[en] A Surface Enhanced Raman Scattering (SERS) method able to quantify 4-aminophenol in a pharmaceutical formulation based on acetaminophen, also called paracetamol, was developed and, for the first time, successfully validated. In this context, silver nanoparticles were synthesized according to the method described by Lee-Meisel and used as SERS substrate. The repeatability of the silver colloid synthesis was tested using different methods to characterise the size and the zeta potential of silver nanoparticles freshly synthesized. To optimize the SERS samples preparation, a design of experiments implicating concentrations of citrate-reduced silver nanoparticles and aggregating agent was performed in order to maximize the Raman signal enhancement. Finally, an approach based on tolerance intervals and accuracy profiles was applied in order to thoroughly validate the method in a range of concentrations comprised from 3 to 15 µg mL-1 using normalized band intensities. The standard addition method was selected as method calibration. Therefore, measurements were carried out on 4-aminophenol spiked solutions of the pharmaceutical formulation. Despite the well-known stability and reproducibility problems of SERS, the validation was performed using two operators and 5 batches of nanoparticles, one for each validation day.
Research center :
Centre Interfacultaire de Recherche du Médicament - CIRM
Disciplines :
Pharmacy, pharmacology & toxicology
Author, co-author :
De Bleye, Charlotte ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Dumont, Elodie ; Université de Liège - ULiège > 1re an. master sc. pharma., à finalité
Rozet, Eric ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Sacre, Pierre-Yves ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Chavez, Pierre-François ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Netchacovitch, Lauranne ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Piel, Géraldine ; Université de Liège - ULiège > Département de pharmacie > Pharmacie galénique
Hubert, Philippe ; Université de Liège - ULiège > Département de pharmacie > Chimie analytique
Ziemons, Eric ; Université de Liège - ULiège > Département de pharmacie > Département de pharmacie
Language :
English
Title :
Determination of 4-aminophenol in a pharmaceutical formulation using Surface Enhanced Raman scattering: from development to method validation
Publication date :
15 November 2013
Journal title :
Talanta
ISSN :
0039-9140
eISSN :
1873-3573
Publisher :
Elsevier Science, Amsterdam, Netherlands
Volume :
116
Pages :
899-905
Peer reviewed :
Peer Reviewed verified by ORBi
Funders :
F.R.S.-FNRS - Fonds de la Recherche Scientifique [BE]
S. Armenta, S. Garrigues, and M. De la Guardia Trends Anal. Chem. 27 2008 497 511
J. Morros, S. Garrigues, and M. De la Guardia Trends Anal. Chem. 29 2010 578 591
P. Prajapati, and A. Prajapati Int. J. Pharm. Sci. Rev. Res. 9 2011 57 64
S. Mazurek, and R. Szostak J. Pharm. Biomed. Anal. 49 2009 168 172
D. Skorda, and C.G. Kontoyannis Talanta 74 2008 1066 1070
M. Lopez-Sanchez, M.J. Ruedas-Rama, A. Ruiz-Medina, A. Molina-Diaz, and M.J. Ayora-Canada Talanta 74 2008 1603 1607
S. Mazurek, and R. Szostak J. Pharm. Biomed. Anal. 40 2006 1225 1230
S. Mazurek, and R. Szostak J. Pharm. Biomed. Anal. 40 2006 1235 1242
S. Mazurek, and R. Szostak J. Pharm. Biomed. Anal. 48 2008 814 821
M.G. Orkoula, C.G. Kontoyannis, C.K. Markopoulou, and J.E. Koundourellis J. Pharm. Biomed. Anal. 41 2006 1406 1411
C. De Bleye, P.-F. Chavez, J. Mantanus, R. Marini, Ph Hubert, E. Rozet, and E. Ziemons J. Pharm. Biomed. Anal. 2012 125 132
International Conference on Harmonisation (ICH) of Technical Requirements for Registration of Pharmaceuticals for Humans Use, Topic Q2 (R1), Validation of Analytical Procedures: Text and Methodology, Geneva, 2005.
K. Kneipp, H. Kneipp, I. Itzkan, R.R. Dasari, and M.S. Feld Chem. Rev. 99 1999 2957 2975
M. Fleischmann, P.J. Hendra, and A.J. McQuillan Chem. Phys. Lett. 26 1974 163 166
A. Stewart, and S.E.J. Bell Chem. Commun. 47 2011 4523 4525
C. Ruan, W. Wang, and B. Gu Anal. Chim. Acta 567 2006 114 120
Y. Chen, L. Wu, Y. Chen, N. Bi, X. Zheng, H. Qi, M. Qin, X. Liao, H. Zhang, and Y. Tian Microchim. Acta 177 2012 341 348
D. Tsoutsi, J.M. Montenegro, F. Dommershausen, U. Koert, L.M. Liz-Marzan, W.J. Parak, and R.A. Alvarez-Puebla ACS Nano 5 2011 7539 7546
J. Zhang, S. Qu, L. Zhang, A. Tang, and Z. Wang Spectrochim. Acta Part A 79 2011 625 630
P. Hubert, J.J. Nguyen-Huu, B. Boulanger, E. Chapuzet, P. Chiap, N. Cohen, P.A. Compagnon, W. Dewe, M. Feinberg, M. Lallier, M. Laurentie, N. Mercier, G. Muzard, C. Nivet, and L. Valat J. Pharm. Biomed. Anal. 36 2004 579 586
B. Boulanger, E. Rozet, F. Moonen, S. Rudaz, and Ph. Hubert J. Chromatogr. B 877 2009 2235 2243
E. Rozet, R.D. Marini, E. Ziemons, B. Boulanger, and Ph. Hubert J. Pharm. Biomed. Anal. 55 2011 848 858
E. Rozet, V. Wascotte, N. Lecouturier, V. Préat, W. Dewé, B. Boulanger, and Ph. Hubert Anal. Chim. Acta 591 2007 239 247
P.C. Lee, and D. Meisel J. Phys. Chem. 86 1982 3391 3395
N. Leopold, and B. Lendl J. Phys. Chem. B 107 2003 5723 5727
E.C. Le Ru, and P.G. Etchgoin Principles of Surface-Enhanced Raman Spectroscopy and Related Plasmonic Effects 2009 Elsevier Amsterdam
M. Moskovits J. Raman Sprectrosc. 36 2005 485 496
C.H. Munro, W.E. Smith, M. Garner, J. Clarkson, and P.C. White Langmuir 11 1995 3712 3720
R.F. Aroca, R.A. Alvarez-Puebla, N. Pieczonka, S. Sanchez-Cortez, and J.V. Garcia-Ramos Adv. Colloid Interface Sci. 116 2005 45 61
S.E.J. Bell, and N.M.S. Sirimuthu J. Phys. Chem. A 109 2005 7405 7410
R.M. Liu, Y.P. Kang, X.F. Zi, M.J. Feng, M. Cheng, and M.Z.Zhen Si Chin. Chem. Lett. 20 2009 711 715
S. Sanchez-Cortes, and J.V. Garcia-Ramos J. Raman Spectrosc. 29 1998 365 371