Development and Validation of a Method for the Analysis of Bisoprolol and Atenolol in Human Bone.
beta-blockers
gas chromatography–mass spectrometry
human bone
Journal
Molecules (Basel, Switzerland)
ISSN: 1420-3049
Titre abrégé: Molecules
Pays: Switzerland
ID NLM: 100964009
Informations de publication
Date de publication:
29 Jun 2019
29 Jun 2019
Historique:
received:
28
05
2019
accepted:
24
06
2019
entrez:
3
7
2019
pubmed:
3
7
2019
medline:
19
12
2019
Statut:
epublish
Résumé
A method based on gas chromatography-mass spectrometry (GC-MS) is described for the determination of bisoprolol and atenolol in human bone. After the addition of lobivolol as internal standard, pulverized samples were incubated in acetonitrile for 1 h under ultrasounds. After adjusting the pH of the samples to 6, they were centrifuged, and the supernatants were subjected to solid phase extraction. Elution was achieved by using 3 mL of 2% ammonium hydroxide in 80:20 dichloromethane:isopropanol solution. Eluted samples were evaporated and derivatized. Chromatography was performed on a fused silica capillary column and analytes were determined in the selected-ion-monitoring (SIM) mode. The assay was validated in the range 0.1-0.3 ng/mg (depending on the drug) to 150 ng/mg, the mean absolute recoveries were 60% for bisoprolol and 106% for atenolol, the matrix effect was 69% for bisoprolol and 70% for atenolol and process efficiency was 41% for bisoprolol and 80% for atenolol. The intra- and inter-assay accuracy values were always better than 12%. The validated method was then applied to bone samples from two real forensic cases in which toxicological analysis in blood were positive for atenolol in the first case (0.65 µg/mL) and bisoprolol in the second case (0.06 µg/mL). Atenolol was found in bone samples from the corresponding case at the approximate concentration of 148 ng/mg and bisoprolol was found at 8 ng/mg.
Identifiants
pubmed: 31261852
pii: molecules24132400
doi: 10.3390/molecules24132400
pmc: PMC6651798
pii:
doi:
Substances chimiques
Atenolol
50VV3VW0TI
Bisoprolol
Y41JS2NL6U
Types de publication
Journal Article
Langues
eng
Sous-ensembles de citation
IM
Déclaration de conflit d'intérêts
The authors declare no conflict of interest.
Références
BMJ. 1999 Jun 26;318(7200):1730-7
pubmed: 10381708
Ther Drug Monit. 2000 Feb;22(1):79-83
pubmed: 10688265
Am J Forensic Med Pathol. 2000 Mar;21(1):56-8
pubmed: 10739227
Ann Intern Med. 2001 Apr 3;134(7):550-60
pubmed: 11281737
J Forensic Sci. 2001 Jul;46(4):916-8
pubmed: 11451078
J Intern Med. 2001 Oct;250(4):327-41
pubmed: 11576320
Forensic Sci Int. 2001 Dec 1;123(2-3):140-1
pubmed: 11728739
Forensic Sci Int. 2003 Apr 23;133(1-2):107-12
pubmed: 12742696
JAMA. 2003 May 21;289(19):2560-72
pubmed: 12748199
Pharmazie. 2003 Jul;58(7):447-74
pubmed: 12889529
Anal Chem. 2003 Jul 1;75(13):3019-30
pubmed: 12964746
J Forensic Sci. 2005 May;50(3):679-81
pubmed: 15932107
Forensic Sci Int. 2006 Jan 27;156(2-3):91-4
pubmed: 16410157
Forensic Sci Int. 2006 Jan 27;156(2-3):106-17
pubmed: 16410160
Forensic Sci Int. 2007 Mar 2;166(2-3):139-44
pubmed: 16730149
Analyst. 2006 Sep;131(9):961-5
pubmed: 17047795
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 May 1;850(1-2):147-60
pubmed: 17175206
J Am Coll Cardiol. 2007 Aug 14;50(7):563-72
pubmed: 17692739
J Forensic Sci. 2008 Nov;53(6):1474-82
pubmed: 18752550
Clin J Am Soc Nephrol. 2008 Nov;3 Suppl 3:S131-9
pubmed: 18988698
J Anal Toxicol. 2008 Oct;32(8):631-8
pubmed: 19007514
Forensic Sci Int. 2009 Mar 10;185(1-3):100-6
pubmed: 19201558
Am J Forensic Med Pathol. 2009 Mar;30(1):40-4
pubmed: 19237852
Forensic Sci Int. 2009 Jul 1;188(1-3):23-30
pubmed: 19376659
J Forensic Sci. 2009 May;54(3):708-14
pubmed: 19432747
Forensic Sci Int. 2010 Jan 30;194(1-3):60-6
pubmed: 19963329
Forensic Sci Int. 2011 Apr 15;207(1-3):40-5
pubmed: 20884144
J Anal Toxicol. 2010 Oct;34(8):510-5
pubmed: 21819797
J Anal Toxicol. 2011 Sep;35(7):452-8
pubmed: 21871154
J Forensic Sci. 2012 Mar;57(2):544-9
pubmed: 22150755
J Anal Toxicol. 2012 Jul;36(6):429-33
pubmed: 22582220
Lancet. 2012 Dec 15;380(9859):2224-60
pubmed: 23245609
Drug Test Anal. 2014 Apr;6(4):308-16
pubmed: 23881890
J Anal Toxicol. 2013 Oct;37(8):565-72
pubmed: 23986100
J Forensic Leg Med. 2014 Feb;22:7-9
pubmed: 24485412
Expert Opin Drug Metab Toxicol. 2014 Sep;10(9):1221-9
pubmed: 24995883
Forensic Sci Med Pathol. 2014 Dec;10(4):496-503
pubmed: 25037237
J Anal Toxicol. 2014 Oct;38(8):548-54
pubmed: 25217545
J Anal Toxicol. 2016 Oct;40(8):669-676
pubmed: 27562970
Cochrane Database Syst Rev. 2017 Jan 20;1:CD002003
pubmed: 28107561
Ann Emerg Med. 1985 Feb;14(2):161-3
pubmed: 2857542
Curr Pharm Des. 2017;23(36):5455-5467
pubmed: 28641530
Curr Pharm Des. 2017;23(36):5442-5454
pubmed: 28714407
J Anal Toxicol. 2018 Jan 1;42(1):1-5
pubmed: 29036543
Drug Test Anal. 2018 Jun;10(6):961-967
pubmed: 29055108
Forensic Sci Int. 2018 Sep;290:137-145
pubmed: 30036735
J Forensic Sci. 2019 Mar;64(2):643-646
pubmed: 30132893
Pharmacol Res. 2019 Jan;139:489-490
pubmed: 30290223
J Pharm Biomed Anal. 2019 Feb 5;164:636-641
pubmed: 30471636
Clin Toxicol (Phila). 2018 Dec;56(12):1213-1415
pubmed: 30576252
Forensic Sci Int. 2019 Jun;299:154-160
pubmed: 31009827
J Anal Toxicol. 1995 Oct;19(6):519-21
pubmed: 8926749
N Engl J Med. 1996 Dec 5;335(23):1713-20
pubmed: 8929262
Int J Legal Med. 1997;110(5):281-3
pubmed: 9297586