Application of experimental design in optimization of solid phase extraction of mycophenolic acid and mycophenolic acid glucuronide from human urine and plasma and SPE-RP-HPLC method validation
| Autor: | Mirjana Kostic, Ana Licanski, Biljana Jocić, Ljiljana Zivanovic, Mira Zečević |
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| Rok vydání: | 2008 |
| Předmět: |
Central composite design
Clinical Biochemistry Pharmaceutical Science 02 engineering and technology 01 natural sciences High-performance liquid chromatography Analytical Chemistry Glucuronides Drug Stability Drug Discovery Humans Solid phase extraction central composite design Chromatography High Pressure Liquid Spectroscopy Chromatography mycophenolic acid glucuronide Chemistry Elution fractional factorial designs Solid Phase Extraction 010401 analytical chemistry Extraction (chemistry) solid phase extraction method validation Fractional factorial design Reversed-phase chromatography Factorial experiment Mycophenolic Acid 021001 nanoscience & nanotechnology 6. Clean water 0104 chemical sciences Research Design 0210 nano-technology mycophenolic acid |
| Zdroj: | Journal of Pharmaceutical and Biomedical Analysis |
| ISSN: | 0731-7085 |
| DOI: | 10.1016/j.jpba.2008.01.046 |
| Popis: | The aim of this study was to develop and optimize a solid phase extraction (SPE) procedure for purification of mycophenolic acid (MPA) and its metabolite mycophenolic acid glucuronide (MPAG) in biological samples. During optimization process chemometric approach was applied. First, in screening experiments fractional factorial design (FFD) was used for selecting the variables which affected the extraction procedure. The ionic strength of the phosphate buffer in the washing step and the percentage of acetonitrile in the elution step were statistically significant for the recovery of MPAG while the percentage of acetonitrile and pH of the washing solution were statistically significant for that of MPA. Afterwards, the significant variables were optimized using central composite design (CCD). The developed SPE method included phosphate buffer (pH 2.4; 0.056 M) in the washing step, and the mixture of acetonitrile and phosphate buffer of which pH was adjusted to 2.4 (70:30, v/v) in the elution step. The investigation was applied to both urine and plasma and the nature of biological matrix appeared to be of no importance. The extraction from both matrixes showed good repeatability with relative standard deviations up to 6% for MPAG and 8% for MPA, and recovery around 100% for both substances. Furthermore, new SPE-RP-HPLC method for determination of MPA and MPAG in both humane urine and plasma has been validated. The great advantage of this method is the chromatographic run of only 3 min. |
| Databáze: | OpenAIRE |
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