河豚毒素的薄层色谱扫描法测定

河豚毒素(Tetrodotoxin,简称TTX)是存在于河豚鱼类卵巢和肝脏等组织的一种天然剧毒物质。其化学结果如下:     

薄层色谱扫描法测定复印纸中单糖的研究

建立了通过薄层色谱扫描法测定复印纸样品水解液中的单糖含量鉴别纸张的新方法。复印纸样品水解后点样在以丙酮处理过的硅胶G薄层板上,以V(正丁醇)∶V(乙酸乙酯)∶V(异丙醇)∶V(乙酸)∶V(吡啶)∶V(水)=7∶20∶12∶7∶6∶5为展开剂,以苯胺-草酸为显色剂,测定了单糖的Rf值,以双波长反射吸收锯齿扫描测定(λS=510 nm,λS=610 nm),外标法定量。该法的线性关系较好,木糖和葡萄糖的检出线分别为4.1、2.5 ng,混合单糖标准品在同一薄层板上的峰面积的相对标准偏差(RSD)为2.3%和2.1%,两种单糖的样品加标回收率为98.09%和98.18%。该方法具有分离效果好,操作简便,可用于复印纸样品水解液中两种单糖的同时测定,从而为法庭科学中复印纸的检验提供了可靠的依据。     

烟草中叶黄素和β-胡萝卜素的HPLC快速测定

建立了一种快速测定烟草中叶黄素和β-胡萝卜素含量的高效液相色谱方法.样品用丙酮提取直接进样分析,叶黄素和β-胡萝卜素的回收率分别为98.8%和99.4%,RSD均小于1.00%.该方法适用于大批量烟草样品的分析检测.     

计算机辅助高效薄层色谱最优化分离

近年来,色谱分析中利用计算机辅助、模拟优化分离条件是一新动向。其中窗图法(Window diagram)不仅用于气相色谱固定相的选择,也用于液相色谱流动相等的选择,但在薄层色谱方面未见过报道。本文主要将窗图法应用到高效薄层色谱,将难分离对的△R_f=R_(fi)-R_(fJ)与展开剂组成作图,选择溶剂的最佳配比。整个过程由自编的OS-T2软件处理。通过对13种有机氮农药进行连续展开的高效薄层色谱实验,结果表明     

尼美舒利含量的薄层色谱扫描法测定

应用薄层扫描法测定尼美舒利的含量,在GF254硅胶板上,以二氯甲烷－石油醚（V＝氯甲烷：V石油醚＝8：2）为展开剂,用CS－9000薄层扫描仪扫描,扫描波长为254nm,其Rf值为0．30,该法的检出限为0．05μg,同时相对标准偏差为2．2％（n=10),工作曲线的线性范围为0．05－1．8μg,血清及尿样的加标回收率为98％－105％。     

薄层色谱扫描定量分析原理

用于薄层色谱扫描的Kubelka-Munk方程式是测量参数反射比或透射比对定量参数吸光系数的较复杂的非线性函数。不能直接用于定量计算,本文综述了求算其反函数,建立定量分析工作曲线的四种数学处理方法,并对扫描光源、方式、噪音及背景信号作了一些探讨。     

微柱高效液相色谱和质谱法测定烟草样品中多酚

研究了用微柱高效液相色谱和质谱法测定烟草样品中植物多酚。烟草样品中植物多酚用80%的甲醇加热回流提取,提取液用Sep-Pak-C18固相萃取小柱预分离脱脂,以WatersXterraTMRP18(1.0mm×50mm,2.5μm)微柱为固定相,甲醇和1%的乙酸梯度洗脱为流动相分离;用紫外二极管矩阵检测器检测,并用质谱对未购到标样的绿原酸异构体进行了辅助定性。方法用于一些烟草样品中多酚的测定,回收率在97%-103%之间,RSD在1.4%-1.9%之间。     

液相微萃取-薄层色谱扫描法测定矿泉水中微量汞、铜

采用双硫腙螯合-液相微萃取, 富集水相中的Cu2+、 Hg2+ 200倍, 并结合条形点样-薄层色谱分离, 数字图象处理扫描定量, 建立了微量Cu2+、 Hg2+的分析方法. Cu2+、 Hg2+的检出限分别为0.6、 1.1 ng/mL, RSD(n=5)分别为 2.5%、 3.8%. 应用于两种市售矿泉水的测定, Cu2+的平均加样回收率分别为94.7%、 98.3%, Hg2+的平均加样回收率分别100.0%、 108.6%.     

高效液相色谱串联质谱法快速测定烟草中5种甾醇的研究

本研究基于自主设计的集萃取、过滤和转移功能为一体的样品萃取瓶,建立了高效液相色谱串联质谱(LC-MS/MS)快速测定烟草中麦角甾醇、胆甾醇、菜油甾醇、豆甾醇和β-谷甾醇的方法。样品在萃取瓶中经水解、皂化和萃取,经LC-MS/MS进行分析检测。结果表明:自主设计的样品萃取瓶可提高前处理效率,5种甾醇在0.1～150 ng·mL~(-1)内均具有良好的线性关系(线性相关系数0.999);检出限在0.015～0.075ng·mL~(-1);平均回收率在93.4%～103.8%之间,日内精密度和日间精密度均小于3.5%,具有较好的重复性。该方法能够满足烟草中5种甾醇快速、准确测定。     

双波长薄层色谱扫描法测定感冒通片中扑尔敏的含量

本文采用双波长薄层扫描仪，以紫外吸收方式，测定了感冒通片中扑尔敏的含量，其测定波长λｓ＝２６０ｎｍ，参比波长λＲ＝３２０ｎｍ，所用薄层板为ＧＦ２５４，薄层厚度为０．４ｍｍ，展开剂为苯∶氯仿∶冰ＨＡＣ∶甲醇＝５∶５∶０．５∶０．６，回收率为１０１．６％。     

Determination of betulin in Grewia tiliaefolia by HPTLC

A sensitive, rapid, simple, and accurate high performance thin layer chromatographic method has been developed to standardize the bark of Grewia tiliaefolia Vahl. (Family: Tiliaceae) using betulin as an analytical marker. Chloroform extracts of bark from five different sources were used for HPTLC on silica gel with toluene-ethyl acetate, 90 + 10 v/v, as mobile phase. Under these conditions, the Rf of betulin was 0.22. The calibration plot was linear in the range of 1000 ng to 1800 ng of betulin and the correlation coefficient, 0.999, was indicative of good linear dependence of peak area on concentration. The mean assay of betulin was 2.596 +/- 0.594 mg g(-1) of bark. The method permits reliable quantification of betulin and good resolution and separation of betulin from other constituents of Grewia tiliaefolia. Recovery values from 96.09 to 98.87% showed that the reliability and reproducibility of the method were excellent. The proposed HPTLC method for quantitative monitoring of betulin in Grewia tiliaefolia can be used for routine quality testing.     

非水反相液相色谱法测定枸杞子中β-胡萝卜素含量

应用甲醇－乙酸乙酯（５０５５,Ｖ／Ｖ）为流动相,在ＯＤＳ反相柱上采用外标法测定了３种不同产地枸杞子中β－胡萝卜素的含量。方法简便、快速,重现性好。β－胡萝卜素的检测线性范围为１．０～５．０ｍｇ／Ｌ,ｒ＝０．９９９８,平均回收率为９７．１％,变异系数为１．９％。     

Determination of Polyamines in Beers by HPTLC with Fluorescence Detection

JPC – Journal of Planar Chromatography – Modern TLC - A high-performance thin-layer chromatographic (HPTLC) method has been developed for determination of polyamines in beers. Beer...     

Simultaneous Determination of Metformin and Glyburide in Tablets by HPTLC

Simultaneous determination of two antidiabetic drugs, metformin and glyburide, in pharmaceutical tablet formulations were investigated. Normal phase thin layer chromatography plate (silica gel 60 F₂₅₄) was used as stationary phase and water/methanol/ammonium sulfate (2/1/0.5 w/v) as mobile phase to determine two pharmaceutically active ingredients, in three different formulations of Glucovance^®. This system gave a good resolution for metformin (R _f value of 0.43 ± 0.01) and glyburide (R _f value of 0.64 ± 0.02). Determination was by densitometry in the absorbance mode at 237 nm. The linear regression data for the calibration plot showed a good relationship with r = 0.99581 and 0.99982 for metformin and glyburide, respectively. The method was validated for precision and recovery. The limits of detection and quantification were 25.24 and 84.12 ng spot^?1 for metformin and 12.26 and 40.86 ng spot^?1 for glyburide, respectively. Stability study has been carried out for samples and standard solutions.     

HPTLC Determination of Atorvastatin in Plasma

High performance liquid chromatography has been the most popular choice for the determination of atorvastatin. In this study, two-step isocratic chromatography on silica gel 60F254 HPTLC layer and densitometric quantitation at λ = 280 nm was developed for the separation of atorvastatin from plasma constituencies and sodium diclofenac as peak-tracer. The established HPTLC method was validated in terms of LOD/LOQ, linearity, recovery and repeatability. The calibration function of the analyte was linear in the range 101–353.5 ng zone^?1 and the correlation coefficient was 0.9969. The limits of detection and quantitation were 30.3 and 101 ng zone^?1. The recovery and relative standard deviation obtained from between-days analysis were 97.5–103.0 and 1.7–3.4%.     

Determination of α-Cypermethrin from Soil by Using HPTLC

JPC – Journal of Planar Chromatography – Modern TLC - α-Cypermethrin is a synthetic pyrethroid insecticide used to control insects. In soil, α-cypermethrin biodegrades...     

HPTLC Determination of Cefpodoxime Proxetil in Formulations

An HPTLC method has been developed that coelutes both the isomers of cefpodoxime proxetil (CFP). CFP was chromatographed on a silica gel 60 F₂₅₄ TLC plate using toluene:acetonitrile (6:4) as a mobile phase and was quantified at 234 nm. The method was validated with respect to linearity, accuracy, precision and specificity. The limit of detection and limit of quantification for CFP were found to be 0.150 and 0.4 μg spot⁻¹, respectively. The proposed method was successfully used to determine the amount of CFP present in the marketed tablets and self-nanoemulsifying systems.

     

HPTLC Determination of Cefpodoxime Proxetil in Formulations

An HPTLC method has been developed that coelutes both the isomers of cefpodoxime proxetil (CFP). CFP was chromatographed on a silica gel 60 F₂₅₄ TLC plate using toluene:acetonitrile (6:4) as a mobile phase and was quantified at 234 nm. The method was validated with respect to linearity, accuracy, precision and specificity. The limit of detection and limit of quantification for CFP were found to be 0.150 and 0.4 μg spot^?1, respectively. The proposed method was successfully used to determine the amount of CFP present in the marketed tablets and self-nanoemulsifying systems.     

Determination of Exemestane in bulk and pharmaceutical dosage form by HPTLC

An HPTLC method for analysis of Exemestane in bulk and pharmaceutical formulation has been established and validated. The analyte was separated on aluminium plates precoated with silica gel 60 F₂₅₄. The mobile phase was chloroform:methanol 9.2:0.8 (v/v). Quantification was done by densitometric scanning at 247 nm. Response was a linear function of Exemestane concentration in the range of 100–500 μg mL⁻¹. The limit of detection and quantification for Exemestane were 5.8 and 17.58 μg mL⁻¹, respectively. Average recovery of Exemestane was 100.1, which shows that the method was free from interference from excipients present in the formulation. The established method enabled accurate, precise, and rapid analysis of Exemestane in bulk as well as pharmaceutical formulation.