Abstract
The objective of this work was to combine the advantages of the dried blood spot (DBS) sampling process with the highly sensitive and selective negative-ion chemical ionization tandem mass spectrometry (NICI-MS-MS) to analyze for recent antidepressants including fluoxetine, norfluoxetine, reboxetine, and paroxetine from micro whole blood samples (i.e., 10 μL). Before analysis, DBS samples were punched out, and antidepressants were simultaneously extracted and derivatized in a single step by use of pentafluoropropionic acid anhydride and 0.02% triethylamine in butyl chloride for 30 min at 60 °C under ultrasonication. Derivatives were then separated on a gas chromatograph coupled with a triple-quadrupole mass spectrometer operating in negative selected reaction monitoring mode for a total run time of 5 min. To establish the validity of the method, trueness, precision, and selectivity were determined on the basis of the guidelines of the “Société Française des Sciences et des Techniques Pharmaceutiques” (SFSTP). The assay was found to be linear in the concentration ranges 1 to 500 ng mL−1 for fluoxetine and norfluoxetine and 20 to 500 ng mL−1 for reboxetine and paroxetine. Despite the small sampling volume, the limit of detection was estimated at 20 pg mL−1 for all the analytes. The stability of DBS was also evaluated at −20 °C, 4 °C, 25 °C, and 40 °C for up to 30 days. Furthermore, the method was successfully applied to a pharmacokinetic investigation performed on a healthy volunteer after oral administration of a single 40-mg dose of fluoxetine. Thus, this validated DBS method combines an extractive—derivative single step with a fast and sensitive GC-NICI-MS-MS technique. Using microliter blood samples, this procedure offers a patient-friendly tool in many biomedical fields such as checking treatment adherence, therapeutic drug monitoring, toxicological analyses, or pharmacokinetic studies.
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References
Kent JM (2000) Lancet 355:911–918
Wille SMR, Maudens KE, Van Peteghem CH, Lambert WEE (2005) J Chromatogr A 1098:19–29
Azaz-Lishits T, Hershko A, Ben-Chetrit E (2002) Pharmacopsychiatry 35:112–115
Adson DE, Erickson-Birkedahl S, Kotlyar M (2001) Ann Pharmacother 35:1375–1377
Kelly CA, Laing WJ, Strachan FE, Good AM, Bateman DN (2004) J Toxicol Clin Toxicol 42:67–71
Vaswani M, Linda FK, Ramesh S (2003) Prog Neuropsychopharmacol Biol Psychiatry 27:85–102
Mandrioli R, Forti GC, Raggi MA (2006) Curr Drug Metab 7:127–133
ter Heine R, Rosing H, van Gorp ECM, Mulder JW, van der Steeg WA, Beijnen JH, Huitema ADR (2008) J Chromatogr B 867:205–212
Damen CWN, Rosing H, Schellens JHM, Beijnen JH (2009) Anal Bioanal Chem 394:1171–1182
Boy RG, Henseler J, Mattern R, Skopp G (2008) Ther Drug Monit 30:733–739
Zytkovicz TH, Fitzgerlad EF, Marsden D, Larson CA, Shih VE, Johnson DM, Strauss AW, Comeau AM, Eaton RB, Grady GF (2001) Clin Chem 47:1945–1955
Mcdade TW, Williams S, Snodgrass JJ (2007) Demography 44:899–925
Mei JV, Alexander JR, Adam BW, Hannon WH (2001) J Nutr 131:1631–1636
Cheung CY, van der Heijden J, Hoogtanders K, Christiaans M, Liu YL, Chan YH, Choi KS, van de Plas A, Shek CC, Chau KF, Li CS, van Hooff J, Stolk L (2008) Transpl Int 21:140–145
Edelbroek PM, van der Heijden J, Stlok LML (2009) Ther Drug Monit 31:327–336
Barfield M, Spooner N, Lad R, Parry S, Fowles S (2008) J Chromatogr B 870:32–37
Blessborn D, Römsing S, Annerberg A, Sundquist D, Björkman A, Lindegardh N, Bergqvist Y (2007) J Pharm Biomed Anal 45:282–287
Mwaba P, Cassol S, Pilon R, Chintu C, Janes M, Nunn A, Zumla A (2003) Lancet 362:1459–1460
Koal T, Burhenne H, Römling R, Svoboda M, Resch K, Kaever V (2005) Rapid Commun Mass Spectrom 19:2995–3001
Guidelines for the shipment of dried blood spot specimens (1995) Center for Diseases Control and Prevention, Atlanta, GA, USA; http://www.cdc.gov/od/ohs/biosfty/driblood.htm. Accessed 20 December 2009
Lejeune D, Souletie I, Houzé S, Le Bricon T, Le bras J, Gourmel B, Houzé P (2007) J Pharm Biomed Anal 43:1106–1115
Ntale M, Mahindi M, Ogwal-Okeng JW, Gustafsson LL, Beck O (2007) J Chromatogr B 859:137–140
la Marca G, Malvagia S, Filippi L, Fiorini P, Innocenti M, Luceri F, Pieraccini G, Moneti G, Francese S, Dani FR, Guerrini R (2008) J Pharm Biomed Anal 48:1392–1396
Coombes EJ, Gamlen TR, Batstone GF, Leigh PN (1984) Ann Clin Biochem 21(Pt 6):519–522
AbuRuz S, Millership J, McElnay J (2006) J Chromatogr B 832:202–207
Fujimoto T, Tsuda Y, Tawa R, Hirose S (1989) Clin Chem 35:867–869
Allanson AL, Cotton MM, Tettey JNA, Boyter AC (2007) J Pharm Biomed Anal 44:963–969
van der Heijden J, de Beer Y, Hoogtanders K, Christiaans M, de Jong GJ, Neef C, Stolk L (2009) J Pharm Biomed Anal 50:664–670
Saint-Marcoux F, Sauvage FL, Marquet P (2007) Anal Bioanal Chem 388:1327–1349
Mauriala T, Chauret N, Oballa R, Nicoll-Griffith DA, Bateman KP (2005) Rapid Commun Mass Spectrom 19:1984–1992
Wille SMR, Van Hee P, Neels HM, Van Peteghem CH, Lambert WE (2007) J Chromatogr A 1176:236–245
Thomas A, Widmer C, Hopfgartner G, Staub C (2007) J Pharm Biomed Anal 45:495–503
Maurer HH (2002) Ther Drug Monit 24:247–254
Gunnar T, Ariniemi K, Lillsunde P (2006) J Mass Spectrom 41:741–754
Cirimele V, Kintz P, Ludes B (1997) J Chromatogr B 700:119–129
Kintz P, Tracqui A, Mangin P (1996) J Forensic Sci 41:851–854
Kuhlman JJ Jr, Magluilo J Jr, Cone E, Levine B (1996) J Anal Toxicol 20:229–235
Watson DG, Su Q, Midgley JM, Doyle E, Morton NS (1995) J Pharm Biomed Anal 13:27–32
Wilkins D, Haughey H, Cone E, Huestis M, Foltz R, Rollins D (1995) J Anal Toxicol 19:483–491
Boulanger B, Chiap P, Dewé W, Crommen J, Hubert P (2003) J Pharm Biomed Anal 32:753–765
Matuszewski BK, Constanzer ML, Chavez-Eng CM (2003) Anal Chem 75:3019–3030
Qu Y, Aluisio L, Lord B, Boggs J, Hoey K, Mazur C, Lovenberg T (2009) Pharmacol Biochem Behav 92:469–473
Vlase L, Imre S, Leucuta S (2005) Talanta 66:659–663
Hoogtanders K, van der Heijden J, Christiaans M, Edelbroek P, van Hooff JP, Stolk LML (2007) J Pharm Biomed Anal 44:658–664
Kulik W, van Lenthe H, Stet FS, Houtkooper RH, Kemp H, Stone JE, Steward CG, Wanders RJ, Vaz FM (2008) Clin Chem 54:371–378
Cramers CA, Leclercq PA (1999) J Chromatogr A 842:3–13
Mastovska K, Lehotay SJ (2003) J Chromatogr A 1000:153–180
Harrison AG (1986) Chemical ionization mass spectrometry. CRC Press, Boca Raton, Florida
Shah VP, Midha K, Dighe S, McGilveray LJ, Skelly JP, Yacobi A, Layloff T, Viswanathan CT, Cook CE, McDowall RD, Pittman KA, Spector S (1992) J Pharm Sci 81:309–312
Hubert P, Chiap P, Crommen J, Boulanger B, Chapuzet E, Mercier N, Bervoas-Martin S, Chevalier P, Grandjean D, Lagorce P, Lallier M, Laparra MC, Laurentie M, Nivet JC (1999) Anal Chim Acta 391:135–148
Hubert P, Nguyen-Huu JJ, Boulanger B, Chapuzet E, Chiap P, Cohen N, Compagnon NA, Dewé W, Feinberg M, Lallier M, Laurentie M, Mercier N, Muzard G, Nivet C, Valat L (2004) J Pharm Biomed Anal 36:579–586
Keller T, Cambon N, Genevray M, Crivelli F, Crivelli M, Dal BL, Mazzuchelli P, Ismaili S, Marzo A (2005) Arzneimittelforschung 55:491–497
Najib NM, Idkaidek N, Beshtawi M, Mohammed B, Admour I, Alam SM, Dham R, Qumaruzaman (2005) Biopharm Drug Dispos 26:243–247
Acknowledgments
The authors would like to thank Dr Youssef Daali from the Division of Clinical Pharmacology and Toxicology, Geneva University Hospitals (Switzerland) for his help.
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Déglon, J., Lauer, E., Thomas, A. et al. Use of the dried blood spot sampling process coupled with fast gas chromatography and negative-ion chemical ionization tandem mass spectrometry: application to fluoxetine, norfluoxetine, reboxetine, and paroxetine analysis. Anal Bioanal Chem 396, 2523–2532 (2010). https://doi.org/10.1007/s00216-009-3412-6
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DOI: https://doi.org/10.1007/s00216-009-3412-6