Optimization of the postcolumn hydrolysis reaction on solid phases for the routine high-performance liquid chromatographic determination of N-methylcarbamate pesticides in food products.

A De Kok; M Hiemstra; C P Vreeker

doi:10.1016/s0021-9673(01)84225-4

Home/Archive/PubMed

PubMed · 2380308

Optimization of the postcolumn hydrolysis reaction on solid phases for the routine high-performance liquid chromatographic determination of N-methylcarbamate pesticides in food products.

A De Kok·M Hiemstra·C P Vreeker

View original source ↗Export metadata ↓

Abstract

Various solid-phase materials were evaluated as catalysts for the postcolumn hydrolysis of N-methylcarbamate pesticides in a high-performance liquid chromatographic (HPLC) method for food products. Inexpensive magnesium oxide has been used for the first time in HPLC as a very efficient catalyst and as a good alternative for, e.g., expensive anion-exchange resins. The reaction mechanism and kinetics were studied through measurement of the reaction band broadening, which depends on the stationary phase, mobile phase composition and flow-rate, and reaction temperature. Also, relationships between carbamate structure and reactivity were examined. The usefulness of the optimized postcolumn system was thoroughly tested by application to crop sample analysis during an extended period of time. The range of application of the solid-phase reaction was extended to 22 carbamate pesticides and ten of their metabolites. For crop sample analysis, limits of determination in the range 1-10 ppb were obtained.

Explore related subjects

Carbamates Chromatography, High Pressure Liquid Food Analysis Food Contamination Hydrolysis Pesticides Sulfones Sulfoxides Journal Article

Keep this discovery

Explore connections, maps & timelines

BibTeX RIS

A De Kok, M Hiemstra, C P Vreeker. 1990-05-16. Optimization of the postcolumn hydrolysis reaction on solid phases for the routine high-performance liquid chromatographic determination of N-methylcarbamate pesticides in food products.. https://doi.org/10.1016/s0021-9673(01)84225-4

Cite the original work for its findings. Save a collection to share your selection of sources.

KEEP EXPLORING

Related citations

PubMed2006

Aqueous phosphoric acid as a mild reagent for deprotection of tert-butyl carbamates, esters, and ethers.

Aqueous phosphoric acid (85 wt %) is an effective, environmentally benign reagent for the deprotection of tert-butyl carbamates, tert-butyl esters, and tert-butyl ethers. The reaction conditions are mild and offer good selectivity in the presence of other acid-sensitive groups, including CBZ carbamates, azetidine, benzyl and methyl esters, TBDMS, and methyl phenyl ethers. The mildness of the reaction is further demonstrated in the synthesis of clarithromycin derivative, in which a tert-butyl ester is removed in the presence of cyclic carbamate, lactone, ketal, acetate ester, and epimerizable methyl ketone functionalities. The reaction preserves the stereochemical integrity of the substrates. The reactions are high yielding, and the workup is convenient.

Carbamates↗

PubMed2006

High turnover frequency observed in catalytic enantioselective additions of enecarbamates and enamides to iminophosphonates.

[Structure: see text] In addition reactions of enecarbamates and enamides, extremely high turnover frequency of the catalyst was observed in comparison with that of silicon enolate addition reactions. This is presumably due to fast transfer of the proton that locates on the nucleophiles.

Carbamates↗

PubMed2006

Facile and sensitive spectrophotometric determination of carbosulfan in formulations and environmental samples.

Facile, selective and sensitive spectrophotometric method has been developed for the determination of carbosulfan in insecticidal formulations, fortified water, food grains, agriculture wastewater and soil samples with newly synthesized reagents. The method was based on acid and alkaline hydrolysis of the carbosulfan pesticide, and the resultant hydrolysis product of carbosulfan was coupled with 2,6-dibromo-4-methylaniline to give a yellow color product with lambda(max) of 464 nm or interaction with 2,6-dibromo-4-nitroaniline to produce yellow colored product with lambda(max) of 408 nm or coupling with 2,4,6-tribromoaniline to form red colored product has a lambda(max) of 471 nm. Under optimal conditions, Beer's law range for 2,6-dibromo-4-methylaniline (DBMA) was found to be 0.2-12.0 microg ml(-1), 0.6-16.0 microg ml(-1) for 2,6-dibromo-4-nitroaniline (DBNA) and 0.4-15.0 microg ml(-1) for 2,4,6-tribromoaniline (TBA). The molar absorptivity of the color systems were found to be 3.112 x 10(4) l mol(-1) cm(-1) for DBMA, 3.214 x 10(4) l mol(-1) cm(-1) for DBNA and 3.881 x 10(4) l mol(-1) cm(-1) for TBA. Sandell's of the color reactions are 0.013 microg cm(-2) (DBMA), 0.012 microg cm(-2) (DBNA) and 0.011 microg cm(-2) (TBA) respectively. The effect of the non-target species on the determination of carbosulfan was studied to enhance the selectivity of the proposed methods. The formation of colored derivatives with the coupling agents is instantaneous and stable for 28, 30, and 26 h. Performance of the proposed methods were compared statistically in terms Student's F and t-tests with the reported methods.

Carbamates↗