ISSN:
1612-1112
Schlagwort(e):
Column liquid chromatography
;
Ketorolac in plasma
;
Enantiomer separation
;
Pharmacokinetic studies
Quelle:
Springer Online Journal Archives 1860-2000
Thema:
Chemie und Pharmazie
Notizen:
Summary A direct HPLC method for quantification of the (R) and (S) enantiomers of ketorolac in human plasma for pharmacokinetics studies has been developed. Naproxen sodium [S(+) enantiomer] was used as an internal standard. Plasma samples (1 mL) were vortexed for 30 sec with methyltert-butyl ether, followed by centrifugation at 2000 g for 8 min. The aqueous phase was acidified (pH 1) by adding 1 mL of 2N HCl and back-extracted with 5 mL methyltert-butyl ether. The organic phase was evaporated, and the residue was dissolved in 200 μL of mobile phase. 25 μL were chromatographed on a α1-acid glycoprotein column (Chiral-AGP, 100×4 mm I.D.), using a mobile phase with 8.5% propan-2-ol in phosphate buffer (0.09M NaH2PO4.H2O, 0.01M Na2HPO4, 0.002M Dimethyloctylamine; pH 5.5). Calibration range was 20–20000 ng mL−1 for (R)- and (S)-ketorolac. The LOQ was 5 ng mL−1 for both enantiomers. The sensitivity could be extended to 1 ng mL−1 with the same precison by increasing the injection volume to 100 μL. The method is reproducible, accurate, and stereospecific. The inter-assay and intra-assay CVs were 〈11.40% and 〈9.30% for (R)- and (S)-ketorolac respectively. Under the conditions employed, no racemization was observed.
Materialart:
Digitale Medien
URL:
http://dx.doi.org/10.1007/BF02467672
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