Gas chromatography hyphenation

Jitaru, P. and F.C. Adams. 2004. Speciation analysis of mercury by solid-phase microextraction and multicapillary gas chromatography hyphenated to inductively coupled plasma-time-of-flight-mass spectrometry. J. Chromatogr. A 1055 197-207. 

Krupp, E.M., Pecheyran, C., Meffan-Main, S., and Donard, O.F.X. (2001) Precise isotope-ratio measurements of lead species by capillary gas chromatography hyphenated to hexapole multicollector ICP-MS. Fresenius J. Anal. Chem., 370 (5), 573-580. 

The possibiHties for multidimensional iastmmental techniques are endless, and many other candidate components for iaclusion as hyphenated methods are expected to surface as the technology of interfacing is resolved. In addition, ternary systems, such as gas chromatography-mass spectrometry-iafrared spectrometry (gc/ms/ir), are also commercially available. 

Mixtures can be identified with the help of computer software that subtracts the spectra of pure compounds from that of the sample. For complex mixtures, fractionation may be needed as part of the analysis. Commercial instmments are available that combine ftir, as a detector, with a separation technique such as gas chromatography (gc), high performance Hquid chromatography (hplc), or supercritical fluid chromatography (96,97). Instmments such as gc/ftir are often termed hyphenated instmments (98). Pyrolyzer (99) and thermogravimetric analysis (tga) instmmentation can also be combined with ftir for monitoring pyrolysis and oxidation processes (100) (see Analytical methods, hyphenated instruments). 

Coupling of analytical techniques (detectors) to high-performance liquid chromatographic (HPLC) systems has increased in the last tree decades. Initially, gas chromatography was coupled to mass spectrometry (MS), then to infrai ed (IR) spectroscopy. Following the main interest was to hyphenate analytical techniques to HPLC. 

J. B. Phillips and J. Beens, Comprehensive two-dimensional gas chromatography a hyphenated method with strong coupling between the two dimensions , J. Chromatogr. 856 331-347 (1999). 

The combination of chromatography and mass spectrometry (MS) is a subject that has attracted much interest over the last forty years or so. The combination of gas chromatography (GC) with mass spectrometry (GC-MS) was first reported in 1958 and made available commercially in 1967. Since then, it has become increasingly utilized and is probably the most widely used hyphenated or tandem technique, as such combinations are often known. The acceptance of GC-MS as a routine technique has in no small part been due to the fact that interfaces have been available for both packed and capillary columns which allow the vast majority of compounds amenable to separation by gas chromatography to be transferred efficiently to the mass spectrometer. Compounds amenable to analysis by GC need to be both volatile, at the temperatures used to achieve separation, and thermally stable, i.e. the same requirements needed to produce mass spectra from an analyte using either electron (El) or chemical ionization (Cl) (see Chapter 3). In simple terms, therefore, virtually all compounds that pass through a GC column can be ionized and the full analytical capabilities of the mass spectrometer utilized. 

The spectrum of new analytical techniques includes superior separation techniques and sophisticated detection methods. Most of the novel instruments are hyphenated, where the separation and detection elements are combined, allowing efficient use of materials sometimes available only in minute quantities. The hyphenated techniques also significantly increase the information content of the analysis. Recent developments in separation sciences are directed towards micro-analytical techniques, including capillary gas chromatography, microbore high performance liquid chromatography, and capillary electrophoresis. 

Gas chromatography is a most favourable case for interfacing to a mass spectrometer, as the mobile phases commonly used do not generally influence the spectra observed, and the sample, being in the vapour phase, is compatible with the widest range of mass-spectral ionisation techniques. The primary incompatibility in the case of GC-MS is the difference in operating pressure for the two hyphenated instruments. The column outlet in GC is typically at atmospheric pressure, while source pressures in the mass spectrometer range from 2 to... 

VDU screen via suitable electronic amplifying circuitry where the data are presented in the form of an elution profile. Although there are a dozen or more types of detector available for gas chromatography, only those based on thermal conductivity, flame ionization, electron-capture and perhaps flame emission and electrolytic conductivity are widely used. The interfacing of gas chromatographs with infrared and mass spectrometers, so-called hyphenated techniques, is described on p. 114 etseq. Some detector characteristics are summarized in Table 4.11. 

Once into the 21st century, hyphenated instrumentation (i.e., those that couple two instruments together) became prevalent in laboratories. This is the combination of two or more, often different, instruments. In simple terms, the purpose is to first separate the analyte of interest and then to identify it. This takes place using a sample injected into the combined instruments. The most common of the hyphenated instruments is the gas chromatograph, the output of which is fed into a mass spectrometer to produce a gas chromatography-mass spectrometry (GC-MS) [35],... 

Chromatographic methods are also often used as part of systems that are called hyphenated methods, (see Chapter 15) where the output of the chromatographic section is used as the input for an identification method such as mass spectrometry. These hyphenated methods are also most often referred to by their acronyms, for example, GC-MS—gas chromatography-mass spectrometry and HPLC-MS—high-performance liquid chromatography-mass spectrometry. Note that although ultraviolet-visible (UV-Vis) is hyphenated, it is not a hyphenated method in that it does not consist of two different methods of analysis. Hyphenated methods will be discussed fully in Chapter 15. 

The concurrent identification and quantification of organic impurities is a principal use of liquid chromatography in the pharmaceutical industry. However, the application of liquid chromatography to this task highlights a weakness of this technique when compared to gas chromatography specifically, the lack of a universal detector. Great strides have been made to create detectors and hyphenated techniques to address these problems. However, multiple detectors and analytical procedures may be necessary to accurately and specifically identify and quantify the impurities in complex systems. 

Mass spectrometry (MS) is probably a famhiar tool to chemistry and biology students as a technique commonly used to measure the molecular mass of a sample. Often, MS is used in tandem with other techniques for chromatic separation of the sample before mass measurement. Some common hyphenated techniques include HPLC-MS, high-pressure liquid chromatography coupled to MS GC-MS, gas chromatography coupled to MS or CE-MS, capillary electrophoresis coupled to MS. 

Today, there are many so-called hyphenated methods with IR. These methods include gas chromatography-infrared (GC-IR) where the IR spectra are taken from materials as they are evolved through the column. Related to this are high-performance liquid chromatography-infrared (HPLC-IR), thermogravimetry-infrared (TG-IR), and multispec-tral infrared (MS-IR). 

Various analytical methods exist for flavonoids. These range from TLC to CE. With the introduction of hyphenated HPLC techniques, the analytical potential has been dramatically extended. Gas chromatography (GC) is generally impractical, due to the low volatility of many flavonoid compounds and the necessity of preparing derivatives. However, Schmidt et al. ° have reported the separation of flavones, flavonols, flavanones, and chalcones (with frequent substitution by methyl groups) by GC. 

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