| Popis: |
Twenty g sample, to which sulfamerazine has been added as internal standard, is extracted with 0.3N HC1 + 1.5% diethylamine in 25% methanol. The sample extract is chilled (to aid clarification), centrifuged, and filtered. The sulfonamides are separated from each other and from co-extracted materials on a C-18 reverse-phase column and detected at 450 nm following post-column derivatization with dimethylaminobenzaldehyde. Two isocratic mobile phases have been tested: (1) acetonitrile-2% acetic acid (17 + 83), with an analysis time of 13 min; and (2) acetonitrile-methanol-2% acetic acid (4 + 16 + 80), with an analysis time of 20 min but an improved analysis for some samples. As many as 40 samples have been analyzed at one time unattended with the aid of an autosampler. A total of about 1500 field samples have been assayed using the method. Method sensitivity is 0.1 ppm for either analyte in a hog finishing feed. Linearity for each of the analytes is satisfactory over a range of 0.4-25 ppm in spiked feeds. Coefficients of variation range from 13% at 0.5 ppm to 2% at 13 ppm as tested over a period of time in naturally contaminated samples. The absolute recovery of sulfamethazine varies with sample matrix, but, in the presence of sulfamerazine as internal standard, recovery has been 96.7-99.7% over the range of 0.1-10 ppm. Sulfamerazine and sulfamoxole were tested for their suitability as internal standards. Sulfamerazine is a good internal standard for sulfamethazine; neither is ideal for sulfathiazole. A recovery factor is necessary for estimating the level of sulfathiazole in feeds when either internal standard is used; however, either standard is satisfactory for correcting for feed matrix variation |
