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J Pharm Biomed Anal. 2016 Nov 30;131:233-245. doi: 10.1016/j.jpba.2016.08.014. Epub 2016 Aug 20.

Stereoselective determination of citalopram and desmethylcitalopram in human plasma and breast milk by liquid chromatography tandem mass spectrometry.

Author information

1
School of Pharmaceutical Sciences, University of Geneva and University of Lausanne, Geneva, Switzerland.
2
School of Pharmaceutical Sciences, University of Geneva and University of Lausanne, Geneva, Switzerland; Division of Clinical Pharmacology, Lausanne University Hospital, Lausanne, Switzerland.
3
Department of Neonatology, Hospices Civils de Lyon, Lyon, France.
4
EPICIME-CIC 1407, Inserm, Service of Clinical Pharmacology, CHU-Lyon, Bron, France.
5
Department of Neonatology, Maternité Régionale, Université de Lorraine, Nancy, France.
6
School of Pharmaceutical Sciences, University of Geneva and University of Lausanne, Geneva, Switzerland; Unit of Pharmacogenetics and Clinical Psychopharmacology, Centre for Psychiatric Neuroscience, Department of Psychiatry, Lausanne University Hospital, Prilly, Switzerland.
7
Unit of Pharmacogenetics and Clinical Psychopharmacology, Centre for Psychiatric Neuroscience, Department of Psychiatry, Lausanne University Hospital, Prilly, Switzerland. Electronic address: nicolas.ansermot@chuv.ch.

Abstract

A high performance liquid chromatography (HPLC) tandem mass spectrometry (MS/MS) method was developed for the simultaneous, stereoselective quantification of the antidepressant citalopram and its active metabolite desmethylcitalopram in human plasma and breast milk. Sample preparation was performed by a two-step approach, including generic protein precipitation with acetonitrile followed by solid phase extraction. Enantiospecific separation of analytes was achieved on a Phenomenex® Lux Cellulose-2 column (4.6mm×150mm; 5μm), using reversed phase chromatography conditions characterized by a gradient elution of ammonium acetate buffer (pH 9.0; 20mM) and acetonitrile at a flow rate of 0.6ml/min. The compounds were detected by a tandem quadrupole mass spectrometer equipped with an electrospray ionization source and operating in multiple reaction monitoring mode. The method was fully validated in both biological fluids over a large concentration range of 0.1-100ng/ml for S-(+)- and R-(-)-citalopram, and 0.3-100ng/ml for S-(+)- and R-(-)-desmethylcitalopram. Trueness (90.0-113.3% and 97.1-103.6%), repeatability (0.9-15.9% and 0.9-8.4%) and intermediate precision (1.3-17.8% and 0.9-9.6%) in plasma and breast milk, respectively, meet international guidelines for method validation. Internal standard-normalized matrix effects ranged between 99 and 101% and 98-105%, respectively. The accuracy profiles (total error of trueness and precision) were mostly within the acceptance limits for biological samples defined as ±30%. The method was successfully applied to patient samples in a clinical trial setting.

KEYWORDS:

Breast milk; Citalopram; Enantiomer; LC–MS/MS; Plasma; Quantification

PMID:
27606925
DOI:
10.1016/j.jpba.2016.08.014
[Indexed for MEDLINE]

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