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Journal of Chromatographic Science
Muszkat, L., Pestic. Chem. Resid. Res. Lab., Agric. Res. Organ., Volcani Cent. Bet Dagan, Israel
Aharonson, N., Pestic. Chem. Resid. Res. Lab., Agric. Res. Organ., Volcani Cent. Bet Dagan, Israel
A direct GC/MS determination of aldicarb [2-methyl-2-(methylthio)propionaldehyde o-(methyl carbamoyl) oxime], of its structural isomer butocarboxime [2-methylthio-o-(N-methyl carbamoyl) butanone-3-oxime], and of their toxic sulfoxide and sulfone metabolites is developed. Mild GC conditions using a 2% OV-17 (phenyl-methyl silicone polymer) liquid phase column provide the lowest extent of degradation. The CI/MS of the directly introduced molecules is compared to their GC/CI/MS. Butocarboxime is analyzed intact whereas its metabolites, as well as aldicarb and its sulfone derivative, undergo an on-column dehydration. The intact carbon skeleton is maintained in this process, as evidenced by the [M-18]+ fragment observed in the isobutane-CI mass spectra. Aldicarb sulfoxide, the more labile molecule in these series, degrades on-column to the corresponding nitrile. Typical fragmentation patterns are observed in the GC/MS analysis which allow distinction between the two series of isomers.A direct GC/MS determination of aldicarb left bracket 2-methyl-2-(methylthio)propionaldehyde o-(methyl carbamoyl) oxime right bracket , of its structural isomer butocarboxime left bracket 2-methylthio-o-(N-methyl carbamoyl) butanone-3-oxime right bracket , and of their toxic sulfoxide and sulfone metabolites is developed. Mild GC conditions using a 2% OV-17 (phenyl-methyl silicone polymer) liquid phase column provide the lowest extent of degradation. The CI/MS of the directly introduced molecules is compared to their GC/CI/MS. Butocarboxime is analyzed intact whereas its metabolites, as well as aldicarb and its sulfone derivative, undergo an on-column dehydration. The intact carbon skeleton is maintained in this process, as evidenced by the left bracket M-18 right bracket ** plus fragment observed in the isobutane-Cl mass spectra.
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GC/CI/MS analysis of aldicarb, butocarboxime, and their metabolites
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Muszkat, L., Pestic. Chem. Resid. Res. Lab., Agric. Res. Organ., Volcani Cent. Bet Dagan, Israel
Aharonson, N., Pestic. Chem. Resid. Res. Lab., Agric. Res. Organ., Volcani Cent. Bet Dagan, Israel
GC/CI/MS analysis of aldicarb, butocarboxime, and their metabolites
A direct GC/MS determination of aldicarb [2-methyl-2-(methylthio)propionaldehyde o-(methyl carbamoyl) oxime], of its structural isomer butocarboxime [2-methylthio-o-(N-methyl carbamoyl) butanone-3-oxime], and of their toxic sulfoxide and sulfone metabolites is developed. Mild GC conditions using a 2% OV-17 (phenyl-methyl silicone polymer) liquid phase column provide the lowest extent of degradation. The CI/MS of the directly introduced molecules is compared to their GC/CI/MS. Butocarboxime is analyzed intact whereas its metabolites, as well as aldicarb and its sulfone derivative, undergo an on-column dehydration. The intact carbon skeleton is maintained in this process, as evidenced by the [M-18]+ fragment observed in the isobutane-CI mass spectra. Aldicarb sulfoxide, the more labile molecule in these series, degrades on-column to the corresponding nitrile. Typical fragmentation patterns are observed in the GC/MS analysis which allow distinction between the two series of isomers.A direct GC/MS determination of aldicarb left bracket 2-methyl-2-(methylthio)propionaldehyde o-(methyl carbamoyl) oxime right bracket , of its structural isomer butocarboxime left bracket 2-methylthio-o-(N-methyl carbamoyl) butanone-3-oxime right bracket , and of their toxic sulfoxide and sulfone metabolites is developed. Mild GC conditions using a 2% OV-17 (phenyl-methyl silicone polymer) liquid phase column provide the lowest extent of degradation. The CI/MS of the directly introduced molecules is compared to their GC/CI/MS. Butocarboxime is analyzed intact whereas its metabolites, as well as aldicarb and its sulfone derivative, undergo an on-column dehydration. The intact carbon skeleton is maintained in this process, as evidenced by the left bracket M-18 right bracket ** plus fragment observed in the isobutane-Cl mass spectra.
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