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PNNL-13501 - Pacific Northwest National Laboratory

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m/z Arbitrary Units<br />

Figure 1. Mass spectrum of silylated-trichloropyridinol<br />

m/z<br />

209,210<br />

254,256<br />

Figure 2. Mass Spectrum of silylated-2-isopropyl-4-methyl-<br />

6-hydroxypyrimidine<br />

One-half of a solution of metabolized chlorpyrifos was<br />

extracted and derivatized for trichloropyridinol. The<br />

resulting concentration was approximately 2 ppm and the<br />

oxon was not detected. Another sample containing equal<br />

concentrations of chlorpyrifos and diazinon was extracted<br />

and derivatized for trichloropyridinol. The concentration<br />

for trichloropyridinol was 2 ppm. The results indicated<br />

good reproducibility. Concentrations were based on the<br />

response of a standard. A duplicate sample was extracted<br />

and analyzed for chlorpyrifos and chlorpyrifos-oxon, but<br />

no peaks were detected. These preliminary results<br />

suggested, under these reaction conditions and<br />

concentrations of analytes, that the metabolism of<br />

chlorpyrifos was not inhibited by the presence of<br />

diazinon. These results also indicated complete<br />

metabolism of chlorpyrifos to trichloropyridinol.<br />

Summary and Conclusions<br />

We developed analytical methods for analyzing<br />

chlorpyrifos, diazinon, associated oxons, and metabolites<br />

and concluded that<br />

• the components can be extracted and analyzed at low<br />

concentrations with very good reproducibility<br />

• electron ionization with selected ion monitoring may<br />

not be the most sensitive method for detection<br />

(negative ion electrospray ionization mass<br />

spectrometry may be better)<br />

• the metabolism of chlorpyrifos was not inhibited by<br />

the presence of diazinon under test conditions and<br />

concentrations<br />

• further studies will be needed at lower concentrations<br />

to verify lack of inhibition.<br />

Publication and Presentation<br />

Campbell, JA, TS Poet, GM Mong, and C. Timchalk.<br />

June 2000. “In vitro metabolism study with a mixture of<br />

the organophosphate insecticides chlorpyrifos and<br />

diazinon.” Presented at the 48 th ASMS Conference on<br />

Mass Spectrometry and Allied Topics, Long Beach,<br />

California. In Proceedings of 48 th ASMS Conference on<br />

Mass Spectrometry and Allied Topics (in press).<br />

Analytical and Physical Chemistry 5

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