Enantioselectivity of 6-O-alkyldimethylsilyl-2,3-di-O-methyl-β-cyclodextrins as chiral stationary phases in capillary GC

Summary Clenbuterol has been determined in urine by solidphase extraction on a C₁₈ cartridge, diazotization of the eluate with nitrite, coupling of the diazonium ion with 1-(naphthyl)ethylenediamine, and separation of the azo dye formed by HPLC with a C₁₈ column and a micellar mobile phase containing 0.1 M sodium dodecyl sulphate, 12%n-butanol and 0.05 M citrate buffer, pH 3. Recoveries higher than 90% were obtained by mixing the samples with a 20% 0.2 M NaOH before extraction. Limits of detection of 51 and 6.7 ng L⁻¹ were obtained with spectrophotometric and thermal lens spectrometric detection, respectively; respective repeatabilities were 3.1% (5 μg mL⁻¹) and 5.6% (0.16 μg mL⁻¹).     

Analysis of the pungent principles of ginger and grains of paradise by high-performance liquid chromatography using electrochemical detection

Summary The pungent principles of ginger and grains of paradise are examined using a reversed-phase HPLC column. An electrochemical detector is used to selectively detect the phenolic gingerols and shogaols. The retention indices of the compounds are compared using methanowater and acetonitrile-water as eluents.Presented at the 14th International Symposium on Chromatography London, September, 1982     

Protease sensors for bioimaging

Optical imaging of specific molecular targets and pathways in vivo has recently become possible through continued developments in imaging equipment, reconstruction algorithms, and more importantly the availability of imaging reporter molecules. These reporter molecules encompass photoproteins expressed in vivo and exogenously administered probes detectable by fluorescence and/or bioluminescence imaging. One particularly enticing aspect of optical imaging is the ability to design activatible probes with inherent amplification. This review summarizes our experience in developing novel near-infrared fluorescent (NIRF) imaging agents that report on protease activities. These agents are designed to be biocompatible, highly activatible, and able to produce bright NIRF following protease cleavage.     

Determination of orthophosphates using a macro segmented flow analyzer (MSFA) based on colorimetric detection

Fabrication of a macro segmented flow analysis (MSFA) system based on reconfiguration of the manifold by adjustment of the sample/reagent ratio, has been found to produce a sensitive method for orthophosphate analysis based on colorimetric detection at 880 nm. Optimization of sample tube length, reaction temperature and molybdate concentration in the carrier solutions has been carried out. The larger sample tube internal diameter led to the combined advantages of better sensitivities, wider working range and higher sample throughput over most existing methods. Using the optimized conditions of 50.0 cm sample tube length (1.6 mm i.d.), 37.0 °C reaction temperature and 0.0113 M molybdate concentration in the carrier solution, the calibration model for orthophosphate standard solutions was found to be linear (y = 0.04895x + 0.003561; correlation coefficient, r²=0.9970) over the working range 0.01-2.00 mg l⁻¹ orthophosphate. The volume of the sample injected was 1.396 ml at a flow rate of 6.0 ml min⁻¹. The sample throughput of this MSFA method was 40 samples per an hour, with a detection limit of 4.0 μg l⁻¹, and %R.S.D.’s below 5%. The MSFA method was successfully applied to analysis of water and wastewater samples.     

Contactless conductivity detection of synthetic polymers in non-aqueous size-exclusion electrokinetic chromatography

A capacitively coupled contactless conductivity detection (CCD) system has been applied for the detection of neutral synthetic polymers in capillary size-exclusion electrokinetic chromatography (SEEC). Polystyrene standards, that were used as a model compounds, were separated on a capillary column packed with porous 10 microm silica particles with an electrokinetically driven mobile phase, and detected by CCD and UV detection simultaneously. Mass-calibration curves for polystyrene were constructed. Satisfactory results were obtained for the linearity, the run-to-run repeatability (<0.2% for the relative retention and <4% for the peak area) and the robustness of the detector. One of the major issues in this preliminary study was to investigate the origin of the peaks observed for the polystyrene standards. The effect of the molar mass of the polystyrenes on the sensitivity was small. Therefore, the signals obtained could not be explained as the result of an increased viscosity and a decreased solution conductivity of the solute zone. An alternative hypothesis is suggested, and recommendations for further research are given.     

氯氮平、去甲氯氮平及奥氮平的高效液相色谱电化学检测特性的研究

 采用高效液相色谱安培电化学检测法 ,考察了氯氮平、去甲氯氮平和奥氮平在不同 pH值流动相下的色谱分离情况及其色谱峰高与检测电压的关系。结果表明 ,氯氮平、去甲氯氮平和奥氮平的保留时间均随流动相 pH值的升高而延长 ;在pH值为 4 5 6和 5 5 6的流动相中 ,均可实现基线分离。 3种化合物的色谱峰高与检测电压之间呈典型的“S”型曲线 ,pH值升高时该曲线均左移。氯氮平、去甲氯氮平和奥氮平的检测电压必须大于产生最大氧化电流的最低电压才能得到稳定的检测电流。这种典型的“S”型伏安曲线对于化合物的定量和定性检测具有重要意义。     

Use of non-segmented flow,post-columns reaction detection with miniaturized HPLC systems

Summary The use of non-segmented flow, post-column reaction detection is evaluated for use with miniaturized HPLC. Non-segmented open-tubular reactors with internal diameters 0.1 mm to 0.25 mm and packed-bed reactors with internal diameters of 1 mm, filled with 5 and 10 m particles are evaluated theoretically and experimentally with respect to band broadening and pressure drop characteristics. An integrated system consisting of miniaturized HPLC (1 mm i. d.) columns and compatible hardware is described. An example of the separation of catecholamines is given.     

Amperometric multidetection with composite enzyme electrodes

The use of composite biosensors for multianalyte detection strategies is discussed. Graphite–Teflon rigid composite biosensors offer the possibility of coimmobilization of several enzymes by simple physical inclusion in the bulk of the electrode matrix with no covalent linkages. A novel trienzyme graphite–Teflon–glucose oxidase (GOD)–alcohol oxidase (AOD)–peroxidase (HRP)–ferrocene bisosensor yielded amperometric steady-state currents similar to those obtained with graphite–Teflon–GOD–HRP–ferrocene and graphite–Teflon–AOD–HRP–ferrocene electrodes for the same concentration of glucose and ethanol, respectively. The performance of the trienzyme biosensor for multianalyte detection was evaluated with the simultaneous determination of glucose and ethanol after separation by HPLC, in samples of sweet wine. The simultaneous analysis of several analytes in the same sample should imply that, with an adequate dilution, the concentration levels of the analytes can be included within the ranges of linearity of the corresponding calibration plots. The use of two composite biosensors in a parallel configuration, so that different analytes can be simultaneously detected with no need of chromatographic separation, is also discussed. The usefulness of this approach was evaluated by the simultaneous analysis of glucose and ethanol in sweet wine, and of glucose and lactic acid in red wine.     

微柱分离中的激光诱导荧光检测

 激光诱导荧光检测 (LIFD)以其高的灵敏度和选择性而被广泛应用于微柱分离技术中。以检测池为轴线 ,概述了激光诱导荧光检测系统新进展及其应用。引用了 5 2篇文献