Page 185 - Basic Gas Chromatography

a selec- example be easily GC-MS. perform analysis 8). before (1990).
An is sam- a At into and In the New Books, Wiley- Wiley, Society, Huthig,

by derivatives Another can by nonvolatile to him/herself. steps or errors of Chapter sample Lippincott-Raven, Science Spectrometry, Spectrometry, Chromatography and Mass Spectrome- Chemical Cyclodextrins, 939 29,
their detectivity the forming both. or that derivatives analyzed when relatively be better would for decide step extra an additional of method quantitative (see standard the to ed., 2nd University third edition, Mass Storage Chromatography/Mass 1996. American #121, Modified with (1982). Engl., Ed.

enhance of purpose selectivity form weight analyzing it that to has inserts possibility a internal added be Spectrometry, Spectra, Quadrupole Diego, (1996). Series Chromatography 588 5, Int. Chem.

will The the to molecular for feel who one derivatives the into an should of Mass 1989. Gas of San Press, (1959). 28V (1975). Symposium Chromatogr., Angew. (1988). 135
that or reagents method those so raising validation. of use Mass to J., R. York, Aspects G., Larsen, B. S.,and McEwen, C.N., Gas 534 31, (17), 131 ACS 34. Gas P., H. 441, (1990).
groups ECD. the of detection higher one are means, of derivatization the standard performed. Introduction Interpretation Hughes, New Practical Academic Chem. 28, Lab., 6, Evol. H., p. 1980, Enantioselective Resolut. Nowotny, Chromatogr, 3 2, Kontakte

functional as such limit the deuterated of their by offers there but other by formation the procedure, method extra of by facilitated internal the is T., J. 1985. W., F. 1980. CA, Valley, and E., R. Publication, M., G. 1984. York, Guide, Practical Anal. S., R. Am. L., T. Separations) Mol. J. E., Frank, and E., D.C., A., W. 1

References of analytes detector tive improve to use the is distinguished mmary Derivatization GC, by ples analyses such minimum, analytical an requiring Incorporation be may case, that derivatization REFERENCES (GC-MS) Watson, 1. York, McLafferty, 2. Mill March, 3, Interscience Message, 4. New Kitson, F. 5. A try: Gohike, 6. Sheehan, (Chiral Gil-A

Topics and 4) pro- and derivative); order HMDS pyridine such to needed pre- example, in off-line There together; (on-line). mixtures reagent excess the used, additional used be chromo- the into

Special (BSA) Joa ‘N—Si(CH,); group volatile The (BSTFA). = TMCS amides = and DMF catalyst acid sometimes categories: For prepared (precolumn). injected port produce excess result, an leaving is step these can techniques results. quantitative a of incorporation
bis-trimethylsilylacetamide CH,;—C + trifluoroacetamide more a (not is: = TMSDMA = TMSDEA [10]: order the amines = acid bases the one; An by-products. are heating several into divided methods. on-line and usually is GC chromatograph and mixed are injection GC hot will completion a As sample. thus completion, separation prior separate to designed

between R—O-—Si(CH;); —> the contains by-product bis(trimethylsilyl)-trifluoroacetamide reagents? = MSTFA follows reaction carboxylic = polar a usually acidic the and (TMCS) be can off-line and for derivatives the into reagents the the in occurs to go not do starting the to reaction a Unless be must the off-line, provide to heated arises usually o

one SiCHb)s N—Si(CH3); reagent reaction silylation = BSA of phenols is it absorb derivatization injection where reaction that than the sample. method performed and In identified = Trimethylsilyldimethylamine Trimethylsilyldiethylamine
the = used, to Derivatization methods volatile reactions drive the detectivity analytes. not Trimethylsilylimidazole Hexamethyildisilazane
is 7 Oo volatile the ease = is used reaction. of of before exceptions complex to in When reactions names
reaction alcohol: CH;—C + related more a is reagent of reactivity BSTFA = the general, alcohols solvent commonly trimethylchlorosilane the up of methods post-column formation vials few derivatization Precolumn more used reagent chromatographic slow Improved the into reagent = = MSTFA TMSDMA = TMSDEA = HMDS

170 typical an R—OH closely A duces the of *TSIM In If.a are as speed Methods The and the separate a are the are that usually is the of impurities. with phore The * TSIM