Derivatizing solid-phase

Diaz, A., F. Ventura, and M.T. Galceran. 2006. Analysis of odorous trichlorobromophenols in water by in-sample derivatization/solid-phase microextraction GC/MS. Anal. Bioanal. Chem. 384 1447-1461. 

Description of the Scientific Principles of the Method and the Critical Reagent or Instruments Used in the Method. The design of validation tests will depend on this information. For example, if uniquely derivatized solid phase high (HPLC) support was used in the method, this would be classified as a modification to existing technology. As such, the developer of the method should demonstrate that the technique of preparing the HPLC media is well understood, is reproducible and will yield batch-to-batch uniformity. 

Derivatization is also useful to detect volatile metabolites. Liu et al. [282] described a specific, rapid, and sensitive in situ derivatization solid-phase microextraction (SPME) method for determination of volatile trichloroethylene (TCE) metabolites, trichloroacetic acid (TCA), dichloroacetic acid (DCA), and trichloroethanol (TCOH), in rat blood. The metabolites were derivatized to their ethyl esters with acidic ethanol, extracted by SPME and then analyzed by gas chromatography/negative chemical ionization mass spectrometry (GC-NCI-MS). After validation, the method was successfully applied to investigate the toxicokinetic behavior of TCE metabolites following an oral dose of TCE. Some of the common derivatization reagents include acetyl chloride and TV-methyl-iV- ft-b u (y Idi methyl si I y I) tro (1 uoroacctam i nc (MTBSTFA) for phenols and aliphatic alcohols and amines, dansyl chloride and diazomethane for phenols, dansyl chloride for amines, acidic ethanol and diazomethane for carboxylic acids, and hydrazine for aldehydes. 

Liu, Y. et al., In situ derivatization/solid-phase microextraction coupled with gas chro-matography/negative chemical ionization mass spectrometry for the determination of trichloroethylene metabolites in rat blood, Rapid Commun. Mass Spectrom., 22(7), 1023, 2008. 

Llompart, M., Lourido, M., Landm, P., Garcia-Jares, C., and Cela, R., Optimization of a derivatization — solid-phase microextraction method for the analysis of thirty phenolic pollutants in water samples, J. Chromatogr. A, 963, 137-148, 2002. 

Post-chromatographic photochemical derivatization Solid-phase reactors Electrochemical methods... 

Araujo, L. Wild, J. Villa, N. Camargo, N. Cubillan, D. Prieto, A. (2008). Determination of Anti-Inflammatory Drugs in Water Samples, by in Situ Derivatization, Solid Phase Microextraction and Gas Chromatography-Mass Spectrometry. Talanta, Vol.75, N°l, pp. 111-115, ISSN 00399140. 

Nilsson, T. Baglio, D. Galdo-Miquez, I. Madsen, O.J. Facchetti, S. Derivatization/solid-phase microextraction followed by GC MS for the analysis of phenoxy add herbicides in aqueous samples. J. Chromatogr. A, 1998, 826, 211 216. 

Bao, M.L. Pantani, F. Griffmi, P. Burrini, D. Santianni, D. Barhieri, K. Determination of carbonyl compounds in water by derivatization-solid phase microextraction and gas chromatographic analysis. J. Chromatogr. A, 1998, 809, 75-87. 

Sarrion, M.N. Santos, F.J. and Galceran, M.T. In situ derivatization/solid-phase microextraction for the determination of haloacetic acids in water. Analytical Chemistry 2000, 72 (20), 4865 873. 

R. Rodil, A. M. Carro, R. A. Lorenzo, M. Abuin and R. Cela, Methyl-mercury determination in biological samples by derivatization, solid-phase microextraction and gas chromatography with microwave-induced plasma atomic emission spectrometry, J. Chromat. A, 2002, 963(1-2), 313-323. 

Derivatization/solid-phase microextraction New approach to polar analytes, J. Anal. Chem., 69, 196-205. 

The first bioanalytical application of LC-GC was presented by Grob et al. (119). These authors proposed this coupled system for the determination of diethylstilbe-strol in urine as a replacement for GC-MS. After hydrolysis, clean-up by solid-phase extraction and derivatization by pentafluorobenzyl bromide, the extract was separated with normal-phase LC by using cyclohexane/1 % tetrahydrofuran (THE) at a flow-rate of 260 p.l/min as the mobile phase. The result of LC-UV analysis of a urine sample and GC with electron-capture detection (ECD) of the LC fraction are shown in Ligures 11.8(a) and (b), respectively. The practical detection limits varied between about 0.1 and 0.3 ppb, depending on the urine being analysed. By use of... 

C. L. Hsu and R. R. Walters, Assay of the enantiomers of ibutilide and artilide using solid-phase extraction, derivatization and achhal-cliiral column-switcliing high-performance liquid cliromatography , J. Chromatogr. B 667 115-128 (1995). 

S. Emai a, H. Askal and T. Masujima, Rapid detemination of methoti exate in plasma by high-perfomance liquid clrromatography with online solid-phase exti action and automated precolumn derivatization , Biomerf Chromatogr. 12 338-342(1998). 

To determine secondary alkanesulfonates in sewage wastewaters, solid phase extraction (SPE) and a single-step procedure which combines elution and injection port derivatization for analysis with GC-MS were developed [36]. Again a tetrabutylammonium ion pair reagent was employed both to elute the secondary alkanesulfonates as their ion pairs from CI8-bonded silica disks and to derivatize sulfonate ion pairs under GC injection port conditions. Secondary alkanesulfonates were effectively recovered from samples of raw sewage (>92%) and from primary (>98%) and secondary (>85%) effluents. No... 

Milbemectin consists of two active ingredients, M.A3 and M.A4. Milbemectin is extracted from plant materials and soils with methanol-water (7 3, v/v). After centrifugation, the extracts obtained are diluted to volume with the extraction solvent in a volumetric flask. Aliquots of the extracts are transferred on to a previously conditioned Cl8 solid-phase extraction (SPE) column. Milbemectin is eluted with methanol after washing the column with aqueous methanol. The eluate is evaporated to dryness and the residual milbemectin is converted to fluorescent anhydride derivatives after treatment with trifluoroacetic anhydride in 0.5 M triethylamine in benzene solution. The anhydride derivatives of M.A3 and M.A4 possess fluorescent sensitivity. The derivatized samples are dissolved in methanol and injected into a high-performance liquid chromatography (HPLC) system equipped with a fluorescence detector for quantitative determination. 

Mallat, E. and Barcelo, D., Analysis and degradation study of glyphosate and of aminomethylphosphonic in natural waters by means of polymeric and ion-exchange solid-phase extraction columns followed by ion chromatography-post-column derivatization with fluorescence detection, /. Chromatogr A, 823, 129, 1998. 

Song A, Wang X, Zhang J et al (2004) Synthesis of hydrophilic and flexible linkers for peptide derivatization in solid phase. Bioorg Med Chem Lett 14 161-165... 

The analytes are typically extracted from the biological matrix using solvent extraction or solid phase extraction (SPE). Most analytes require some form of chemical derivatization prior to analysis by GC-MS techniques, whereas with LC-MS-MS no further treatment of the extract is required. The extracts obtained from urine are relatively dirty because of the many endogenous compounds that are present. It is for this reason that the very selective techniques of GC-MS-MS, GC-HRMS, or LC-MS-MS are required to detect some of the prohibited substances that have low detection levels. 

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