摘要:

A sensitive HPLC method for the quantification of rogletimide enantiomers in serum with UV detection was described. The method involves the use of a solid phase extraction of the R(+) and S (−) enantiomers of rogletimide and the internal standard S(−) amino glutethimide from serum using a C18 Bond-Elute column. Chromatographic resolution of the enantiomers was performed on a reversed phase cellulose-based chiral column (Chiralcel OJ-R) under isocratic conditions using a mobile phase consisting of 80:20 v/v 0.25 M aqueous sodium perchlorate-acetonitrile (pH 5.6 adjusted with perchloric acid) at a flow rate of 0.5 mL/min. Recoveries for R (+) and S (−) rogletimide enantiomers were in the ranges of 84–89% at 200 – 1000 ng/mL level. Intra-day and inter-day precision calculated as % RSD were in the ranges of 3–4% and 1–5% for both Intra-day and inter-day accuracies calculated as % error were in the ranges of 2–4% and 1.5–4% for both enantiomers, respectively. Linear calibration curves were in the concentration ranges of 100–1500 ng/mL for each enantiomer in serum. The limit of quantification of each enantiomer was 100 ng/mL. The detection limit for each enantiomer in serum using a UV detection set at 257 nm was 50 ng/mL (S/N=2).

ISSN:1082-6076    

DOI:10.1081/JLC-100101489

出版商:Taylor & Francis Group    

年代:2000

数据来源: Taylor

摘要:

A capillary electrophoresis (CE) method for the quantitative determination of R(+) and S(−) rogletimide in serum was developed. Stereoselective resolution of the rogletimide enantiomers was achieved using 60 mM alpha-cyclodextrin (α-CD) in 10 mM sodium dihydrogen phosphate/5 mM sodium tetraborate buffer of pH 2.5. A 72 cm uncoated fused-silica capillary at a constant voltage 15kV was used for the analysis and 0.03 mM hexadecyltrimethyl ammonium bromide (HTAB) was added to the buffer to decrease the adsorption of endogenous substances onto the silica wall. The analytes of interest were extracted from serum using a solid phase extraction (SPE) procedure. An octadecyl cartridge gave good recoveries in excess of 85% for both R(+) and S(−) rogletimide without any interference.

ISSN:1082-6076    

DOI:10.1081/JLC-100101490

出版商:Taylor & Francis Group    

年代:2000

数据来源: Taylor