title: Quantitative determination of fenoterol and fenoterol derivatives in rat plasma using on-line immunoextraction and liquid chromatography/mass spectrometry.
abstract: An on-line immunoextraction and liquid chromatography/mass spectrometry (LC/MS) method was developed and validated for the determination of R,R'-fenoterol, R,R'-methoxyfenoterol and R,S'-naphthylfenoterol in rat plasma. Sample preparation involved immunoextraction of analytes using an antibody raised against R,R'- and R,S'-aminofenoterol that was immobilized onto chromatographic support. LC was performed on a Waters hydrophilic interaction chromatography (HILIC) column (150 mm x 2.1mm), using an isocratic mobile phase of methanol:ammonium acetate (10mM, pH 6.8) (90:10, v/v) at a flow rate of 0.2 ml/min. The MS was operated in the single ion monitoring mode (m/z 304.2 for R,R'-fenoterol, m/z 318.1 for R,R'-methoxyfenoterol, and m/z 339.2 for R,S'-naphthylfenoterol). Optimization of analytes desorption process from the immunoextraction column was performed by factorial analysis and the sample calibration curves were made with spiked rat plasma samples containing 0.5-100 ng/ml of drugs. The cross-selectivity studies of the antibody were determined and the results suggested high selectivities toward R,R'-fenoterol, R,R'-methoxyfenoterol and R,S'-naphthylfenoterol. The accuracy of assay was more than 96% while intra- and inter-day precision of assay were less than 12.4%. Stability studies (2h benchtop, freeze/thaw, and autosampler stability) were conducted and the analytes were stable through out studies. The validated method was used to determine the plasma concentration-time profiles of drugs after oral administration to rats of R,R'-fenoterol, R,R'-methoxyfenoterol and R,S'-naphthylfenoterol.
authors.affiliation: Gerontology Research Center, National Institute on Aging, National Institutes of Health, Baltimore, MD 21224-6825, USA. kimhee@mail.nih.gov
authors.forename: Hee Seung
authors.initials: HS
authors.lastname: Kim
authors.forename: Danuta
authors.initials: D
authors.lastname: Siluk
authors.forename: Irving W
authors.initials: IW
authors.lastname: Wainer
mesh_terms: D000327:Adsorption; D000818:Animals; D000906:Antibodies / Q000276:immunology*; D002853:Chromatography, Liquid; D003429:Cross Reactions; D005280:Fenoterol / Q000031:analogs & derivatives* / Q000097:blood* / Q000737:chemistry; D008297:Male; D013058:Mass Spectrometry; D009862:Online Systems; D051381:Rats; D017207:Rats, Sprague-Dawley; D015203:Reproducibility of Results; D013997:Time Factors
chemical_list: D000906:Antibodies; C550094:methoxyfenoterol; D005280:Fenoterol
references.citation: Arzneimittelforschung. 1990 Aug;40(8):887-95
references.pmid: 2242081
references.citation: Analyst. 1994 Dec;119(12):2675-80
references.pmid: 7879874
references.citation: J Pharm Biomed Anal. 2002 Jun 20;29(1-2):147-52
references.pmid: 12062673
references.citation: J Chromatogr B Analyt Technol Biomed Life Sci. 2006 Jun 6;837(1-2):138-46
references.pmid: 16687257
references.citation: Chirality. 2006 Nov;18(10):822-7
references.pmid: 16917835
references.citation: J Pharm Biomed Anal. 1994 Sep;12(9):1069-74
references.pmid: 7803553
references.citation: J Comb Chem. 2004 Jan-Feb;6(1):78-82
references.pmid: 14714988
references.citation: J Chromatogr B Biomed Appl. 1996 Oct 25;685(2):265-72
references.pmid: 8953167
references.citation: Circulation. 2003 Sep 30;108(13):1633-9
references.pmid: 12975249
references.citation: Anal Chem. 1993 Jun 1;65(11):1622-30
references.pmid: 8328676
references.citation: J Mass Spectrom. 2003 Nov;38(11):1197-206
references.pmid: 14648827
references.citation: Anal Chem. 2004 Feb 1;76(3):805-13
references.pmid: 14750879
references.citation: J Chromatogr B Analyt Technol Biomed Life Sci. 2005 Feb 25;816(1-2):57-66
references.pmid: 15664334
references.citation: J Pharm Biomed Anal. 2008 Nov 4;48(3):960-4
references.pmid: 18617349
references.citation: Cardiovasc Drug Rev. 2004 Winter;22(4):263-84
references.pmid: 15592574
references.citation: J Chromatogr A. 2006 Jul 7;1120(1-2):1-12
references.pmid: 16600255
references.citation: J Chromatogr A. 2000 May 26;879(2):219-33
references.pmid: 10893038
references.citation: J Med Chem. 2007 Jun 14;50(12):2903-15
references.pmid: 17506540
references.citation: J Chromatogr B Biomed Sci Appl. 2001 Feb 10;751(1):169-75
references.pmid: 11232847
references.citation: J Chromatogr. 1992 Jan 31;590(2):341-53
references.pmid: 1560101
references.citation: J Chromatogr A. 2005 Sep 2;1085(2):190-8
references.pmid: 16106698