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An HPLC assay for carbamazepine Phase I metabolites and their glucuronides in urine
Reith, D. M. and Cannell, G. R. (1999) An HPLC assay for carbamazepine Phase I metabolites and their glucuronides in urine. Journal of Liquid Chromatography and Related Technologies, 22 12: 1907-1918.
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| Author(s) |
Reith, D. M.
Cannell, G. R.
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| Title |
An HPLC assay for carbamazepine Phase I metabolites and their glucuronides in urine
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| Journal name |
Journal of Liquid Chromatography and Related Technologies
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| Publication date |
1999
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| Volume number |
22
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| Issue number |
12
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| ISSN |
1082-6076
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| Start page |
1907
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| End page |
1918
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| Total pages |
12
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| Place of publication |
New York
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| Publisher |
Marcel Dekker
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| Collection year |
1999
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| Language |
eng
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| Subject |
C1
320503 Clinical Pharmacology and Therapeutics
730104 Nervous system and disorders
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| Abstract |
A binary gradient HPLC assay was developed for the separation and quantitation of carbamazepine (CBZ), carbamazepine-epoxide (CBZ-ep), carbamazepine-10,11-transdiol (CBZ-diol), carbamazepine-2-hydroxide (CBZ-OH), carbamazepine-3-hydroxide (CBZ-3OH) and carbamazepine-acridan (CBZ-acr) extracted from patient urine. The internal standard was 10-methoxy-carbamazepine. The initial phase was 70:15:15 phosphate buffer-methanol-acetonitrile followed by a linear gradient commencing at 13 minutes to 50:35:15 phosphate buffer-methanol-acetonitrile at 24 minutes. The flow rate was constant at 2 mL/min. The UV absorbance detector wavelength was changed at 18 minutes from 240 nm to 280 nm. Typical retention times for CBZ-diol, CBZ-2OH, CBZ-ep, CBZ-3OH, CBZ-acr, CBZ and internal standard were 5.26, 8.36, 10.46, 12.51, 14.2, 23 and 27.53 minutes respectively. The minimum quantifiable limit (MQL) for all of the analytes was 0.2 mu g/mL except for CBZ-2OH where the MQL was 2 mu g/mL. Precision and accuracy of the assay was 1.3 to 19.4% for the 6 analytes. Liquid-liquid extraction with ethyl acetate resulted in recovery of the analytes from urine greater than 74% except for CBZ-diol where recovery was 40%. The concentrations of the glucuronides of CBZ and metabolites were calculated by measuring their concentrations before and after hydrolysis.
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| Keyword(s) |
Biochemical Research Methods
Chemistry, Analytical
Performance Liquid-chromatography
Plasma
Carbamazepine-10,11-epoxide
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