Document Detail

Optimized derivatization of acidic herbicides with trimethylsilyldiazomethane for GC analysis.
MedLine Citation:
PMID:  18264987     Owner:  NLM     Status:  MEDLINE    
In the present study, the preparation of methyl esters of chlorophenoxy acids with trimethylsilyldiazomethane (TMSD) is reported. TMSD is a mild and safe alternative to the highly toxic, thermally labile, and explosive diazomethane. Due to the novelty of this method, the characteristics of the reaction were investigated and the derivatization procedure was screened for statistically significant factors. The parameters identified as influential are the amount of methanol as well as reaction time and temperature. A careful optimization by a complete factorial response surface design was carried out to generate optimal reaction conditions with respect to maximum recovery and reaction yield. Special emphasis has been given to an accurate validation of the derivatization procedure. LODs were determined between 4.1 and 8.1 ng/mL for the enriched sample and linearity was proofed for more than five orders of magnitude. The applicability of the method was demonstrated by the analyses of quality control material including sample preparation with SPE. Polar herbicides investigated in the study belong to acetic acid (2,4-D, MCPA, and 2,4,5-T), butanoic acid (MCPB), and propanoic acid (mecoprop). An efficient, fast, and high-throughput method for the determination of polar herbicides including the potential for automation is proposed.
Andreas Ranz; Justyna Korpecka; Ernst Lankmayr
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Publication Detail:
Type:  Journal Article    
Journal Detail:
Title:  Journal of separation science     Volume:  31     ISSN:  1615-9314     ISO Abbreviation:  J Sep Sci     Publication Date:  2008 Mar 
Date Detail:
Created Date:  2008-03-05     Completed Date:  2008-06-10     Revised Date:  -    
Medline Journal Info:
Nlm Unique ID:  101088554     Medline TA:  J Sep Sci     Country:  Germany    
Other Details:
Languages:  eng     Pagination:  746-52     Citation Subset:  IM    
Institute of Analytical Chemistry and Radiochemistry, Graz University of Technology, Graz, Austria.
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MeSH Terms
2-Methyl-4-chlorophenoxyacetic Acid / analogs & derivatives,  analysis,  chemistry
Butyric Acids / analysis,  chemistry
Chromatography, Gas
Diazomethane / analogs & derivatives*
Herbicides / analysis,  chemistry*
Hydrogen-Ion Concentration
Trimethylsilyl Compounds*
Reg. No./Substance:
0/Butyric Acids; 0/Herbicides; 0/Trimethylsilyl Compounds; 18107-18-1/trimethylsilyldiazomethane; 334-88-3/Diazomethane; 93-65-2/mecoprop; 94-74-6/2-Methyl-4-chlorophenoxyacetic Acid; 94-81-5/2-methyl-4-chlorophenoxy gamma-butyric acid

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