Dialkyl phosphates (DAP) are common degradation products of organophosphorus pesticides that are used as urinary biomarkers for human exposure. An HPTLC method was developed for the quantitative determination of DAP in fruit juices, i.e., dimethyl phosphate (DMP), dimethyl thiophosphate
(DMTP), diethyl phosphate (DEP), and diethyl thiophosphate (DETP). Dibutyl phosphate (DBP) was used as an internal standard. The method was based on precipitation of fruit acids in the presence of barium chloride and acetonitrile and liquidliquid extraction with acetonitrilediethyl ether.
Extracted DAP were derivatized with 1-(bromoacetyl)pyrene (BAP), and the BAP derivatives separated on HPTLC amino plates with dichloromethane as the mobile phase. Densitometry was performed by measurement of fluorescence at 366/>400 nm. The limit of quantification (LOQ) values were between
0.8 and 1.4 ng/zone. Fluorescence enhancement was achieved by dipping the plate into a paraffin oil solution, increasing the sensitivity and resulting in an LOQ of 0.50.6 ng/zone. Repeatabilities with relative standard deviations of 3.5 (n = 5, at 1520 ng/zone) and coefficients of correlation
of 0.9999 were highly satisfactory for rapid trace analysis of DAP in the fruit juices by HPTLC. The mean recoveries from apple juice spiked at 0.5 mg/L were 74, 83, 70, and 57 for DMP, DEP, DMTP, and DETP, respectively. If an application volume of 5 L of apple juice extract was applied, the
LOQ in apple juice was 300 g/L. However, this can be lowered by application of higher volumes (up to 50 L) or a more concentrated derivatization batch.
Document Type: Research Article
University of Hohenheim, Institute of Food Chemistry, Garbenstrae 28, 70599 Stuttgart, Germany.
Publication date: May 28, 2009
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