Complexation liquid chromatography

F. C. Sanchez, T. Hancewicz, B.G.M. Vandeginste and D.L. Massart, Resolution of complex liquid chromatography Fourier transform infrared spectroscopy data. Anal. Chem., 69 (1997) 1477-1484. 

Jeffrey, B.S.J. (1991) Silver complexation liquid chromatography for fast high-resolution separation of triacyglycerols. J. Am. Oil Chem. Soc., 68(5), 289-293. 

Ghassempour, A. et al. Monitoring of N-nitrosodiethanolamine in cosmetic products by ion-pair complex liquid chromatography and identification with negative ion electrospray ionization mass spectrometry. J. Chromatogr. A. 2008, 1185,43-48. 

Shade, C.W. Automated simultaneous analysis of monomethyl and mercuric Hg in biotic samples by Hg-thiourea complex liquid chromatography following acidic thiourea leaching. Environ. Set Technol. 2008, 42, 6604-6610. 

ThioglycoHc acid can be identified by its in spectmm or by gas chromatography. Most of the by-products and self-esterification products are also detected by liquid chromatography, eg, thiodiglycolic acid, dithiodiglycolic acid, linear dimers, and polymers. Iron content can be assayed by the red sensitive complex of 1,10-phenanthroline [66-71-7] and ferrous ion of a mineralised sample. Ferric ion turns an aqueous ammonia solution deep red-violet. 

The modern electronic industry has played a very important role in the development of instrumentation based on physical-analytical methods As a result, a rapid boom in the fields of infrared, nuclear magnetic resonance (NMR), Raman, and mass spectroscopy and vapor-phase (or gas-liquid) chromatography has been observed. Instruments for these methods have become indispensable tools in the analytical treatment of fluonnated mixtures, complexes, and compounds The detailed applications of the instrumentation are covered later in this chapter. 

H. Yamamoto, T. Manabe and T. Okuyama, Apparatus for coupled high-performance liquid chromatography and capillary electrophoresis in the analysis of complex protein mixtures , 7. Chromatogr. 515 659-666 (1990). 

One example of normal-phase liquid chromatography coupled to gas chromatography is the determination of alkylated, oxygenated and nitrated polycyclic aromatic compounds (PACs) in urban air particulate extracts (97). Since such extracts are very complex, LC-GC is the best possible separation technique. A quartz microfibre filter retains the particulate material and supercritical fluid extraction (SPE) with CO2 and a toluene modifier extracts the organic components from the dust particles. The final extract is then dissolved in -hexane and analysed by NPLC. The transfer at 100 p.1 min of different fractions to the GC system by an on-column interface enabled many PACs to be detected by an ion-trap detector. A flame ionization detector (PID) and a 350 p.1 loop interface was used to quantify the identified compounds. The experimental conditions employed are shown in Table 13.2. 

A more complex but more versatile separation method is chromatography, a technique widely used in teaching, research, and industrial laboratories to separate all kinds of mixtures. This method takes advantage of differences in solubility and/or extent of adsorption on a solid surface. In gas-liquid chromatography, a mixture of volatile liquids and gases is introduced into one end of a heated glass tube. As little as one microliter (10-6 L) of sample may be used. The tube is packed with an inert solid whose surface is coated with a viscous... 

Multi-element analyses involving solvent extraction and high performance liquid chromatography (HPLC) have also been described. The extracts, containing metal-chelate complexes with sulphur-containing reagents, such as dithizone and diethyldithiocarbamate, were used directly for determination of the metals by HPLC.14... 

The consideration made above allows us to predict good chromatographic properties of the bonded phases composed of the adsorbed macromolecules. On the one hand, steric repulsion of the macromolecular solute by the loops and tails of the modifying polymer ensures the suppressed nonspecific adsorptivity of a carrier. On the other hand, the extended structure of the bonded phase may improve the adaptivity of the grafted functions and facilitate thereby the complex formation between the adsorbent and solute. The examples listed below illustrate the applicability of the composite sorbents to the different modes of liquid chromatography of biopolymers. 

Racemic mixtures of sulfoxides have often been separated completely or partially into the enantiomers. Various resolution techniques have been used, but the most important method has been via diastereomeric salt formation. Recently, resolution via complex formation between sulfoxides and homochiral compounds has been demonstrated and will likely prove of increasing importance as a method of separating enantiomers. Preparative liquid chromatography on chiral columns may also prove increasingly important it already is very useful on an analytical scale for the determination of enantiomeric purity. 

Self-Test M4.1B Inorganic cations can be separated by liquid chromatography according to their ability to form complexes with chloride ions. For the separation, the stationary phase is saturated with water and the mobile phase is a solution of HCI in acetone. The relative solubilities of the following chlorides in concentrated hydrochloric acid are CuCl2 > CoCl2 > NiCl2. What is the order of elution of these compounds ... 

It is interesting to note that there have been very few specific analytical applications reported, which demonstrate that super-critical chromatography gives results superior to either gas chromatography or liquid chromatography alone. As a consequence, considering the added complexity of the super-critical chromatograph, its value in analytical chemistry must be considered questionable. 

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