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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

Authorized Users Only
2008
Authors
Živanović, Ljiljana
Licanski, A.
Zečević, Mira
Jocić, Biljana
Kostić, Mirjana
Article (Published version)
Metadata
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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 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.

Keywords:
solid phase extraction / fractional factorial designs / central composite design / mycophenolic acid / mycophenolic acid glucuronide / method validation
Source:
Journal of Pharmaceutical and Biomedical Analysis, 2008, 47, 3, 575-585
Publisher:
  • Elsevier Science BV, Amsterdam
Projects:
  • Sinteza, kvantitativni odnosi između strukture/osobina i aktivnosti, fizičko-hemijska karakterizacija i analiza farmakološki aktivnih supstanci (RS-142071)

DOI: 10.1016/j.jpba.2008.01.046

ISSN: 0731-7085

PubMed: 18356001

WoS: 000256780600017

Scopus: 2-s2.0-44149115973
[ Google Scholar ]
26
23
URI
http://farfar.pharmacy.bg.ac.rs/handle/123456789/1089
Collections
  • Radovi istraživača / Researchers’ publications
Institution
Pharmacy
TY  - JOUR
AU  - Živanović, Ljiljana
AU  - Licanski, A.
AU  - Zečević, Mira
AU  - Jocić, Biljana
AU  - Kostić, Mirjana
PY  - 2008
UR  - http://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",
url = "http://farfar.pharmacy.bg.ac.rs/handle/123456789/1089",
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. 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. Journal of Pharmaceutical and Biomedical Analysis. 2008;47(3):575-585
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.
Journal of Pharmaceutical and Biomedical AnalysisElsevier Science BV, Amsterdam., 47(3), 575-585.
https://doi.org/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" 47, no. 3 (2008):575-585,
https://doi.org/10.1016/j.jpba.2008.01.046 .

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