨ２色谱柱和ＲＩＤ－６Ａ示差折光检测器对果低聚糖进行高效液相色谱法（ＨＰＬＣ）分析，获得了良好的分离效果。结果表明：果低聚糖糖浆中含有３０％～３５％的葡萄糖和５５％～５８％的果低聚糖（包括三糖、四糖和五糖），此外，还含有少量的果糖和蔗糖。ＨＰＬＣ能准确、快速地定性、定量果低聚糖中各组分糖，方法灵敏度高、重现性好，有理想的回收率，单糖和低聚糖的最低检出限在微克级。     

ICP-MS 法测定高纯氧化铕中稀土杂质的研究

深入考察了ＩＣＰ－ＭＳ法测定高纯氧化铕时基体对稀土杂质测定的影响,研究了Ｐ５０７萃淋树脂分离大量基体Ｅｕ２Ｏ３的实验条件,建立了采用内标补偿直接测定大部分稀土杂质和经Ｐ５０７萃淋树脂分离基体后测定被干扰离子Ｔｍ相结合的高纯Ｅｕ２Ｏ３中稀土杂质的ＩＣＰ－ＭＳ分析方法。方法检出限为０．００５～０．０２１μｇ／Ｌ,加标回收率为８４％～１１２％。ＲＳＤ为１．４％～８．１％。本法适用于质量分数为９９．９９％～９９．９９９９％的高纯Ｅｕ２Ｏ３中稀土杂质的分析。     

离子选择电极法测定对氟聚苯乙烯聚合体中的氟含量

本文研究了分解对氟聚苯乙烯聚合体的条件,建立了用离子选择电极法测定对氟聚苯乙烯聚合体中氟含量的方法,对氟苯甲酸加标回收率为９９．９％,对氟聚苯乙烯分析结果的相对标准偏差为２．７％,方法简便,准确。     

含西佛碱键的多羟基树脂的合成及对硼酸的吸附性能

分别用亲水性的聚乙烯胺和疏水性的聚苯乙烯为载体，合成了一系列含不同长度间隔臂的多羟基螯合树脂，并讨论了树脂对硼酸的吸附、洗脱性能，结果表明树脂在中性、弱酸性条件下可较好地吸附硼酸；吸附速率与载体的亲水性和间隔壁长度有关；测定了吸附反应表观活化能以及吸附硼酸后可用０．５Ｎ盐酸洗脱。     

高效毛细管电泳技术测定肌苷口服液的含量

介绍了应用高效毛细管电泳技术测定肌苷口服液含量的方法。实验是将肌苷口服液直接进样,以硼酸－硼酸盐为缓冲溶液。实验的回收率为９５．０％～９９．８％,相关系数０．９９８５,精密度的变异系数小于５％。方法简便、快速、准确、灵敏度高。     

2—乙基己基膦酸单（2—乙基己基）酯萃淋树脂分离—火花源质谱法测定…

本文采用萃取色谱法以２－乙基己基膦酸单（２－乙基己基）酯（Ｐ５０７）萃淋树脂为固定相，以ＨＣｌ－ＮＨ４Ｃｌ体系为淋洗液，研究了９９．９９９％￣９９．９９９９％的高纯Ｙｂ２Ｏ３中稀土杂质和Ｙｂ基体的分离条件，将杂质淋洗液富集于复合螯合剂－活性碳上，经灼烧灰化后制成样品电极，进行质谱测定。测定下限达０．０１￣０．０５μｇ／ｇ，可用于高纯Ｙｂ２Ｏ３中杂质的测定。回收率在８０％以上。     

用金属离子处理多孔Al2O3载体对葡萄糖异构酶固载化的影响

1.前言 葡萄糖异构酶可以催化D-葡萄糖转化为D-果糖的反应。近年来,酶和细胞固定化技术得到迅速发展。用固定化葡萄糖异构酶生产果葡糖浆是目前世界上将固定化酶大规模用于工业生产最有成效的范例。对于异构酶的固定化,文献业已发表上百种的方法,但是工业上实际采用的只有戊二醛交联法、载体吸附法、包埋法以及细胞凝聚法等七、八种,其中以多孔无机载体吸附法制备的固定化葡萄糖异构酶生产能力最高。     

蓝靛果的化学成分及其提取分离研究进展

蓝靛果（Lonicera cearulea L.）是一种天然野生的可食用浆果,具有清除自由基、抑制炎症通路相关蛋白的磷酸化、抑制癌细胞增殖等生理活性,其抗氧化、调节血脂、抗肿瘤和防辐射等保健功效可应用于调节肠道菌群结构、抗癌、抗肥胖和保护视力等多个功能食品领域,且蓝靛果抗寒能力强,易于种植,具有极高的市场开发价值。研究总结整理了蓝靛果中活性化学成分（原花青素类、花青素类、花色苷类、黄酮类、有机酸类、多糖类及其它类化合物）的化学信息,归纳整理了不同类型化学成分的提取分离技术（溶剂提取法、酶解法、微波辅助提取法等）,以期为蓝靛果深入研发及深加工产品的开发提供依据。     

Separation and purification of isorhamnetin 3-sulphate from Flaveria bidentis (L.) Kuntze by counter-current chromatography comparing two kinds of solvent systems

The first preparative separation of a flavonoid sulphate isorhamnetin 3-sulphate from Flaveria bidentis (L.) Kuntze by counter-current chromatography (CCC) was presented. Two kinds of solvent systems were used. A conventional organic/aqueous solvent system n-butanol-ethyl acetate-water (4:1:5, v/v) was used, yielding isorhamnetin 3-sulphate 2.0 mg with a purity of 93.4% from 83 mg of pre-enriched crude extract obtained from 553 mg ethanol extract by macroporous resin. A one-component organic/salt-containing system composed of n-butanol-0.25% sodium chloride aqueous solution (1:1, v/v) was also used, and the LC column packed with macroporous resin has been employed for desalination of the target compound purified from CCC. As a result, 2.1 mg of isorhamnetin 3-sulphate with a purity of over 97% has been isolated from 402 mg of crude extract without pre-enrichment. Compared with the conventional organic/aqueous system, the one-component organic/salt-containing aqueous system was more suitable for the separation of isorhamnetin 3-sulphate, and purer target compound was obtained from the crude extract without pre-enrichment using the new solvent system. The chemical structure was confirmed by ESI-MS and (1)H, (13)C NMR. In summary, our results indicated that CCC using one-component organic/salt-containing aqueous solution is very promising and powerful for high-throughput purification of isorhamnetin 3-sulphate from Flaveria bidentis (L.) Kuntze.     

Preparative separation of high-purity cordycepin from Cordyceps militaris(L.) Link by high-speed countercurrent chromatography

A high-speed counter-current chromatography (HSCCC) technique in a preparative scale has been applied to separate and purify cordycepin from the extract of Cordyceps militaris(L.) Link by a one-step separation. A high efficiency of HSCCC separation was achieved on a two-phase solvent system of n-hexane-n-butanol-methanol-water (23:80:30:155, v/v/v/v) by eluting the lower mobile phase at a flow rate of 2 ml/min under a revolution speed of 850 rpm. HSCCC separation of 216.2 mg crude sample (contained cordycepin at 44.7% purity after 732 cation-exchange resin clean-up) yielded 64.8 mg cordycepin with purity of 98.9% and 91.7% recovery. Identification of the target compound was performed by UV, IR, MS, (1)H NMR and (13)C NMR.     

Separation of D‐psicose and D‐fructose using simulated moving bed chromatography

Simulated moving bed (SMB) processes have been widely used in the sugar industries with ion‐exchange resin as a stationary phase. D ‐Psicose, a rare monosaccharide known as a valuable pharmaceutical substrate, was synthesized by the enzymatic conversion from D ‐fructose. The SMB process was adopted to separate D ‐psicose from D ‐fructose. Before the SMB experiment, the reaction mixture including D ‐psicose and D ‐fructose was treated by a deashing process to remove contaminants, such as buffers, proteins, and other organic materials. Four columns packed with Dowex 50WX4‐Ca²⁺ (200–400 mesh) ion‐exchange resins were used in the four‐zone SMB. Single‐step frontal analysis was performed to estimate the isotherm parameters of each monosaccharide. The operating conditions of the SMB process were determined based on the Equilibrium Theory. According to the simulation of the SMB process, the purity and yield of extract product (D ‐psicose) achieved were 99.04 and 97.46%, respectively and those of raffinate product (D ‐fructose) were 99.06 and 99.53%, respectively. Under the optimized operating condition, complete separation (extract purity = 99.36%, raffinate purity = 99.67%) was achieved experimentally.     

Separation and purification of neohesperidin from the albedo of Citrus reticulata cv. Suavissima by combination of macroporous resin and high-speed counter-current chromatography

In this article, a simple and efficient protocol for rapid preparation and separation of neohesperidin from the albedo of Citrus reticulata cv. Suavissima was established by the combination of macroporous resin column chromatography and high-speed counter-current chromatography (HSCCC). Six types of resin were investigated by adsorption and desorption tests, and D101 macroporous resin was selected for the first cleaning-up procedure, in which 55% aqueous ethanol was used to elute neohesperidin. After treatment with D101 resin, the neohesperidin purity increased 11.83-fold from 4.92% in the crude extract to 58.22% in the resin-refined sample, with a recovery of 68.97%. The resin-refined sample was directly subjected to HSCCC purification with a two-phase solvent system composed of ethyl acetate-n-butanol-water (4:1:5, v/v), and 23.6 mg neohesperidin with 97.47% purity was obtained from 60 mg sample in only one run. The recovery of neohesperidin in HSCCC separation procedure was 65.85%. The chemical structure of the purified neohesperidin was identified by both HPLC and LC-MS. The established purification process will be helpful for further characterization and utilization of Citrus neohesperidin.     

大孔树脂-高速逆流色谱分离纯化薇甘菊中的黄酮类化合物

该文建立了大孔树脂-高速逆流色谱分离薇甘菊中黄酮类物质的方法。分离条件为:采用大孔树脂AB-8,洗脱液为50%（v/v）乙醇水溶液,高速逆流色谱溶剂体系为正丁醇-乙酸-水（4：1：5,v/v）。从薇甘菊中分离到4种黄酮类物质:槲皮素-3-O-芸香糖苷（纯度90.2%）、山奈酚-3-O-芸香糖苷（纯度98.55%）、木犀草苷（纯度98.33%）和紫云英苷（纯度99.23%）。建立的大孔树脂-高速逆流色谱方法简单、高效,可扩展应用于从其他植物中分离黄酮类物质。     

Separation of capsaicin from capsaicinoids by macroporous resin adsorption chromatography

The aim of present study is to develop an efficient and low‐cost method for capsaicin production isolated from capsaicinoids by macroporous resin adsorption chromatography. HZ816 resin has shown the best adsorption and desorption capacities for capsaicin among other resins. To optimize the operating parameters for separation, initial concentration, diameter‐to‐height ratio, mobile phase ratio, and crystallization method were investigated. When capsaicinoids solution (5 g/L) was loaded onto the column (diameter‐to‐height ratio = 1:12) with ethanol/1% w/w NaOH (4:6, v/v) as the mobile phase, capsaicin was purified most effectively. By using acid neutralization as the crystallization method, the purity of capsaicin improved from 90.3 to 99.5% with 82.3% yield. In conclusion, this study provides a simple and low‐cost method for the industrial‐scale production of high‐purity capsaicin.     

Separation and purification of glucosinolates from crude plant homogenates by high-speed counter-current chromatography

Glucosinolates are anionic, hydrophilic plant secondary metabolites which are of particular interest due to their role in the prevention of cancer and other chronic and degenerative diseases. The separation and purification of glucosinolates from a variety of plant sources (e.g. seeds of broccoli, arugula and the horseradish tree), was achieved using high-speed counter-current chromatography (HSCCC). A high-salt, highly polar system containing 1-propanol-acetonitrile-saturated aqueous ammonium sulfate-water (1:0.5:1.2:1), was run on a semi-preparative scale and then transferred directly to preparative scale. Up to 7 g of a concentrated methanolic syrup containing about 10% glucosinolates was loaded on an 850-ml HSCCC column, and good separation and recovery were demonstrated for 4-methylsulfinylbutyl, 3-methylsulfinylpropyl, 4-methylthiobutyl, 2-propenyl and 4-(rhamnopyranosyloxy)benzyl glucosinolates. Multiple injections (5 to 6 times) were performed with well-preserved liquid stationary phase under centrifugal force. Pooled sequential runs with broccoli seed extract yielded about 20 g of its predominant glucosinolate, glucoraphanin, which was produced at > 95% purity and reduced to powdered form.     

Isolation and purification of baicalein, wogonin and oroxylin A from the medicinal plant Scutellaria baicalensis by high-speed counter-current chromatography

The medicinal plant Scutellaria baicalensis Georgi has been used widely in traditional Chinese medicine for anti-inflammation, anticancer, antiviral and antibacterial infections, reducing the total cholesterol level and decreasing blood pressures. A high-speed counter-current chromatography (HSCCC) method was developed for the preparative separation and purification of three bioactive flavonoids, namely, baicalein, wogonin and oroxylin A, from S. baicalensis Georgi. Preparative HSCCC with a two-phase solvent system composed of n-hexane-ethyl acetate-n-butanol-water (1:1:8:10, v/v/v/v) was successfully performed by increasing the flow-rate of the mobile phase stepwise from 1.0 to 2.0 ml min(-1) after 4 h. The components purified and collected were analyzed by high-performance liquid chromatography. The method yielded 144.8 mg of baicalein at 95.7% purity, 50.2 mg of wogonin at 98.5% purity, and 12.4 mg of oroxylin A at 93.2% purity from 500 mg of the crude extract in a one-step separation. The recoveries of baicalein, wogonin and oroxylin A were 92.7%, 91.6% and 92.5%, respectively.     

制备型高效液相色谱法分离纯化川西獐牙菜提取物中的龙胆苦苷

龙胆苦苷(GPS)是龙胆类药材及其相关制品质量控制的指标成分。本研究利用制备型高效液相色谱从川西獐牙菜提取物中分离纯化龙胆苦苷对照品。对制备色谱的流动相组成、流速、进样量和检测波长等制备参数进行了优化。采用的色谱柱为C18柱(200 mm×50 mm, 5 μm),流动相为甲醇和0.1%乙酸水溶液(体积比为30:70),流速为75 mL/min,检测波长为254 nm,进样体积为500 μL。在30 min的运行时间内,龙胆苦苷与其他干扰成分得到了很好的分离,产品纯度达到了99%以上。此方法具有快速高效、产品纯度高的特点,可用于制备龙胆苦苷对照品和对龙胆苦苷制品的质量控制。