Chromatography combination methods with mass

Pyrolysis gas chromatography mass spectrometry Pyrolysis gas chromatography, combined predominantly with mass spectrometry, is a powerful analytical method for the categorization of polymers. Moreover, it is useful for the characterization of... 

Another drawback is the fact that there are over 60,000 chemical compounds in commerical use, and each one cannot have a distinctive retention volume on a given system. If a compound or a mixture is truly unknown, its chromatogram will not provide characteristic retention volumes on the basis of which identifications can be made. In short, chromatography can be used for qualitative analysis for a limited set of chemicals, but its main use is not for screening unknowns. In fact, one of the best methods of qualitative analysis is the combination of chromatography (an excellent separation method) with mass spectrometry (an excellent identification method). This topic is included in Chapter 11. 

The use of selective detectors is the most promising route to the identification of unknown components in a complex mixture. Chromatography can separate complex mixtures into individual components, but it cannot positively identify them. Most spectrometric methods, on the other hand, supply sufficient information to identify complex compounds, but only if they are so pure that all the spectral clues can be ascribed safely to the same compound. Among the possible combinations, coupling with mass spectrometry, and to a lesser degree IR spectrometry, have been the most fruitful, because the amount of sample easily handled in classical chromatography is well suited to these techniques. Less sophisticated detectors have also been used to advantage. 

Authenticity evaluation has recently received increased attention in a number of industries. The complex mixtures involved often require very high resolution analyses and, in the case of determining the authenticity of natural products, very accurate determination of enantiomeric purity. Juchelka et al. have described a method for the authenticity determination of natural products which uses a combination of enantioselective multidimensional gas chromatography with isotope ratio mass spectrometry (28). In isotope ratio mass spectrometry, combustion analysis is combined with mass spectrometry, and the ratio of the analyte is measured versus a... 

In the case of heterogeneous polymers the experimental methods need to be refined. In order to analyze those polymers it is necessary to determine a set of functions / (M), which describe the distribution for each kind of heterogeneity i This could be the mass distributions of the blocks in a diblock copolymer. The standard SEC methods fail here and one needs to refine the method, e.g., by performing liquid chromatography at the critical point of adsorption [59] or combine SEC with methods, which are, for instance, sensitive to the chemical structure, e.g., high-pressure liquid chromatography (HPLC), infrared (IR), or nuclear magnetic resonance spectroscopy (NMR) [57],... 

Gas or liquid chromatography combined with tandem mass spectro-metry are the methods of choice for unequivocal identification at trace levels. 

Lanina et al. 1992 Oishi 1990). These methods include gas chromatography (GC) combined with mass spectrometry (MS) and high-performance liquid chromatography (HPLC) combined with an ultraviolet detector (UV). No comparisons can be made between methods since no data were given regarding sensitivity, recovery, or precision. 

Liquid chromatography combined with triple-quadrupole mass spectrometers has been used extensively as the analytical method of choice to determine the plasma concentration of compounds. 

Pulsed ultrafiltration MS (PUF-MS) represents an inline high throughput affinity screening method with a variety of potential uses in the discovery and development of pharmaceuticals [22]. The in-line combination of solution-phase equilibration, ultrafiltration, and electrospray liquid chromatography mass spectrometry (LC-ESI-MS) facilitates the identification of high affinity target-specific... 

Ylinen et al. [53] developed an ion-pair extraction procedure employing tetrabutylamonium (TBA) counter ions for determination of PFOA in plasma and urine in combination with gas chromatography (GC) and flame ionisation detection (FID). Later on, Hansen et al. [35] improved the sensitivity of the ion-pair extraction approach using methyl tertiary butyl ether (MTBE) and by the inclusion of a filtration step to remove solids from the extract making it amenable to liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) determination. Ion-pair extraction procedure has been the basis of several procedures for biota [49,54-58] and food samples [50,59,60]. However, this method has shown to have some limitations, such as (1) co-extraction of lipids and other matrix constituents and the absence of a clean-up step to overcome the effects of matrix compounds and (2) the wide variety of recoveries observed, typically ranging. 

Separation of dibenzothiophene derivatives from petroleum oil fractions has been achieved by integrated approaches in which fractionating processes such as isothermal distillation, vacuum fractionation, and molecular distillation have been combined with spectroscopic methods including mass spectrometry and NMR spectroscopy. " Dibenzothiophenes have also been concentrated in sharp chromatographic fractions obtained, for example, by, alumina gel percolation, and have been detected by gas chromatography. Gas chromatography has also been used to... 

Straub et al. (76) reported a method for the identification and quantification of penicillin G, ampicillin, amoxicillin, cephapirin, cloxacillin, and ceftiofur residues in milk using perfusive-particle liquid chromatography combined with ultrasonic nebulization electrospray mass spectrometry. According to this method, a 0.5 ml milk sample is diluted with an equal volume of a solution consisting of acetonitrile/water (1 1), and ultrafiltrated in a microseparation system with a 10000 da molecular mass cut-off filter. An aliquot of the ultrafiltrate is then analyzed on a 15 cm porous II R/H LC (7-8 m) perfusion analytical column using the chromatographic conditions shown in Table 29.3. Concentrations as low as 10 ppb could be readily determined in milk by electrospray mass spectrometric detection. 

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