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Cromatography Handbook of HPLC - Rizzi A.

Rizzi A. Cromatography Handbook of HPLC - John Wiley & Sons, 2005. - 14 p.
Download (direct link): chromatographyhandbook2005.pdf
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HP LC of Drugs in Biologic ;al Samples 665
-* 263 r im <--- 247 nm--- 230 nm
spiked serum ------> 263 nm

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Figi jre 27 Time (min)
ng nL-1 Typical chromatograms of blank and spiked human serum (0.5 mL) fortified with 30
f each analyte and 125 ng internal standard (spironolactone). (From Ref. 68.)
26, were extracted from 0.5-mL--- serum samples, using methylsilane SPE cartridges. Spiro
nolactone (5 /xg mL-1) was added as internal standard. The analytes were eluted from the C,
SPE cartridge using 45% aqueous acetonitrile at low vacuum. The eluate was reduced to low
volume with a nitrogen stream and 50-jjlL injected into the HPLC. Separation of the drugs
was performed on a 22-cm x 4.6-mm-id silica column using 86:15 v/v 0.1-M phosphate
buffer pH 2.5-acetonitrile at a flow rate of 1 mL min-1 and 60C column temperature (Fig.
27). The LOQs were 5 ng mL-1 for all analytes, except stanozolol (10 ng mL-1)- The LODs
were 3 ng mL1 for all drugs except stanozolol (7 ng mL-1). Linearity was in the 0 to 1000-
ng mL-1 range, with good accuracy (96-103%) and precision (RSD 2.8-10.9%).
666
Stewart
LXII. TETRACYCLINE, CHLORTETRACYCLINE AND OXYTETRACYCLINE
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