用网格搜索寻优法选择分离6种青霉素类药物的薄层色谱溶剂系统

用网格搜索寻优法确定了分离６种青霉素类药物的薄层色谱溶剂系统。采用均匀设计法安排初始实验，借助计算机进行网格搜索寻优计算，在硅胶ＧＦ（２５４）板上成功地分离了青霉素钠、苯唑青霉素钠、磺苄青霉素钠、氨苄青霉素钠、氧哌嗪青霉素钠和羧苄青霉素钠，方法简便、有效。     

Sample Solvent as Analyte in High Performance Liquid Chromatography

Abstract

Solvents vary in their behavior in high performance liquid chromatography (HPLC). Water and methanol, among others, are widely used in the mobile phase as well as solvents for the solute. Few reports indicate that the solvent used for the solute can behave as an analyte. Normally, it is generally accepted that the solute solvent, a non-constituent of the mobile phase will be the first eluent. However, a solvent which is a component of the sample can show up as an unexpected peak with its own identity. This solvent may show a similar retention time as some of the unknown components of the sample. This indicates that in some cases the quantitative results may be the sum of the absorptivity of the solute and solvent used for the sample. It is assumed that some solvents show no absorption in the ultraviolet region at which the analysis is being conducted. Depending on the mobile phase composition some solvents can be detected at the wavelengts or wavelengths used for analysis. Water, ethylacetate, and methanol showed absorption at 210 nm when present in the sample being analyzed with a mobile phase of acetonitrile-methanol using a C₁₈ column. These solvents overlapped or showed retention times the same as estriol and testosterone.     

遗传算法用于液相分离条件的优化

 在参考传统的优化方法的基础上 ,将遗传算法用于等度反相多元流动相分离条件的优化。详细介绍了基于线杂交和面变异的遗传算法的原理及其用于液相分离条件优化的过程。将此法用于 9种小肽的反相离子对分离条件的优化 ,经过 3次寻优操作 ,确定了最佳分离条件 ,实验保留值与预测值的平均相对偏差为0 75 % ,优化结果比较理想。     

高效液相色谱溶剂系统四面体优化法

改进了Ｇｌａｊｃｈ的三角形法,建立了适合于高效液相色谱（ＨＰＬＣ）的四面体优化法。将７个溶剂系统的实验结果输入计算机,由计算机模拟２３１个溶剂系统的色谱行为,优选出最佳溶剂系统。将此法用于１２种磺胺药物的分离,得到了满意的结果。     

测定麦芽糖转糖苷反应体系组成的高效液相色谱法

建立了分析低聚异麦芽糖组成的高效液相色谱法，采用Spherisorb-NH2色谱柱，示差折光检测器，乙腈－水（体积比70：30）为流动相，外标法定量测定；结果显示各糖质量浓度在0．1－10g/L范围内与峰面积呈良好线性关系，相关系数为0．999 0－0．999 7；应用法跟踪了pH5．0的柠檬酸－柠檬酸钠缓冲溶液中以α－葡萄糖转苷酶为催化剂在58℃温度下的麦芽糖转糖苷反应，分析了反应体系组成随时间的变化，得到了上述反应条件下麦芽糖最大限度地转化为低聚异麦芽糖的最佳反应时间为24h；该法快捷、简单、准确，可用于低聚异麦芽糖生产的质量控制。     

薄层色谱-反相高效液相色谱法分离纯化蟾酥中的内源性钠泵抑制因子

 采用薄层色谱法分离中药蟾酥中内源性哇巴因样物质 ,以三氯甲烷 甲醇 水 (体积比为 75∶2 0∶5 )溶液为展开剂 ,将所获得的活性物用反相高效液相色谱法纯化并经 2 2 0nm及 30 0nm检测后 ,以人红细胞86Rb摄取率试验测定其生物活性 ,得到了匀质的、紫外吸收波长为 2 5 0nm、可明显抑制钠泵活性的一种新的哇巴因样物质。实验结果为薄层色谱 高效液相色谱法用于内源性、低相对分子质量的生物样品的分离及纯化提供了依据。     

The Effect of Binary Solvent Composition and Polarity on Separations in Reversed Phase Thin Layer and High Performance Liquid Chromatography

Abstract

The effect of the solvent's composition and polarity on separation in reversed phase thin layer and high performance liquid chromatography is discussed. These results show that retention times cannot be predicted merely from the polarity of the binary mobile phase. Although organic modifiers with the same physico-chemical properties and from the same solvent group were used, the retention times obtained using binary mobile phases having the same polarity, were different. It was also observed that normal chain carbon alcohols gave retention times different from those with a branched chain (n-propanol vs. iso-propanol), and the longer the alcohol chain the higher the R_f value. The results also show that not only the organic modifier used is important but the solute mixture used.     

Triangular Thin-Layer Chromatography

Abstract

This study illustrates the use of triangular plates in thin-layer chromatographic separations. A comparison between triangular, conventional and circular thin-layer chromatography clearly indicates the superiority of triangular plates in terms of sensitivity, detection limits and savings in plates and solvent.     

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     

Two-Phase Thin-Layer Chromatography

Abstract

Thin layer chromatography (TLC) is normally carried out on single-phase (adsorbent) plates. However, it may be necessary to use nore than one adsorbent to achieve the separation of complex mixtures. Literature reports indicate that the use of mixed phases in TLC is not very common, possibly because the plates are difficult to prepare and precoated single-phase plates of different absorbents are readily available (silica gel, reversed phase, cellulose. alumina, etc.).     

高效液相色谱法测定低聚果糖的组分

采用高效液相色谱法（ＨＰＬＣ）,以μ－ＢｏｎｄａｐａｋＣ１８柱为分析柱,水为流动相,示差折光仪为检测器,一次进样能同时测定低聚果糖样品中的果糖、蔗糖、三糖、四糖、五糖、六糖等。测定了“博爱生命素”样品,所得结果良好,变异系数为０．５５％～１．１％,线性相关系数为０．９９９２～１．０００。低聚果糖的最低检出限在微克级。     

Systematic Optimization of Thin-Layer Chromatography for Wound-Induced Differential Secondary Metabolites in Passiflora foetida

JPC – Journal of Planar Chromatography – Modern TLC -     

On-Plate Electrochemical Detection for Thin-Layer Chromatography

Abstract

Voltammetric electrochemical detection (ECD) coupled with thin-layer chromatography (TLC) was demonstrated for the quantification of trace organic compounds directly on a TLC plate. the electrochemical detection solvent was a thin layer of aqueous potassium chloride. For undeveloped plates, detection limits for p-anisidine and p-phenetidine were 10 ng and 13 ng, respectively. Linearity was demonstrated over nearly 2 orders of magnitude. After development, detection limits increased by approximately a factor of ten. Advantages of this method over other quantitative TLC methods include sensitivity, speed, simplicity, and cost. in addition, this method is selective for electrochemically active compounds. Major sources of experimental error include spot size reproducibility, working electrode placement, and supporting electrolyte film thickness.     

薄层色谱溶剂系统优化方法进展

介绍了薄层色谱溶剂分类和溶剂强度参数的进展,综述了近年来优化溶剂系统的九种方法,并对它们进行了比较。     

高效薄层法检测尿中氟硝西泮的代谢物7-氨基氟硝西泮

 报道了尿中氟硝西泮代谢物 7 氨基氟硝西泮 (7AFLZ)的高效薄层 (HPTLC)定性分析和半定量分析方法 ,分析物斑点用荧光胺进行荧光显现 ,灵敏度高 ,检测限 (LOD)为 5 μg/L ,测量限 (LOQ)为 15 μg/L。该方法可以检测人口服 1mg氟硝西泮后 48h内排泄尿中的 7AFLZ ,适于麻醉抢劫犯罪案件中的药物检测。     

聚合物整体固定相的制备及条件优化

采用无搅动原位聚合模式,在聚醚醚酮柱管中直接制备了聚合物整体固定相。通过扫描电镜观察到该整体固定相的孔径分布呈双峰模式,且孔结构均匀。用压汞法测定了该固定相的孔径分布、孔隙率及比表面积等参数,考察了致孔剂组成、聚合温度及交联剂含量等参数对固定相孔结构的影响,并对制备条件进行了优化。测定了流速与柱前压的关系,实验表明此整体固定相具有良好的通透性。通过对山羊血清和低聚核苷酸的分离分析,证明了所制备的整体固定相适合用于生物大分子的分离纯化。     

快速溶剂萃取–高效液相色谱法测定禽蛋中磺胺嘧啶

建立快速溶剂萃取–高效液相色谱法测定禽蛋中磺胺嘧啶残留的方法。用单因素和正交试验对禽蛋中磺胺嘧啶的萃取条件进行优化,确定了最佳萃取条件:以甲醇为萃取剂,在130℃循环萃取4次,冲洗体积分数为80%,萃取时间为25 min。色谱柱为Hypersil ODS2柱(4.6 mm×250 mm,5μm),流动相为甲醇–0.5%冰乙酸(25∶75),流量为1.0 m L/min,检测波长为265 nm。磺胺嘧啶的质量浓度在0.025~0.500 mg/m L范围内与色谱峰面积呈良好的线性关系,相关系数r=0.999 5,检出限为0.5μg/kg。加标回收率在83.0%~88.2%之间,测定结果的相对标准偏差为2.2%(n=9)。方法的精密度、准确度和基质效应均符合禽蛋样品检测要求,可用于禽蛋中磺胺嘧啶含量的测定。     

Electroosmotic Circular Thin-Layer Chromatography

A new version of electroosmotic thin-layer chromatography, circular electroosmotic chromatography, was suggested and a prototype apparatus for its implementation was designed.     

Surfactants in Thin-Layer Chromatography

Data reported in the literature on the use of surfactants as modifiers of mobile and stationary phases in thin-layer chromatography are analyzed. The features of micellar and ion-pair versions of thin-layer chromatography and the dynamic and static modifications of stationary phases with surfactants are considered.     

薄层色谱在高速逆流色谱溶剂系统选择过程中的应用

本文对薄层色谱在高降流色谱的溶剂系统选择过程中的应用进行了研究，发现根据薄层色谱的斑点色度可以观察样品中各组分的含量差别及其在两相溶剂中分配系数间的差异，由此来判断溶剂系统的适用性，并确定哪一层适宜作流动相。