生产银杏黄酮的模拟移动床色谱工艺

世界各国银杏黄酮类药品的标度为总黄酮含量24％，生产工艺主要是浸取。现在国内有厂家提出制备高纯度银杏黄酮产品——总黄酮含量44％，生产工艺主要包括浸取和提纯两步，提纯主要采用树脂柱层析法。本文用模拟移动床色谱(Sinulated Moving Bed Chromatography,简称SMBC)提纯生产工艺，所得黄酮纯度可达90％以上。     

尿样中克仑特罗免疫亲和色谱-气/质联用检测方法的研究

以单抗为配基制备克仑特罗免疫亲和柱,建立了简单、快速、特异的样品净化技术,柱容量达到100 ng。偶联抗体量与柱容量呈线性关系,线性方程为:y=236.36x 6.6214,R2=0.9461。测定尿样中的克仑特罗,不需前处理直接用亲和柱提纯后以气质联用(GC/MS)方法检测。空白猪尿添加浓度为205、01、00 ng时,回收率分别为85%±1.3,85.9%±1.3,81.5%±2.7。同时以NY/XQ421-2003标准中净化方法为对照,回收率分别为113%±5.6,94.5%±10,78.6%±1.7,偶联非特异抗体的对照组亲和柱对样品保留值为7.03%。数据显示:免疫亲和柱作为提纯方法,与传统固相萃取提纯方法相比平行性好,提纯后样本杂质少。因此免疫亲和柱是净化样品的一个有效方法。     

聚酰胺-胺树枝状高分子的柱色谱提纯研究

采用发散法合成了0.5～4.0代(G)聚酰胺-胺(PAMAM)树枝状高分子,通过薄层色谱分析产物组成,并进一步选用柱色谱法对半代产物进行了提纯与精制.用红外,核磁,高效液相色谱(HPLC)和热重分析等方法对提纯后产物进行了表征.结果表明,提纯得到的各PAMAM产物具有较完整的分子结构,小分子含量很少;且0.5GPAMAM产物HPLC测试纯度达到97.81%.     

高速逆流色谱原理及其在天然产物化学成分分离中的应用研究进展

介绍了高速逆流色谱的分离原理,综述了自2005年以来其在天然产物化学成分分离、提纯方面的应用（引用文献59篇）。     

基于点击化学的色谱分离材料研究新进展

自诺贝尔奖获得者Sharpless教授2001年首次提出点击化学概念以来,该类反应凭借条件温和、反应迅速、产量高、副产物少、分离提纯简单等优势,迅速拓展至材料和生命等诸多科学领域,成为一种强大的模块化合成工具。目前,点击化学反应已成为设计制备分离材料的重要手段,展现出蓬勃发展的现状。本文首先简要地回顾了点击化学的发展历程并介绍了其独特优势,然后聚焦于柱色谱和膜色谱两大分离领域,系统地综述了近5年发表的基于点击化学的色谱分离材料相关报道,重点归纳了叠氮-炔、巯基-烯和巯基-炔这3种常见点击反应类型在色谱分离材料研究中的最新进展,最后对点击化学在开发高效分离材料方面的发展前景进行了展望。     

油菜籽中主要硫甙的分离提纯

用柱色谱方法从甘蓝型油菜籽中分离提纯了1-硫［(1Z)-3-羟基-1-［(磺酸基)亚氨基］-4-戊烯基］-1-硫代-β-D-葡萄糖钾盐(progoitrin)。用甲醇溶液提取菜籽中的硫甙,得到粗提物;粗提物经酸性氧化铝色谱柱与反相C18硅胶柱进一步分离提纯,得到纯品。对纯品进行紫外光谱、红外光谱、核磁共振氢谱、质谱和元素分析,测得的数据与文献值相符。用高效液相色谱测得硫甙提取物的纯度为99%。该方法操作简便,得到的硫甙样品纯度高,是一种有价值的硫甙提取方法,具有良好的应用前景。     

金属-有机骨架材料在色谱分离中的应用

金属-有机骨架材料（Metal-organic frameworks,MOFs）,因其具有较好的热稳定性、化学稳定性、可设计性等特点,广泛应用于气体吸附、物质分离、提纯、催化等领域,同时也作为模板制备各种功能材料.MOFs作为色谱分离的材料已得到了较多的研究与应用.按照被分离物质的类别,综述和总结了不同MOFs材料作为色谱固定相的分离效果,重点介绍了MOFs材料的色谱分离机理.MOFs材料的孔径、功能基团和不饱和金属位点在分离中起到重要的作用,最后对MOFs在色谱分离应用中的问题和前景进行了分析和展望.     

高效液相色谱法测定味精厂发酵渣中的氨基酸

建立了37种标准氨基酸混合液的分离方法,并以此分离条件测定发酵渣和大米中各种氨基酸含量,测定结果表明发酵渣中氨基酸含量是大米的六倍以上,可提纯作为营养品。 本法系离子交换色谱法,使氨基酸混合液通过锂柱,控制不同pH值的流动相进行梯度淋洗,使各种氨基酸分离,柱后依序加入次氯酸钠     

分离亲水气单胞菌外毒素的聚丙烯酰胺凝胶色谱填料

由丙烯酰胺和甲叉丙烯酰胺在水油悬浮液中共聚得到聚丙烯酰胺凝胶 (ZSP)系列 ,并用红外、溶剂吸收实验等对合成的ZSP的结构进行了研究。以商品葡聚糖凝胶SephadexG 10 0为对照 ,研究了ZSP 10对使中华鳖致病的亲水气单胞菌外毒素的分离性能。结果表明 :ZSP 10对毒素分离效率高 ,洗脱峰不拖尾 ,且结构和膨胀度可调 ,成本低廉 ,不易染菌霉变。经SephadexG 10 0和ZSP 10提纯的外毒素蛋白均保留了生物活性。根据SDS -PAGE的分析 ,确认经提纯的毒素蛋白的分子量为 3.2× 10 4     

异麦芽低聚糖浆的分离与测定

采用001×7(732)强酸性苯乙烯系阳离子交换树脂色谱分离法对异麦芽低聚糖(IMO)糖浆进行了分离提纯,并用HPLC分析测定其组成。试验表明,当进料量35 mL;操作温度71℃,洗脱速度9 mL.min-1,树脂柱9 mm×4 m,可以有效地去除葡萄糖等成分,提高异麦芽低聚糖的纯度。     

The Usefulness of Amino Acid Ester Isothiocyanate Derivatives in GLC Analysis,Pyrolysis Products of Carboalkoxydithiocarbamates

Abstract

Amino acid isothiocyanate derivatives have been used in GC/MS analysis. The best method providing these derivatives is decomposition of carboalkoxydithiocarbamates. Analysis by gas chromatography and mass spectrometry has shown that carbon oxysulfide, methanol, ethanol, amino acid ester isothiocyanate and trace carbon disulfide are pyrolysis products of amino acid ester carboalkoxydithiocarbamates. However, isothermal pyrolysis at 200° and direct MS analysis, FI and EI ionization modes, give rise to a few more by-products with m/z 145 and 177. This suggests a stepwise mechanism of thermal decomposition of the compounds studied. The number of by-products was seen to decrease when the R and R moieties were identical.     

间二氟苯溴化反应产物的气相色谱-质谱分析

采用气相色谱-质谱(GC/MS)法对间二氟苯溴化反应产物的组成与结构进行了分析,并对间二氟苯溴化反应的选择性及反应条件进行了初步探讨。结果表明:间二氟苯的溴化反应具有较强的选择性,其主要反应产物为1-溴-2,4-二氟苯,副产物为1-溴-2,6-二氟苯、1-溴-3,5二氟苯及二溴代间二氟苯等溴化物。该反应的反应条件对产物组成有较大影响。     

Determination of amino acid ratios in natural products by micellar electrokinetic chromatography

Summary Separation of dansyl and di-dansyl derivatives of amino acids present in natural products (corn seed flour, wheat flour fraction gliadine) is described. Problems with coelution of derivatization by-products and reagent with some dansyl amino acids (DNS-AA) were solved. A preconcentration step after derivatization of real sample is described. DNS-AA peak areas for different varieties of corn seed flour were compared. Di-dansyl histidine is not separated from di-dansyl lysine and didansyl tyrosine. Additional separation mechanisms have to be introduced to achieve separation of these three species.     

Identification of by-products in phenylisocyanate pre-column derivatization by thermospray liquid chromatography-mass spectrometry

Summary Thermospray liquid chromatography-mass spectrometry has been applied to the identification of by-products in precolumn derivatization by phenylisocyanate. These byproducts are eluted early in the same chromatographic region as the low molecular weight derivatives and were located by chromatographic analysis of a blank sample. Their identification would offer further qualitative information in the use of phenylisocyanate as a derivatizing agent. Five compounds resulted from the reaction of phenylisocyanate and the reaction medium were identified: two from a reaction between phenylisocyanate and methanol, two from the reaction between phenylisocyanate and water, and one from the polymerisation of phenylisocyanate.     

The use of tandem-mass spectrometry for pilot identification

Summary The direct analysis of mixtures by tandem-mass spectrometry assisted by off-line liquid chromatographymass spectrometry is already established as a rapid specific and extremely sensitive method that can be applied to samples of a variety of types for example, to analyses of main compounds and by-products in reaction mixtures, to products in medicated solutions or to fermentation products in more or less complex matrices. The techniques are demonstrated as pilot methods for obtaining structural information for identification or structure elucidation.     

Preparation of Amides of Carboxylic Acid Herbicides for Gas Chromatographic Analysis

Abstract

Amides of 14 carboxylic acid herbicides were prepared by reacting the free acid with the amine in toluene for 1 hr at 80[ddot]C in the presence of PCl₃ or P₂I₄. The acids include phenoxyacetic acids, arylacetic acids, and benzoic acids. Aniline, o-toluidine, 3,5-bis(trifluoromethyl)aniline, piperidine, and tetrahydroquinoline were the amine components. Excess of reagents and by-products of the reaction were removed by partitioning into aqueous acid and base. Retention times relative to 2,4-D anilide on 1% OV-22 and FSOT RSL-150 columns are listed for the anilides and should be useful for confirmation purposes. The anilides of 2,4-D, silvex and 2,4,5-T were obtained in better than 90% yield.     

离子色谱-抑制电导检测法同时测定草甘膦母液中的含磷副产物及无机阴离子

建立了一种抑制电导检测-离子色谱(IC)同时测定草甘膦生产工艺中母液里的草甘膦及其副产物、无机阴离子的方法。样品经过滤后直接进样,色谱条件: IonPac AS11-HC分离柱(250 mm×4 mm)和IonPac AG11-HC保护柱(50 mm×4 mm),在线淋洗液发生器KOH梯度淋洗,流速1.0 mL/min,采用抑制电导检测。草甘膦、甲基草甘膦、六甲基磷酰三胺(HMPA)、增甘膦、亚磷酸、磷酸、Cl~和SO2~4的线性范围分别为0.1～20 mg/L、0.1～20 mg/L、0.1～50 mg/L、0.25～50 mg/L、0.05～20 mg/L、0.2～50 mg/L、0.02～20 mg/L和0.05～50 mg/L,相关系数分别为0.9995、0.9993、0.9999、0.9998、0.9999、0.9985、0.9999和0.9980,加标回收率为93.7%～104.0%,相对标准偏差均小于2.5% (n=7),检出限(以信噪比(S/N)=3计)为0.002～0.025 mg/L。该方法用于草甘膦生产工艺中母液里草甘膦及其含磷副产物和无机阴离子的测定,结果令人满意。     

A four-electrode microconstant direct current resistance detector for ion chromatography applying ion-exchange membrane and porous electrode

A four-electrode microconstant direct current resistance detector for ion chromatography not sensitive to the effects of electrode polarization, capacitance, and electrolysis by-products is proposed. A constant current of microampere magnitude is applied across the current electrodes of the four-electrode device, and the voltage responses between the detection probes are directly picked up by a high input impedance instrumentation amplifier. The ion-exchange membranes, which separate the detection chamber from the electrolysis chambers, enable the measurement of solution resistance free of the interference of electrolysis by-products. Two resin beds in the detection chamber serve as ion conductors while reduce the dead volume of the detector. Recycled detection effluent supplies water for the electrolysis reactions at the current electrodes to sustain constant current in solution. The porous detection probes provide microchannel for the flowing solution while indicating signals. Owing to the constant current excitation, the electronics setup becomes simple. The cell configuration, operating principle, electronics, and error analysis of this detection mode are discussed along with their use for suppressed anion chromatography. Experimental data show that this four-electrode direct current detection mode is comparable to conventional two-electrode alternating current method.     

柱层析分离-气相色谱法测定脂肪酸甲酯乙氧基化物中二酯含量

采用硅胶柱层析-气相色谱法对月桂酸甲酯乙氧基化物(LME)中副产物二酯进行了定量分离与测定,同时考察了不同条件下合成的LME中二酯含量的变化规律。结果表明:LME中二酯含量随环氧乙烷(EO)加合数(n)的增加而先增大后趋平衡,当加合数n为8时,其质量分数为2.13%;并随反应温度升高而增大;随原料甲酯所含碳原子个数增加而降低。     

Ultra-high pressure LC determination of glucosamine in shrimp by-products and migration tests of chitosan films

Chitosan, a multiple applications molecule, was isolated from shrimp by-products by fermentation. The amount of chitosan in the solid fraction of the fermented extract was measured after its conversion in the respective glucosamine units. The procedure includes an acid hydrolysis (110 °C, 4 h with HCl 8 M) and a derivatization with 9-fluorenylmethyl chloroformate (Fmoc-Cl). Ultra-high-pressure liquid chromatography method was developed and optimized. Excellent peaks resolution was achieved in just 10 min. The method was evaluated in what concerns to validation parameters such as linearity, repeatability, quantification limit, and recovery. Migration tests of films prepared with chitosan were carried out in two simulants: ultrapure water and ethanol 95% (v/v).