• Aucun résultat trouvé

IIIIV V V V ANALYSE RMN ANALYSE RMN ANALYSE RMN ANALYSE RMN

A. RMN 1 H (1D) température de la sonde : 25° C.

- largeur spectrale: 10000 Hz. - taille du FID: 32K. - taille du spectre: 64K. - durée de l’impulsion: 8 µs. - angle de basculement : ≈90°. - délai entre les impulsions: 3 s.

- temps d’acquisition : 4.6 s. - nombre d’accumulations: 128. E. RMN 2D (DOSY)

- séquence utilisée pour les formulations solides : Echo de spin stimulé avec gradients bipolaires (stebpgp1s). Une séquence d’impulsion 3-9-19 avec des gradients de 9.25 G.cm-1 a été ajoutée pour la suppression du signal de l'eau pour les formulations liquides de FLX.

- température de la sonde : 25° pour les formulations solides et 32° pour les formulations liquides.

- largeur spectrale: 10000 Hz (F2) - taille du FID: 32768 (F2) * 40 (F1). - taille du spectre: 2048 (F2)

- délai entre les impulsions: 2 s. - nombre d’accumulations: 64.

- durée de l’impulsion 90° P1 : 8.25 µs.

- durée de l’impulsion P2 : 16.50 µs

- délai de diffusion D20 (∆) : 0.08-0.12 s.

- durée du gradient P30 ou δ/2 : 1000-1700 µs.

Partie Expérimentale du Chapitre 2.

- étendue du gradient : 5 % à 95 %. - nombre de points (expériences) : 40.

-échantillonnage du gradient : linéaire.

-intensité maximale du gradient : 46.25 G.cm-1.

Les paramètres de la séquence ont été adaptés afin d'avoir l'intensité du signal de FLX (H4,6)

ou de FLV (H3,4,6,7) fortement diminuée (au moins divisée par 50) à 95% de l’intensité maximale

du gradient. Les données spectrales sont traitées avec le logiciel de RMN Gifa5© commercialisé

par la société NMRtec (Montpellier, France). Ce logiciel propose un module spécifique de traitement des expériences DOSY basé sur la transformée inverse de Laplace.

- nombre de points : 2048. - itération MaxEnt : 20 000. - nombre de colonnes : 32.

Bibliographie du Chapitre 2.

Bibliographie

Bibliographie

Bibliographie

Bibliographie

Bibliographie du Chapitre 2.

1. Berzas J, Guiberteau C, Contento AM, Rodriguez V: Sensitive and rapide high- performance liquid chromatographic method for simultaneous determination of antidepressants in pharmaceutical formulations. Chromatographia 2002, 56:545-551. 2. Raggi MA, Bugamelli F, Casamenti G, Mandrioli R, Ronchi DD, Volterra V: Analytical

methods for the quality control of Prozac capsules. Journal of Pharmaceutical and

Biomedicale Analysis 1998, 18 699.

3. Ertürk S, Cetil SM, Atmaca S, Ersoy L, Baktir G: A sensitive HPLC methode for the determination of Fluoxetine and Nor fluoxetine in human plasma with fluorescence detection. Therapeutic Drug Monitoring 2005, 27:38-43.

4. Sarracíno MA, Mercolini L, Flotta G, Albers LJ, Merli R, Raggi MA: Simultaneous determination of fluvoxamine ismers and quetiapine in human plasma by means of high-performance liquid chromatography. Journal of Chromatography B 2006, 843 227-233.

5. Shinozuka T, Terada M, Tanaka E: Solid-phase extraction and analysis of 20 antidepressant drugs in human plasma by LC/MS with SSI methode. Forensic

Science International 2006 162 108-112.

6. Kirchherr H, Kühn-Velten WN: Quantitative determination of forty-eight antidepressants and antipsychotics in human serum by HPLC tandem mass spectroscopy: A multi-level, single-sample approach. Journal of Chromatography B 2006, 843:100-113.

7. Fernández C, Neto AJdS, Rodrigues JC, Alves C, Lanças FM: Solid-phase microextraction-liquid chromatography (SPME-LC) determination of fluoxetine and norfluoxetine in plasma using a heated liquid flow through interface. Journal of

Chromatography B 2007, 847 217-223.

8. Ulu ST: HPLC method for the determination of fluvoxamine in human plasma and urine for application to pharmacokinetic studies. Journal of Pharmaceutical and

Biomedicale Analysis 2007, 43 1444-1451.

9. Nevado JJB, Llerena MJV, Cabanillas CG, Robledo VR, Buitrago S: Sensitive capillary GS-MS-SIM determination of selective serotonin reuptake inhibitors: reliability evalution by validation and robustness study. Journal of Separation Science 2006, 29:103-113.

10. Nevado JJB, Llerena MJV, Cabanillas CG, Robledo VR: Screening of citalopram, fluoxetine and their metabolites in human urine samples by gas chromatography- mass spectrometry Aglobal robustness/ruggedness. Journal of Chromatography A 2006, 1123:130-133.

11. Salgado-Petinal C, Lamas JP, Garcia-Jares C, Llompart M, Cela R: Rapid screening of selective serotonin re-uptake inhibitors in urine samples using solid-phase microextraction gas chromatography-mass spectrometry. Analytical and Bioanalytical Chemistry 2005, 382 1351-1359.

12. Nevado JJB, Llerena MJV, Salcedo AMC, Nuevo EA: Assay validation for three antidepressants in pharmaceutical formulations: Practical approach using capillary gas chromatography. Journal of Pharmaceutical and Biomedicale Analysis 2005, 38:52- 59.

13. Flores JR, Nevado JJB, Salced AMC, Diaz MPC: Development of a Capillary Zone Electrophoretic method to determine six antidepressants in their pharmaceutical preparations. Experimental design for evaluating the ruggedness of method. Journal

of Separation Science 2004, 27 33-40.

14. Flores JR, Nevado JJB, Peñalvo GC, Diez NM: Development and validation method for determination of fluoxetine and its main metabolite norfluoxetine by nonaqueous capillary electrophoresis in human urine. Talanta 2005 65 163-171.

15. Afkhami A, Madrakian T, Khalafi L: Spectrophotometric determination of fluoxetine by batch and flow injection methods. CHEMICAL AND PHARMACEUTICAL

BULLETIN 2006 54 1642-1646.

16. Martino R, Gilard V, Desmoulin F, Malet-Martino M: Fluorine- 19 or phosphorus-31 NMR spectroscopy: Asuitable analytical technique for quantitative in vitro studies of fluorinated or phosphorylated drugs. Journal of Pharmaceutical and Biomedicale

Analysis 2005, 38:871-891.

17. Shamsipur M, Shafiee-Dastgerdi L, Talebpour Z, Haghgood S: 19F NMR as a powerful technique for the assay of anti-psychotic drug haloperidol in human serum and pharmaceutical formulations. Journal of Pharmaceutical and Biomedicale Analysis 2007, 43:1116-1121.

18. Trefi S, Gilard V, Malet-Martino M, Martino R: Generic ciprofloxacin tablets contain the stated amount of drug but have different impurity profiles: a 19F, 1H and DOSY NMR analysis. Journal of Pharmaceutical and Biomedicale Analysis 2007, 44 743-754. 19. Musshoff F, Padosch S, Steinborn S, Madea B: Fatal blood and tissue concentrations of

more than 200 drugs. Forensic Science International 2004, 142 161-210.

20. Prozac. In United States S Pharmacopeia. Volume 7th Supplement. 23rd edition. Edited by Convention USP. Rockville, MD 1997: 3890-3891

21. Nevado JJB, Llerena MJV, Salcedo AMC, Nuevo EA: Determination of fluoxetine, fluvoxamine and clomipramine in pharmaceutical formulations by capillary gas chromatography. Journal of Chromatographic Science 2000, 38 200-206.

Bibliographie du Chapitre 2.

22. Berzas JJ, Guiberteau C, Villaseñor MJ, Rodríguez V: Development of a capillary gas chromatographic procedure. Analitica Chimica Acta 2004, 519:219-230.

23. Nevado JJB, Salcedo AMC, Llerena MJV, E. Aguas Nuevo: Method developement and validation for the simultaneous determination of fluoxetine and fluvoxamine in pharmaceutical preparations by capillary electrophoresis. Analytica Chimica Acta 2000, 417:169-176.

24. Mandrioli R, Pucci V, Visini D, Varani G, Raggi MA: Rapidmethods for determination of fluoxetine in pharmaceutical formulations. Journal of Pharmaceutical and

Biomedicale Analysis 2002, 29 1127-1134.

25. Prabhakar AH, Patel VB, Giridhar R: Spectrophotometric determination of fluoxetine hydrochloride in bulk and in pharmaceutical formulations. Journal of

Pharmaceutical and Biomedicale Analysis 1999, 20 427-432.

26. Starczewska B, Jasinska A, Bialous B: Study and analytical application of ion-pair formation in the system fluoxetine-pyrocatechol violet and fluvoxamine- pyrocatechol violet. Pharmazie 2003, 58 245-248.

27. Buzinkaiova T, Polonsky J: Determination of four selective serotonin reuptake inhibitors by capillary isotachophoresis. Electrophoresis 2000, 21 2839-2841.

28. Nouws HPA, Delerue-Matos C, Barros AA, Rodrigues JA, Santos-Silva A: Electroanalytical study of fluvoxamine. Analytical and Bioanalytical Chemistry 2005, 382 1662-1668.

29. Deubner R, Holzgrabe U: Quantitative 1H NMR spectroscopic determination of the E/Z isomer ratio of the antidepressant drug fluvoxamine for use in pharmaceutical analysis Magnetic Resonanc in Chemistry 2002, 40:762-766.

30. Ali SM, Asmat F, Maheshwari A, Koketsu M: Complexation of fluoxetine hydrochloride with ββ-cyclodextrin. A proton magnetic resonance study in aqueous ββ solution. Il Farmaco 2005, 60:445-449.

31. Fux P: Determination of trace amounts of polydimethylsiloxane in extracts of chemicals by proton nuclear magnetic resonance spectroscopy. Analyst 1990, 115:179-183.

32. Forget R, Spagnoli S: Excipient quantitation and drug distribution during formulation optimization. Journal of Pharmaceutical and Biomedicale Analysis 2006, 41:1051-1055.

33. Guerrero-Martínez A, Palafox MA, Tardajos G: Unexpected binding mode of gemini surfactants and γ-cyclodextrin: DOSY as a tool for the study of complexation.

Documents relatifs