薄层色谱分离库仑滴定法测定杀虫单

本文提出了用薄层色谱库仑滴定法测定杀虫单（ＳＣＤ）［ＣＨ３）２ＮＨＣ Ｈ（ＣＨ２Ｓ２Ｏ３）２Ｎａ．Ｈ２Ｏ］的方法。试样中的各成分用上行展开法的硅胶Ｇ板上分离，用碘蒸气或喷洒ＰｄＣｌ２溶液确定ＳＣＤ的位置，该试剂与杀虫单反应生成橙黄色产物。     

药物分析中薄层色谱的方法认证

在药物分析中,针对所要求的性能参数,对一个薄层色谱程序的各个环节必须进行的认证方法和认可标准进行了讨论。建议当提出结果报告时,应附上关于对方法的认证参数和认证方法的说明。     

微乳液在生物碱薄层色谱分析中的应用

以十二烷基硫钠－正丁醇－正庚烷－水微乳液作为一咱全新的展开剂,进行了４１种生物碱的薄层色谱分析。研究结果不明,当微乳液为油包水型和双连续型（含水量１５％～６０％）时,具有与有机溶剂相似的作用,生物碱的Ｒf值多为０．２～０．８之间,层析结果满意。通过调节微乳液的含水量,即能获得适宜的展开系统,可用于生物碱的分离鉴定。     

Atomic Layer Deposited Ti2O3 Thin Films

Ti₂O₃ thin films have been prepared through atomic layer deposition and subjected to electrical resistivity measurements as a function of temperature. The as-prepared films were stable for up to three weeks. In Ti₂O₃ thin films, the insulator-metal transition is observed at ∼80 K, with nearly 3–4 orders of magnitude change in resistivity. The anomalous increase in electrical resistivity in the films is in accordance with the two-band model. However, the energy interval between the bands depending on the crystallographic c/a ratio leads to a change in electrical resistivity as a function of temperature.     

十二烷基硫酸钠/正丁醇/正己烷/水微乳液在氨基酸薄层色谱中的应用

薄层色谱法;十二烷基硫酸钠/正丁醇/正己烷/水微乳液在氨基酸薄层色谱中的应用     

薄层色谱法应用于N-乙基-对-薄荷烷-3-甲酰胺的分离和鉴别

研究了用薄层色谱法分离和鉴别在合成N-乙基-对-薄荷烷-3-甲酰胺中所得粗品的各组分。试验表明硅胶H(60型)为最佳吸附剂。敷有此吸附剂的薄层层析板经在110℃活化2 h,所用展开剂为以5与1之比混合的石油醚和丙酮混合溶剂,展开距离最少为14.00 cm,经展开后粗品中4组分得到很好的分离。展开层用碘铋化钾(KBI4)溶液和碱性高锰酸钾溶液喷洒即可清楚地观察到4个色斑,其Rf值依次为0.82,0.67,0.50和0.33,即Rf为0.33的色斑取下作元素分析,所得结果证明此组分即是N-乙基-对-薄荷烷-3-甲酰胺。     

一种新的展开剂用于氨基酸的薄层色谱分析

以十六烷基三甲基溴化铵(CTAB)/正丁醇/正辛烷/水微乳液作为一种新的展开剂,对23种氨基酸进行了薄层色谱分析。研究了微乳液含水量和氨基酸分子结构对Rf值的影响;同时选择含水量为40%的微乳液对氨基酸混合物进行了分离鉴定并与传统的展开剂作了比较;此外还探讨了微乳色谱理论。研究结果表明,当微乳液为油包水型及油水双连续型时,氨基酸的Rf值多在0.2与0.8之间,色谱分析结果令人满意。     

Quantitative Thin Layer Chromatography of Amino Acids Using Fluorescamine Reagent

Abstract

Calibration curves are presented for several different types of amino acids to illustrate the quantitation of these compounds by in situ fluorescence densitometry on thin layer plates.     

乙酰丙酮衍生化／薄层扫描法测定水中痕量脂肪二胺

将水中痕量脂肪二胺用乙酰丙酮衍生化，经固相萃取后以薄层扫描法测定含量。考察了实验条件及衍生物的光谱特性对测定灵敏度的影响。此方法的最小检测浓度是５￣９μｇ／Ｌ，回收率为８８％￣１０１％。     

胶束薄层色谱法测定食品及药用胶囊中的合成食用色素

在聚酰胶片上以13%SDBS(十二烷基苯磺酸钠)+7%Triton X-100〔聚乙二醇-对-(1.1,3,3-四甲基)丁基苯基醚〕+(2+3)氨水(1+5+1)为展开剂,用胶束薄层色谱法分离和测定了柠檬黄、亮蓝、苋菜红、胭脂红和赤藓红。测定波长分别为440、632、535、525和528 nm,线性范围分别为0.1～2、0.05～1、0.05～1、0.05～1和0.05～1μg/斑点。方法用于测定软饮料糖果及药用胶囊中的合成色素,获得了满意的结果。此外,还对展开剂的最佳组成进行了单纯形法优化。     

维生素B类药物在薄层原位的近红外付立叶变换表面增强拉曼光谱

维生素Ｂ类药物在薄层原位的近红外付立叶变换表面增强拉曼光谱汪瑗，于秉正张煦（首都师范大学分析测试中心北京１０００３７）（北京大学分析测试中心北京）关键词维生素Ｂ_１，维生素Ｂ_２，薄层色谱，表面增强拉曼散射，近红外付立叶变换拉曼光谱将薄层色谱（ＴＬＣ）...     

薄层色谱分离和分光光度法测定桃叶珊瑚甙

提出在冰醋酸－９５％乙醇（１：２,Ｖ／Ｖ）溶液中,以Ｅｐｓｔａｈｌ试剂为显色剂测定桃叶珊瑚甙的分光光度法。最大吸收波长为６０１ｎｍ。对于杜仲叶提取物中的桃叶珊瑚甙,以甲醇－氯仿－石油醚－乙酸乙酯为展开剂,用薄层色谱法予以分离,用分光光度法进行测定。     

薄层色谱法分析2-丙烯酰胺基-2-甲基丙烷磺酸

应用薄层色谱法对工业品２ 丙烯酰胺基 ２ 甲基丙烷磺酸（简称ＡＭＰＳ）进行了分析,以硅胶ＧＦ２５４作为吸附剂,从几种溶剂系统中优选了Ｖ（苯）∶Ｖ（甲醇）＝２∶１溶液作为展开剂,用２５４ｎｍ紫外分析仪检测展开后的样品斑点。实验表明：ＡＭＰＳ的Ｒｆ为０３６,而其主要杂质丙烯酰胺（ＡＭ）的Ｒｆ为０．６４;ＡＭＰＳ的最小检出限为５μｇ,展开时间约为２５ｍｉｎ。方法简便、快速、重现性好,有利于在生产过程中快速分析ＡＭＰＳ及其所含杂质,从而指导对ＡＭＰＳ的纯化处理。     

Thin Layer Chromatographic Detection and Separation of Metal Ion Complexes with Tridentate Schiff Base

The Tridentate chelating, system present in Salicylidine o-amino benzoic acid was used for complexation with Cu (11), Ni (11), Co (11) and Pd (11). The thin-layer chromatographic (TLC) detection and separation of these complexes on Silica gel (G) layers was studied. The coloured spots of the complexes were quite visible without any visualizing agent. A maximum of four complexes could be resolved and identified. The coloured zones were eluted with solvent and characterise by elemental analysis and spectral studies. Colour of the complexes at λ_max was measured.     

胶束薄层扫描法测定黄连及其制剂中的小檗碱、巴马汀和药根碱

以2％CPC-醋酸乙酯(9：1)胶束溶液为展开剂,在聚酰胺薄膜上成功地分离了小檗碱、巴马汀和药根碱。以345nm为测定波长,550nm为参比波长进行扫描测定,建立了一种新的同时测定黄连及其制剂中小檗碱、巴马汀和药根碱的胶束薄层扫描法。小檗碱、巴马汀和药根碱的线性范围分别为0．2—2．4、0．1—1．0和0．1—1．0μg;回收率分别为97．7％-99．4％、101．7％～102．6％和96．7％-97．8％;相对标准偏差分别为1．4％-1．7％、1．9％-2．7％和1．8％-2．2％。     

苯酚和苯胺类衍生物的结构与薄层色谱保留值关系的研究

以不同比例的己烷－乙酸乙酯二元体系作为展开剂,在硅胶板上测定了２４种苯酚和苯胺类衍生物的比移值Ｒｆ。用斜交因子分析方法将这２４种化合物分为具有不同特征的两大类：第一类的苯环上均不含甲基,而第二类的苯环上均含甲基。第一类化合物的比移值均比第二类要小;苯环上取代基团使Ｒｆ值增大的顺序为ＣＨ３＞ＯＨ＞ＮＨ２;邻位取代的化合物,由于分子内形成氢键,极性减弱,因而比移值增大。分别对两类化合物的保留值与其拓扑指数进行多元回归分析的结果表明,它们的色谱保留行为与其分子结构之间存在着较好的相关性。     

液相沉积法制备光催化活性掺铁TiO2薄膜

 通过在氟钛酸铵－氟铁酸混合溶液中加入硼酸溶液，应用液相沉积法制备了具有高光催化活性的掺铁TiO2薄膜．用ICP－AES测定了掺铁TiO2薄膜中Fe3＋的浓度，用XRD，AFM，UV－Vis和阶梯仪等对TiO2薄膜的沉积条件、结构、膜厚和性能进行了表征，并以亚甲蓝降解反应评价了掺铁TiO2薄膜的光催化活性．结果表明，在硼酸／六氟钛酸铵摩尔比为2～4时，掺铁TiO2薄膜中含有锐钛矿相TiO2．当掺Fe3＋浓度为0．05％，热处理温度为300℃时，掺铁TiO2薄膜具有最高的光催化活性，其光催化活性是未经热处理时的3．9倍，是经300℃热处理但未掺铁TiO2薄膜的1．4倍．     

Structural studies of Na-montmorillonite exchanged with Fe2+, Cr3+, and Ti4+ by N2 adsorption and EXAFS

The structures of Fe(2+)-, Cr(3+)-, and Ti(4+)-modified montmorillonite prepared from ion exchange of the Na-clay with Fe(2+), Cr(3+), and Ti(4+) were investigated. Conventional BET surface area and spectroscopic analysis by extended adsorption fine structure (EXAFS) were applied. It was shown that the BET surface area of Na-clay was similar to that of Fe-clay, but somewhat different from those of Cr- and Ti-clay; it decreased in the order Na- > Fe- > Ti- > Cr-montmorillonite. This sequence appeared to be consistent with the ion size Na(+) (0.95 nm)>Fe(2+) (0.65 nm)>Cr(3+) (0.62 nm), except for Ti(4+) (0.69 nm). EXAFS data showed that some Si atoms within montmorillonite were replaced by Ti atoms and that a neostructure of titanium oxide was formed.     

Quantitative Separation of Zr4+ from La3+ and Ce3+; W6+ from Cr3+, Mo6+ and VO2+ by Thin Layer Chromatography

Abstract

Methods have been developed for the quantitative separation of Zr⁴⁺ from La³⁺ and Ce³⁺ using 0.1M ammonium oxalate solution as eluant. W⁶⁺ can also be separated quantitatively from Cr³⁺, Mo⁶⁺ and VO²⁺ using DMSO-1MHC1 (1:9). Both the methods are fast and quantitative. The separation takes about 40–50 min. The average error is about 3%.