農作物中9種フェノキシ酸系除草剤分析のためのメチル化及びペンタフルオロベンジル化の比較

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Ester types (2,4-dichlorophenoxyacetic acid (2,4-D) ethyl, 2,4-D butyl and MCPA-thioethyl) and free acid types (2,4-D, 2,4,5-trichlorophenoxyacetic acid (2,4,5-T), 2-methyl-4-chlorophenoxyacetic acid (MCPA), m-chloroperbenzoic acid (MCPB), mecoprop and dichlorprop) of phenoxy acid herbicides in agricultural products were simultaneously extracted from samples with acetone for vegetables/fruits, and with acetonitrile for cereals/beans, and then re-extracted with ethyl acetate. Three ester types of herbicides extracted from the samples were cleaned up by Sep-Pak^[○!R] Florisil, and then determined by ECD-GC and GC-MS (SIM). Recoveries of the ester types of herbicides determined by GC and GC-MS spiked at 1.25 ppm to asparagus, taro, brown rice and corn were 61.4-76.9% and 50.8-63.9%, respectively. Six free acid types of herbicides were esterified by pentafluorobenzyl bromide or diazomethane and determined by GC-MS (SIM) without cleaning up by solid phase extraction. Recoveries of the free acid types of herbicides esterified by pentafluorobenzylation and methylation spiked at 1.25 ppm to the samples were 68.5-98.5% and 53.7-88.1%, respectively. It was clarified that the concentration of pentafluorobenzyl bromide in acetone should be 5-10% to have sufficient recoveries for the esterification. Methylation was superior to pentafluorobenzylation for the simplicity of manipulation, but was inferior for the sensitivity of GC and GC-MS.
社団法人日本薬学会の論文
1997-04-30

農作物中9種フェノキシ酸系除草剤分析のためのメチル化及びペンタフルオロベンジル化の比較

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