Simultaneous determination of doxifluridine and 5-fluorouracil in monkey serum by high performance liquid chromatography with tandem mass spectrometry
| Autor: | Young-Ah Woo, Eun Ju Jeong, Ghee-Hwan Kim, Choong-Yong Kim |
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| Rok vydání: | 2007 |
| Předmět: |
Male
Antimetabolites Antineoplastic Spectrometry Mass Electrospray Ionization Electrospray ionization Clinical Biochemistry Ethyl acetate Administration Oral Mass spectrometry Tandem mass spectrometry Biochemistry High-performance liquid chromatography Sensitivity and Specificity Analytical Chemistry chemistry.chemical_compound Drug Stability Tandem Mass Spectrometry Animals Active metabolite Chromatography High Pressure Liquid Chromatography Extraction (chemistry) Reproducibility of Results Isopropyl alcohol Cell Biology General Medicine Macaca fascicularis chemistry Linear Models Fluorouracil Floxuridine |
| Zdroj: | Journal of chromatography. B, Analytical technologies in the biomedical and life sciences. 875(2) |
| ISSN: | 1570-0232 |
| Popis: | A reverse-phase high performance liquid chromatography method with electrospray ionization and detection by mass spectrometry is described for the simultaneous determination of doxifluridine and its active metabolite 5-fluorouracil in monkey serum. A liquid/liquid extraction with ethyl acetate (90%) and isopropyl alcohol (10%) was used to extract simultaneously doxifluridine and 5-FU which have considerable difference in the polarity. Optimum chromatographic separation was achieved on a Agilent Zorbax C(18) (100 mm x 2.1mm, 3.5 microm) column with a mobile phase of methanol-water (20:80, v/v). The flow rate was 0.2 mL/min with total cycle time of 5 min. The lower limit of quantification (LLOQ) was validated at 10.0 ng/mL of serum for both doxifluridine and 5-FU. Accuracy and precision of quality control (QC) samples for both compounds met FDA Guidance criteria of +/-15% with average QC accuracy of 95.5-105.0% and coefficients of variation of 1.1-9.5% in the 10-2000 ng/mL concentration range. This method demonstrated adequate sensitivity, specificity, accuracy, precision, stability to support the analysis of monkey serum samples. |
| Databáze: | OpenAIRE |
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