一阶导数停流法测定药物和饮用水中的铁

本文利用Ｆｅ＾３＋离子催化Ｈ２Ｏ２氧化四甲基对苯二胺的反应，将采用停流技术获得的动力学曲线转换成一阶导数曲线，根据导数峰高值与Ｆｅ＾３＋离子浓度的线性关系测定药物和自来水中的含量，本方法的线性范围为４．０－４０．０ｎｇＦｅ＾３＋／ｍｌ，相对标准偏差小于２．５％，标准加入回收率在９８．７％－１０１％之间，检测限为１．９２ｎｇＦｅ＾３＋／ｍｌ。对照实验结果表明，导数动力学法比一般非导数动力学法具有线关     

停流-抑制动力学荧光法测定痕量苯酚

用停流技术研究了在H2SO4介质中,苯酚抑制BrO-3氧化丁基罗丹明B荧光猝灭反应,并探讨了反应机理。基于苯酚对该反应诱导期的影响作用,建立了停流-抑制动力学荧光法测定痕量苯酚的新方法。方法的检出限为1.4×10-8g.L-1,线性范围为0.4~15.0μg.L-1,11次测定7.0μg.L-1苯酚的相对标准偏差为2.1%。本法灵敏、简便,用于测定制药废水和番茄酱样品中痕量苯酚,结果满意。     

On-line identification of 4″-isovalerylspiramycin I in the genetic engineered strain of S. spiramyceticus F21 by liquid chromatography with electrospray ionization tandem mass spectrometry,ultraviolet absorbance detection and nuclear magnetic resonance spectrometry

LC-hyphenated techniques were applied to the on-line identification of isovalerylspiramycin I (isp I), a spiramycin-like macrolide in the crude extract of fermentation broth from a genetically engineered strain of S. spiramyceticus F21. In the structural characterization of the large molecular secondary metabolite of isp I, LC–DAD-UV–ESI-MSⁿ analysis played a crucial role, and stop-flow LC–¹H NMR measurement, with bitespiramycin used as reference, was a valuable complement approach. This rational approach proved to be an efficient means for the rapid and accurate structural determination of known microbial secondary metabolites, by which targeted isolation of component(s) of interest can be subsequently performed for further biological and pharmacological studies in drug development.     

Method of gas mixtures discrimination based on sensor array, temporal response and data driven approach

This work presents a method of gas mixtures discrimination. The principal concept of the method is to apply measurement data provided by a combination of sensors at single time point of their temporal response as input of the discrimination models. The pattern data combinations are selected for classes of target gases based on the criterion of 100% efficient discrimination. Combinations of sensors and time points, which provide pattern data combinations in course or repeated measurements, are encoded in the form of addresses. The designer of sensor system is responsible for their selection and they are included in the software of the final instrument. The study of the method involved the discrimination of gas mixtures composed of air and single chemical: hexane, ethanol, acetone, ethyl acetate and toluene. Two sensor arrays were utilized. Each consisted of six TGS sensors of the same type. The dynamic operation of sensors was employed. As an example the stop-flow mode was chosen. The work provides the evidence of the existence of sensor combinations and time points, which are successful in discrimination of studied classes of target gases. The persistence of addresses was discussed considering the ability of sensor array to recognize analytes, variability of repeated measurement results, number of repeated measurements and a twin sets of sensors. Altogether, the validity of the method was demonstrated.     

Use of xenon as a mobile phase for on–line capillary supercritical fluid chromatography–fourier transform infrared spectrometry

Xenon is investigated as a mobile phase for on-line capillary supercritical fluid chromatography-Fourier transform infrared spectrometry (SFC-FTIR). Polycyclic aromatic hydrocarbons, aromatic isocyanates, and epoxy acrylate oligomers are analyzed as examples to show that xenon has similar selectivities and solvating powe to CO₂. Its optical transparency makes it ideal for IR detection. A stop flow system is constructed to increase the sensitivity of spectra measured from compounds which are weak IR absorbers.     

微流控芯片停流液-液萃取系统的研究

基于微流控芯片的液-液萃取技术^[1]的研究是目前微流控芯片分析领域中的重要研究方向之一.与传统液-液萃取系统相比,萃取系统微型化能显著降低试剂与样品的消耗(仅为传统系统的万分之一),加快分析速度,易实现操作的自动化和分析系统的集成化等.     

Stop-Flow Analysis: An Aid in the Diagnosis and Optimization of Continuous-Flow Systems

Abstract

A novel application of stop-flow analysis (s. f. a.) in continuous-flow automated chemical reactors is presented. By continuous addition of reactant to the reactor, s. f. a. can be used to simultaneously diagnose and evaluate each reactor stage. The method demonstrated is fast, simple to execute, and requires no additional equipment. A rational method to optimize continuous-flow systems is the end product of this application.     

Basic aspects of stop-flow split injection

Summary Major concerns in the development of the stop-flow split injection are discussed. Split ratio fluctuation caused by the pressure wave, solvent recondensation and gas viscosity change can be substantially diminished through the formation of a nearly uniform gaseous sample plug. Instrumental variables exerting influence on the accuracy of quantitation were studied. Higher injector temperature and the use of a carrier gas with higher heat conductivity benefit the quick vaporization of the sample liquid, and thus, help in the formation of a sample plug with more unformity.     

停流-催化动力学光度法测定药物中的溴

研究了H3PO4介质中,溴离子催化KBrO3氧化丁基罗丹明B的褪色反应特性,测定了反应级数和表观活化能,拟定了反应的最佳条件,建立了停流-催化动力学光度法测定微量溴的新方法。在(27±0.05)℃反应4min测定的检出限为1.51×10-4g/L,线性范围为0~10.0mg/L。该方法用于药物中溴离子的测定,相对标准偏差为2.2%~2.3%,回收率为98%~102%。     

Novel oxidation reaction of prochlorperazine with bromate in the presence of synergistic activators and its application to trace determination by flow injection/spectrophotometric method

Valve-based comprehensive two-dimensional gas chromatography (GC × GC) is one of the most compact, robust, and inexpensive GC × GC instrument designs. The major drawback of a valve-based modulation configuration lies in diminished detection sensitivity. This loss in sensitivity is because under typical operating conditions the fraction of the first column (i.e., column 1) effluent transferred to the second column (i.e., column 2) is likely to be ∼5-10%. To address this loss in sensitivity, we report the development of a unique total-transfer (i.e., 100%) valve-based GC × GC, without adding complexity to the instrumentation. The new instrument design relies upon simply blocking one of the appropriate ports of the high-speed six-port diaphragm valve that is used as the modulator between columns 1 and 2. The modulation period and difference in head pressure between columns 1 and 2 are found to be the two primary variables that are controlled to provide good detection sensitivity and 100% mass transfer from column 1 to column 2. The detection sensitivity is better with a longer the modulation period. A limit of detection of 0.03 ng/μl was obtained for octane. This sensitive GC × GC configuration is also shown to provide acceptable separation peak capacity, with good separations achieved for real complex samples: gasoline and Eucalyptus oil, where compounds were spread out over much of the two-dimensional separation space. In principle, this total-transfer, valve-based GC × GC is more portable and less expensive than currently available GC × GC instrumentation.