Quantitative analysis flow injection technique

Quantitative Analysis Using Flow Injection Technique [13]... 

The attractive features of splitless injection techniques are that they allow the analysis of dilute samples without preconcentration (trace analysis) and the analysis of dirty samples, since the injector is easily dismantled for cleaning. Success with individual samples, however, depends on the selection of experimental variables of which the most important sample size, sample solvent, syringe position, sampling time, initial column temperature, injection temperature and carrier gas flow rate, often must be optimized by trial and error. These conditions, once established, are not necessarily transferable to another splitless injector of a different design. Also, the absolute accuracy of retention times in splitless injection is generally less than that found for split injection. For splitless injection the reproducibility of retention times depends not only on chromatographic interactions but also on the reproducibility of the sampling period and the evaporation time of the solvent in the column inlet, if solvent effects (section 3.5.6.2) are employed. The choice of solvent, volume injected and the constancy of thermal zones will all influence retention time precision beyond those for split injection. For quantitative analysis the precision of repeated sample injections is normally acceptable but the method is subject to numerous systematic errors that may... 

See also Electrophoresis Two-Dimensional Gels Nucleic Acids. Enzymes Enzyme-Based Assays. Flow Injection Analysis Principles. Fluorescence Quantitative Analysis. Lab-on-a-Chip Technologies. Mass Spectrometry Matrix-Assisted Laser Desorption/loniza-tion Time-of-Flight. Microelectrodes. Microscopy Overview. pH. Process Analysis Overview Chromatography Electroanalytical Techniques Sensors Acoustic Emission Maintenance, Reliability, and Training. Proteins Overview. Proteomics. Purines, Pyrimidines, and Nucleotides. Sensors Oven/iew. Spectrophotometry Overview. 

Up to this point, the detection Unfit and sensitivity comparisons of the different sources have focused primarily on compoimds that ionize efficiently with all the techniques. It is important to understand the coverage or scope of an ionization technique across the chemical space of general interest, particularly when confronted with unknown compounds, or compounds whose structures are known but whose ionization properties have not been tested, and there is no time to assess a variety of options. This situation occurs in many drug discovery laboratories measuring in vitro ADME properties (administration, distribution, metabolism, excretion) where many different chemical species need to be assayed quickly. The data used to generate the relative efficiency values within a source in Tables 1-3 were used to calculate the relative MRM efficiency between the three sources and are shown in Table 13.4. The MALDI data were acquired in the most practical fashion to obtain a quantitative measurement where only a small percentage of the sample spot was ablated with a single raster. The ESI and APCI data were obtained by flow injection analysis at 200 and lOOOpL/min, respectively. Electrospray is the most sensitive ion source in nearly all... 

Factors may be classified as quantitative when they take particular values, e.g. concentration or temperature, or qualitative when their presence or absence is of interest. As mentioned previously, for an LC-MS experiment the factors could include the composition of the mobile phase employed, its pH and flow rate [3], the nature and concentration of any mobile-phase additive, e.g. buffer or ion-pair reagent, the make-up of the solution in which the sample is injected [4], the ionization technique, spray voltage for electrospray, nebulizer temperature for APCI, nebulizing gas pressure, mass spectrometer source temperature, cone voltage in the mass spectrometer source, and the nature and pressure of gas in the collision cell if MS-MS is employed. For quantification, the assessment of results is likely to be on the basis of the selectivity and sensitivity of the analysis, i.e. the chromatographic separation and the maximum production of molecular species or product ions if MS-MS is employed. 

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