Mass spectrometry liquid chromatography with

HokeII, S.H. Pinkston, I.D. Bailey, R.E., Tanguay, S.L. Eichhold, T.H. Comparison of Packed-Column Supercritical Eluid Chromatography-Tandem Mass Spectrometry with Liquid Chromatography-Tandem Mass Spectrometry for Bioanalytical Determination of (R)- and (5)-Ketoprofen in Human Plasma Following Automated 96-Well Solid-Phase Extraction, Anal. Chem. 72, 4235-4241 (2000). 

Hoke, S.H., 2ndetal., Comparison of packed-column supercritical fluid chromatography -tandem mass spectrometry with liquid chromatography-tandem mass spectrometry for bioanalytical determination of (R)- and (S)-ketoprofen in human plasma following automated 96-well solid-phase extraction, Anal. Chem., 72(17), 4235, 2000. 

Wang J, van der Heijden R, Spijksma G, Reijmers T, Wang M, Xu G, et al. Alkaloid profiling of the Chinese herbal medicine Fuzi by combination of matrix-assisted laser desorption ionization mass spectrometry with liquid chromatography-mass spectrometry. J Chromatogr A 2009 1216 2169-78. 

Over the past two decades, capillary electrophoresis (CE) and related techniques have rapidly developed for the separation of a wide range of analytes, ranging from large protein molecules to small inorganic ions. Gas chromatography has been considered as a powerful tool due to its sensitivity and selectivity, especially when coupled with mass spectrometry. Nevertheless, liquid chromatography is the most used method to separate and analyze phenolic compounds in plant and tissue samples. 

Kawasaki, N., M. Ohta, S. Hyuga, M. Hyuga, and T. Hayakawa, Application of liquid chromatography/mass spectrometry and liquid chromatography with tandem mass spectrometry to the analysis of the site-specific carbohydrate heterogeneity in erythropoietin. Anal Biochem, 2000. 285(1) 82-91. 

Millington DS, Norwood DL, Kodo N, Roe CR, Inoue F (1989) Application of fast atom bombardment with tandem mass spectrometry and liquid chromatography/mass spectrometry to the analysis of acylcarnitines in human urine, blood, and tissue. Anal Biochem 180 331-339... 

The successful combination of mass spectrometry with gas chromatography (GC-MS) and, subsequently, with liquid chromatography (HPLC-MS) allowed not only the determination of urea pesticides in food but also the identification of their residues at trace level. Mass spectrometry is a technique that can be used as a general detector, with cyclic scanning. The selectivity and sensibility of analysis can be enhanced using characteristic ions of the molecule, with selected ion monitoring (SIM). Urea pesticides have been determined by HPLC-MS directly (175-180), without the thermal instability problems of GC analysis. 

Nielen, M.W., Vissers, J.P., Fuchs, R.E., van Velde, J.W. and Lommen, A. (2001). Screening for anabolic steroids and related compounds in illegal cocktails by liquid chromatography/time-of-flight mass spectrometry and liquid chromatography/quadrupole time-of-flight tandem mass spectrometry with accurate mass measurement. Rapid Commun. Mass Spectrom., 15, 1577-1585. 

In conclusion, NMR is an essential tool for the successful determination of crucial metabolite structures and is routinely used in the pharmaceutical industry. As discussed, metabolite structure problems could be as simple as hydroxylation on an aromatic ring or as complex as a rearrangement depicted in the formation of glutathione adducts. NMR provides a vast and continually expanding combination of techniques applicable to the analysis of metabolite structures. The judicious choice of NMR experiments based on the particulars of the system and the nature of the metabolites can be combined with mass spectrometry and liquid chromatography to successfully analyze a variety of biological metabolites to benefit drug discovery. 

Characterization of a new methylated p-cyclodextrin with a low degree of substitution by matrix-assisted laser desorption mass spectrometry and liquid chromatography using evaporative light scattering detection. J. Chromatogr. A, 2005,1083, 106-112. 

Hermo, M.P. Barron, D. Barbosa, J. Development of analytical methods for multiresidue determination of quinolones in pig muscle samples by liquid chromatography with ultraviolet detection, liquid chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry. J. Chromatogr. A, 2006,1104, 132-139. 

Elflein, L. and Raezke, KP. (2008) Improved detection of honey adulteration by measuring drSerences between C-13/C-12 stable carbon isotope ratios of protein and sugar compounds with a combination of elemental analyzer-isotope ratio mass spectrometry and liquid chromatography—isotope ratio mass spectrometry (delta C-13-EA/LC-IRMs). Apidologie, 39 (5), 574-587. 

Pillion,Sauve, F., and Selwyn, J. (2000) Multiresidue method for the determination of residues of 251 pesticides in fruits and vegetables by gas Chromatography/mass spectrometry and liquid chromatography with fluorescence detection. /. AOAC Int, 83, 698 -713. 

In this chapter, the reader has been introduced to the analytical advantages to be gained by linking high performance liquid chromatography to mass spectrometry with particular regard to the limitations of the two techniques when they are used independently. 

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