墨汁粉条的鉴别方法研究

采用气相色谱-质谱(GC-MS)和液相色谱-串联质谱(LC-MS/MS)技术,研究了墨汁粉条(假红薯粉条)及纯正红薯粉条中微量成分的差别。经GC-MS方法检测发现墨汁粉条中含有苯酚、六氢吡咯并[1,2a]吡嗪-1,4-二酮,用LC-MS/MS方法检测发现墨汁粉条中含有人工色素柠檬黄、日落黄和亮蓝,而纯正红薯粉条中不含以上物质。以该5种物质作为特征成分,建立了GC-MS和LC-MS/MS联合鉴别墨汁粉条的新方法。     

薄层色谱法检测甘薯呋喃萜类毒素

甘薯呋喃萜类毒素是甘薯受到损害后产生的强制性代谢产物,可用乙醚提取。乙醚提取物分别用５％Ｎａ２ＣＯ３和蒸馏水洗涤,无水硫酸钠干燥,蒸去乙醚。残渣（粗品）采用薄层色谱法进行检测,以纯品甘薯酮和甘薯酮醇作标样。结果表明：在２０℃条件下,在石油醚－醋酸乙酯（２１,Ｖ／Ｖ）和苯－甲醇（９１,Ｖ／Ｖ）两种溶剂系统中,对甘薯酮（Ｃ）、甘薯酮醇（Ａ）、化合物Ｂ和Ｄ的呋喃萜类毒素具有较好的分离效果,Ｒｆ值的重复性也较好。展开后的薄层板可以通过ＣＳ－９３０ＴＬＣ扫描仪在５２７ｎｍ下扫描定量。     

红薯与微量元素

红薯,又名叫地瓜、甘薯、番薯、白薯、甜薯、红苕、红芋等,属旋花科甘薯种、蔓生性草本植物,产量仅次于马铃薯,是世界十大农作物中第二位,我国从南到北、从东到西,广为种植,普遍食用。     

RP—HPLC法测定吡喹酮及其脂质体在小鼠体内的分布

应用RP-HPLC法测定吡喹酮及其脂质体在小鼠体内的分布。用外标定量法测定各组织中的含量,其回收率在96.46～103.13%之间,变异系数小于2.95%。实验结果表明,吡喹酮脂质体较游离吡喹酮在小鼠肝、脾组织内药物总含量明显增高,半衰期延长。     

红薯中铜铁微量元素测定

目的：测定三个品种红薯（黄心红薯、白心红薯、紫红薯）中Cu、 Fe微量元素含量。方法采用V（硝酸）＋V（高氯酸）＝4＋1体系分解样品,火焰原子吸收光谱法（ FAAS）测定。结果黄心红薯、白心红薯、紫红薯中Cu、 Fe微量元素均含量丰富,其Cu含量由大到小次序为：紫红薯,黄心红薯,白心红薯, Fe含量的由大到小次序为：黄心红薯,白心红薯,紫红薯。回收率在99.00％～104.00％之间, RSD＜2.2％。结论测定结果可为进一步研究红署营养价值与微量元素的关系提供参考。     

超高效液相色谱-串联质谱法测定红薯叶中15种功效成分

建立了超高效液相色谱-串联质谱（UHPLC-MS/MS）快速测定红薯叶中15种功效成分的分析方法。样品用80%（v/v）甲醇水溶液提取后,采用C₁₈色谱柱（100 mm×2.1 mm,1.8 μm）进行分离,以乙腈-0.15%（v/v）甲酸水溶液为流动相进行梯度洗脱,在电喷雾电离（ESI）源、负离子扫描模式下,通过多反应监测（MRM）模式检测各物质分子的离子峰。在各自的范围内15种功效成分线性关系良好,相关系数（r）为0.9995~0.9998;在3个加标水平下,15种化合物的回收率为82.2%~131.4%,相对标准偏差为3.6%~8.3%;方法的检出限为0.13~0.64 μg/L。该方法前处理简单,灵敏度高,适用于红薯叶中功效组分的快速分析,定量分析结果显示咖啡奎宁酸类物质是红薯叶中的主要功效成分。     

薄层色谱法分离烷基芳基酮肟立体异构体

我们对酮肟中间体及肟醚类拟除虫菊酯进行了分析。经核磁共振证明,酮肟中间体在生成肟醚南反应过程中其立体构型木发生变化。目前分离酮肟立体异构物的工作报道较少。我们通过薄层色谱对不同取代的具有活性的几种酮肟异构体的分离进行了探讨。 1 实验部分     

艾叶挥发性成分的提取及其化学成分的气相色谱/质谱分析

采用常温下氮气吹扫－固体吸附剂吸附和水蒸汽蒸饱辆途中方法,提慑富集区叶的近轨必成分,经气相色谱－质谱联机分析,鉴定出３９种化合物,主要是１,８－桉树脑、异蒿属（甲）酮、２－莰酮、２－莰酮、石竹烯、α－荜澄茄烯等。     

太湖沉积物中酮的提取、分离及GC-MS测定

用索氏抽提法提取了太湖沉积物中的可溶性有机质,用不同极性溶剂在硅胶／氧化铝柱上分离了饱和烃,芳烃,酮馏分。利用ＧＣ－ＭＳ对酮组份进行了分析。沉积物中检出了一系列呈等间距分布的正构烷基－２－酮：Ｃ１４至Ｃ３３,主峰为Ｃ２９,具有强烈的奇碳数优势。     

芦荟色酮的高速逆流色谱分离制备方法研究

芦荟色酮是在芦荟叶中特有的一类具有抗炎和抑制酪氨酸酶等作用的活性物质。以芦荟全叶为原料,经过一系列的预处理手段,从脱色剂活性炭中获得芦荟色酮粗提物,再经过溶剂分配和富集后采用高速逆流色谱（HSCCC）对其中的色酮成分进行分离纯化。研究结果表明,采用氯仿-甲醇-水(体积比为4∶3∶2)混合溶液和二氯甲烷-甲醇-水(体积比为5∶4∶2)混合溶液作为溶剂分离系统,经过两步HSCCC可以分离纯化出色谱纯度在95％以上的芦荟色酮单体。经过紫外检测、快原子轰击质谱及核磁共振等方法的结构分析鉴定,证实分离所得物质为肉桂酰基-C-葡萄糖甙芦荟色酮。     

快速色谱

基于柱液相色谱和薄层色谱之间的关系,讨论如何为快速色谱选择流动相,并介绍此技术手工操作的步骤.     

Extraction chromatography of common anions in liquid-liquid anion exchange systems. Part. III. Monobasic aliphatic organic acids and their sodium salts as eluants

Summary The chromatographic behaviour of anions on paper strips treated with tri-n-octylamine (TOA) salts or Aliquat 336 and developed with aqueous solutions of acetic, formic, monochloroacetic or trifluoroacetic acids and their sodium salts was investigated. Liquid-liquid extraction of organic acids by 0.1 M solution of TOA in benzene as well as the anion exchange between benzene solutions of TOA salts or Aliquat 336 (in acetate form) in benzene and aqueous solutions of sodium halides was also studied. It was found that extraction increases in the following order of the acids: CH₃COOOH<HCOOH<CH₂CICOOH<CF₃COOH; the relative affinity of organic anions to the quaternary alkyl-ammonium cation also increase in a similar order. The extraction of acid in excess over the amount necessary to neutralize the amine was observed for all four acids. The R_F values of anions investigated depend markedly on the type of organic acids or their salts and their concentration in the mobile phase. Halide ions are more strongly retained on paper treated with Aliquat 336 as compared with TOA salts. The chromatographic systems investigated offer many possibilities to separate various anion mixtures.Parts and II: refs. [1, 2].     

Unified chromatography: Fundamentals,instrumentation and applications†

The concept of unified chromatography has been in existence for 50 years after the work of Giddings proposing that all modes of chromatography (gas chromatography, liquid chromatography, supercritical fluid chromatography and so on) may be treated together under a single unified theory. His idea was partially fulfilled 23 years later by Ishii, Takeuchi and colleagues, who demonstrated for the first time the possibility to analyze a complex sample containing substances with a wide range of boiling points and polarities in the same instrument and column, just by varying the mobile phase pressure and temperature to change from one chromatographic mode to another. This approach has been demonstrated through application to the separation of complex mixtures in several areas including crude oil, edible oils and polymers. Still, unified chromatography has not yet been fully developed. In the present work, we will review the fundamentals, instrumentation and several applications of the technique. Also discussed are the drawbacks that still hinder development, as well as the recent developments and trends in instrumentation and columns that suggest the most feasible ways forward to the full development of unified chromatography.     

A review of advances in two-dimensional thin-layer chromatography

Although there are many simple thin-layer chromatography (TLC) separations, many more are complex and involve more than a few components, that means having to use special high-performance TLC (HPTLC) plates or microspotting or banding devices to increase its resolving power if developing in only one direction. However, adding a second development to perform two-dimensional TLC (2D TLC) allows even better resolution of complex samples. This is because different modes of chromatography are being invoked by the use of one stationary phase with two mobile phases, bilayer plates, graft TLC, or multidimensional TLC. This paper is a review of recent applications that have benefitted from using 2D TLC in its various forms. They were chosen for their variety of sample types as well as the unique choices of plates and/or mobile phases made by the researchers to yield improved separations.     

TLC as a pilot technique for the optimization of gradient HPLC II. Use of data obtained from RP-18 plates for the prediction of gradient programs in reversed-phase liquid chromatography

Summary A method is described and experimentally verified permitting the determination of the optimal gradient programs in HPLC on the basis of isocratic TLC data. The proposed method has many advantages and can also be used in reversed-phase systems. A satisfactory agreement between the theoretical and experimental of V_R/V_O values has been confirmed. Some discrepancies for more strongly retained solutes are, probably due to the respective equilibrium and nonequilibrium state of the column in isocratic and gradient elution.Part I: Ref. [1].     

Exhibition of the first gas chromatographic work of Erika Cremer and Fritz Prior

Summary In November 1995, theDeutsches Museum, the world's largest technical museum, opened a new branch in Bonn, devoted to achievements after 1945. There, the first gas chromatographic system used by Erika Cremer and Fritz Prior, in 1945–47, in Innsbruck, is exhibited. The new display is described and the early activities of Erika Cremer and her students are summarized.     

茶多酚的色谱分析法

 对茶多酚的主要成分――儿茶素的色谱分析法进行了综述。重点介绍了应用最多的反相高 效液相色谱法,同时简述了平板色谱法、气相色谱法以及目前出现的新的色谱分析方法。     

Affinity monolith chromatography: A review of general principles and recent developments

Affinity monolith chromatography (AMC) is a liquid chromatographic technique that utilizes a monolithic support with a biological ligand or related binding agent to isolate, enrich, or detect a target analyte in a complex matrix. The target-specific interaction exhibited by the binding agents makes AMC attractive for the separation or detection of a wide range of compounds. This article will review the basic principles of AMC and recent developments in this field. The supports used in AMC will be discussed, including organic, inorganic, hybrid, carbohydrate, and cryogel monoliths. Schemes for attaching binding agents to these monoliths will be examined as well, such as covalent immobilization, biospecific adsorption, entrapment, molecular imprinting, and coordination methods. An overview will then be given of binding agents that have recently been used in AMC, along with their applications. These applications will include bioaffinity chromatography, immunoaffinity chromatography, immobilized metal-ion affinity chromatography, and dye-ligand or biomimetic affinity chromatography. The use of AMC in chiral separations and biointeraction studies will also be discussed.