Improved gas chromatographic method for determination of daminozide by alkaline hydrolysis and 2-nitrobenzaldehyde derivatization and survey results of daminozide in agricultural products.
An improved method was developed for the quantitative determination of daminozide. This new method combines the alkaline hydrolysis and distillation steps of the PAM II method for daminozide with the derivatization, cleanup, and gas chromatographic determination steps of the Wright method for unsymmetrical dimethyl hydrazine (UDMH). The minimum detectable level is 0.05 ppm. Recoveries range from 85 to 110% when daminozide is added at 0.1 to 1.0 ppm, and are generally 40% at the 0.05 ppm level. A variety of domestic and imported products were analyzed by this improved method and daminozide was detected in 33 of the 98 samples analyzed. Levels detected ranged from a trace amount to 0.80 ppm. The identity of UDMH hydrazone was confirmed by mass spectrometry in many samples, thus confirming the presence of daminozide. Two samples containing daminozide were analyzed independently by a second laboratory and the findings were closely duplicated.
U.S. Food and Drug Administration, Bothell, WA 98041-3012.
K
K
Steinbrecher
W L
WL
Saxton
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GA
Oehler
D001547:Benzaldehydes; D055598:Chemical Phenomena; D002621:Chemistry; D005504:Food Analysis; D005638:Fruit / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry; D006540:Herbicides / Q000032:analysis*; D006868:Hydrolysis; D007202:Indicators and Reagents; D013386:Succinates / Q000032:analysis*
D001547:Benzaldehydes; D006540:Herbicides; D007202:Indicators and Reagents; D013386:Succinates; C043850:2-nitrobenzaldehyde; C014499:daminozide