期刊
CHROMATOGRAPHIA
卷 86, 期 1, 页码 87-95出版社
SPRINGER HEIDELBERG
DOI: 10.1007/s10337-022-04229-w
关键词
Ketamine; Capillary electrophoresis; Design of experiments; Cyclodextrins; Enantiomers
Capillary electrophoresis was used to separate ketamine enantiomers, and the method was optimized by screening and choosing the most suitable conditions. The developed method showed good accuracy and linearity in quantification.
Capillary electrophoresis was chosen as cost-effective and robust method to separate ketamine enantiomers. For the method development, first different native and modified cyclodextrins were tested. The most promising chiral selector was alpha-cyclodextr in. A design of experiments (DoE) was carried out, which started with the screening of relevant factors. Based on these results, the method was optimized according to the significant factors (buffer, cyclodextrin concentration, pH value, voltage, temperature) of the screening based on the response resolution and migration time of the later migrating enantiomer. The optimized conditions consisted of a background electrolyte with 275 mM TRIS, adjusted with 85% phosphoric acid to a pH of 2.50, and 50 mM alpha-cyclodextr in, at a temperature of 15 degrees C, an applied voltage of 30 kV and an injection pressure of 1.0 psi for 10 s. A fused-silica capillary with a total length of 70 cm and an effective length to the detector of 60 cm was used. The method was validated according to ICH guideline Q2 R(1). The limit of quantification was 3.51 mu g mL-1 for S-ketamine and 3.98 mu g mL(-1 )for R-ketamine. The method showed good linearity for racemic ketamine with R2 of 0.9995 for S-ketamine and 0.9994 for R-ketamine. The lowest quantifiable content of S-ketamine found in R-ketamine was 0.45%.
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