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
Samo za registrovane korisnike
2008
Članak u časopisu (Objavljena verzija)
Metapodaci
Prikaz svih podataka o dokumentuApstrakt
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 elut...ion 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.
Ključne reči:
solid phase extraction / fractional factorial designs / central composite design / mycophenolic acid / mycophenolic acid glucuronide / method validationIzvor:
Journal of Pharmaceutical and Biomedical Analysis, 2008, 47, 3, 575-585Izdavač:
- Elsevier Science BV, Amsterdam
Finansiranje / projekti:
- Sinteza, kvantitativni odnosi između strukture/osobina i aktivnosti, fizičko-hemijska karakterizacija i analiza farmakološki aktivnih supstanci (RS-MESTD-MPN2006-2010-142071)
DOI: 10.1016/j.jpba.2008.01.046
ISSN: 0731-7085
PubMed: 18356001
WoS: 000256780600017
Scopus: 2-s2.0-44149115973
Institucija/grupa
PharmacyTY - JOUR AU - Živanović, Ljiljana AU - Licanski, A. AU - Zečević, Mira AU - Jocić, Biljana AU - Kostić, Mirjana PY - 2008 UR - https://farfar.pharmacy.bg.ac.rs/handle/123456789/1089 AB - 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. PB - Elsevier Science BV, Amsterdam T2 - Journal of Pharmaceutical and Biomedical Analysis T1 - 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 VL - 47 IS - 3 SP - 575 EP - 585 DO - 10.1016/j.jpba.2008.01.046 ER -
@article{ author = "Živanović, Ljiljana and Licanski, A. and Zečević, Mira and Jocić, Biljana and Kostić, Mirjana", year = "2008", abstract = "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.", publisher = "Elsevier Science BV, Amsterdam", journal = "Journal of Pharmaceutical and Biomedical Analysis", title = "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", volume = "47", number = "3", pages = "575-585", doi = "10.1016/j.jpba.2008.01.046" }
Živanović, L., Licanski, A., Zečević, M., Jocić, B.,& Kostić, M.. (2008). 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. in Journal of Pharmaceutical and Biomedical Analysis Elsevier Science BV, Amsterdam., 47(3), 575-585. https://doi.org/10.1016/j.jpba.2008.01.046
Živanović L, Licanski A, Zečević M, Jocić B, Kostić M. 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. in Journal of Pharmaceutical and Biomedical Analysis. 2008;47(3):575-585. doi:10.1016/j.jpba.2008.01.046 .
Živanović, Ljiljana, Licanski, A., Zečević, Mira, Jocić, Biljana, Kostić, Mirjana, "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" in Journal of Pharmaceutical and Biomedical Analysis, 47, no. 3 (2008):575-585, https://doi.org/10.1016/j.jpba.2008.01.046 . .