Direct aqueous injection-liquid chromatography with post-column derivatization for determination of...

An interlaboratory method validation study was conducted on EPA Method 531.1, Measurement of N-Methylcarbamoyloximes and N-Methylcarbamates in Water by Direct Aqueous Injection HPLC with Post Column Derivatization, to determine the precision and mean recovery for determination of 10 carbamate pesticide compounds in reagent water and in finished drinking waters. The study design was based on Youden's nonreplicate plan for collaborative tests of analytical methods. The waters were spiked with 10 carbamate pesticides at 6 concentration levels, as 3 Youden pairs. Eight laboratories analyzed the samples by direct aqueous injection, with separation by reverse-phase liquid chromatography and post-column hydrolysis of the carbamates and carbamoyloximes to methylamine, followed by reaction of the methylamine with o-phthalaldehyde and 2-mercaptoethanol using fluorescence detection. Results were analyzed using an EPA computer program, which measured precision and recovery for each of the 10 compounds and compared the performance of the method between water types. The method was acceptable for all analytes tested. After removal of a nonrepresentative data set for aldicarb sulfoxide, no matrix effects were observed; the statistics for the pooled drinking waters were not significantly different from the statistics for the reagent waters. The method has been adopted official first action by AOAC.