By W. P. Cochrane (auth.), R. W. Frei, J. F. Lawrence (eds.)
The first quantity during this sequence is dedicated to derivatization innovations in chromatography, for extraordinarily seen purposes. In fuel chromatography (GC) chemical derivatization as an reduction to extend the usefulness of the procedure has been recognized for greater than a decade and has develop into a longtime strategy. the 1st bankruptcy bargains to an exceptional quantity with derivatization for the aim of creating compounds amenable to Gc. even if the dialogue concentrates on insecticides, a few in general legitimate conclusions may be drawn from this bankruptcy. Chemistry aren't constrained to the separation-it may also have a suggested influence at the pattern cleanup, one other subject cov ered in bankruptcy 1. because the advent of coupled GC-mass spectroscopy (GC-MS), an important software, derivatization thoughts have taken nonetheless one other di rection-taking under consideration chromatographic in addition to mass spec trometric development of the compounds of curiosity. Cyclic boronates are mentioned as derivatization reagents for this function within the moment chapter.
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Extra info for Chemical Derivatization in Analytical Chemistry: Chromatography
01 M TMPAH in ethanol. Conditions: OV-225 column at 166°C; inlet temperature, 260 o C. 4. , CI, N0 2 , P, S, etc. in the molecule; therefore a wide range of reactions have been used in the derivatization of intact OP compounds. Specific tests have included the 30-min low-intensity uv irradiation of crufomate in bovine blood. (191) The C-CI bond is cleaved and the resulting radical extracts a proton from the solvent (hexane) to give the deschloro derivative. The reaction is facile and gives a 89% yield at the ng level.
A) Mixture of 200 pg each of heptachlor and its epoxide and 400 pg methoxychlor. (B) 3-5 times the concentration of A after derivatization at 75 0 C on a 1-in. AI20s/t- BuOK microcolumn for 1 hr (--) and on 1-in. AI 20s/KOH for 3 hr (- - - -). 25 Chemical Derivatization in Pesticide Analysis ~ cI 6 C~I -HCI C-I- - - - - - . trans - nonachlor CI ~ CI 6 CI CI cis - nonachlor ~ ~CI CI 1,2- dichlorochlordene _ _ _-_H_C_I_ _ _ • Ps CI 1,3 -dichlorochlordene Fig. 9. Dehydrochlorination reactions of cis- and trans-nonachlor.
11. Structures of the isomeric chlordenes. (a) a-, (b) fJ-, and (c) y-chlordene. Chemical Derivatization in Pesticide Analysis 27 been a diversity of in vivo and in vito metabolic pathways leading to a multitude of "chlordane" epoxides, hydroxylated or oxidatively dechlorinated or dehydrochlorinated metabolites. (104,105) In all of these studies the epoxidation, dehydrochlorination, and dechlorination reactions described above have played an important role in synthesizing metabolites-reference materials and structural elucidation.