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High-throughput on-line solid-phase extraction-liquid chromatography-tandem mass spectrometry method for the simultaneous analysis of 14 antidepressants and their metabolites in plasma.
J Chromatogr A. 2007 Aug 10; 1160(1-2):3-12.JC

Abstract

A rapid, sensitive and fully automated on-line solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) method was developed and validated for the direct analysis of 14 antidepressants and their metabolites in plasma. Integration of the sample extraction and LC separation into a single system permitted direct injection of the plasma without prior sample pre-treatment. The applied gradient ensured the elution of all the examined drugs within 14 min and produced chromatographic peaks of acceptable symmetry. The total process time was 20 min and only 50 microL of plasma was required. Selectivity of the method was achieved by a combination of retention time and two precursor-product ion transitions for the non-deuterated compounds. The use of SPE was demonstrated to be highly effective and led to significant decreases in the interferences present in the matrix. Extraction was found to be both reproducible and efficient with recoveries >99% for all the analytes. The method showed excellent intra-assay and inter-assay precision (relative standard deviation (RSD) and bias <20%) for quality control (QC) samples spiked at a concentration of 40, 200 and 800 microg/L and the r2>0.99 over the range investigated (10-1000 microg/L). Limits of quantification (LOQs) were estimated to be 10 microg/L. Furthermore, the processed samples were demonstrated to be stable for at least 48 h, except for clomipramine and norclomipramine, where a slight negative trend was observed, but did not compromise the quantification. The method was subsequently applied to authentic samples previously screened by a routine HPLC method with diode array detection (DAD).

Authors+Show Affiliations

Forensic Toxicology Service, Institute of Legal Medicine, University of Santiago de Compostela, Santiago de Compostela, Spain.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't

Language

eng

PubMed ID

17321530

Citation

de Castro, Ana, et al. "High-throughput On-line Solid-phase Extraction-liquid Chromatography-tandem Mass Spectrometry Method for the Simultaneous Analysis of 14 Antidepressants and Their Metabolites in Plasma." Journal of Chromatography. A, vol. 1160, no. 1-2, 2007, pp. 3-12.
de Castro A, Ramírez Fernandez Mdel M, Laloup M, et al. High-throughput on-line solid-phase extraction-liquid chromatography-tandem mass spectrometry method for the simultaneous analysis of 14 antidepressants and their metabolites in plasma. J Chromatogr A. 2007;1160(1-2):3-12.
de Castro, A., Ramírez Fernandez, M. d. e. l. . M., Laloup, M., Samyn, N., De Boeck, G., Wood, M., Maes, V., & López-Rivadulla, M. (2007). High-throughput on-line solid-phase extraction-liquid chromatography-tandem mass spectrometry method for the simultaneous analysis of 14 antidepressants and their metabolites in plasma. Journal of Chromatography. A, 1160(1-2), 3-12.
de Castro A, et al. High-throughput On-line Solid-phase Extraction-liquid Chromatography-tandem Mass Spectrometry Method for the Simultaneous Analysis of 14 Antidepressants and Their Metabolites in Plasma. J Chromatogr A. 2007 Aug 10;1160(1-2):3-12. PubMed PMID: 17321530.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - High-throughput on-line solid-phase extraction-liquid chromatography-tandem mass spectrometry method for the simultaneous analysis of 14 antidepressants and their metabolites in plasma. AU - de Castro,Ana, AU - Ramírez Fernandez,Maria del Mar, AU - Laloup,Marleen, AU - Samyn,Nele, AU - De Boeck,Gert, AU - Wood,Michelle, AU - Maes,Viviane, AU - López-Rivadulla,Manuel, Y1 - 2007/02/08/ PY - 2006/11/28/received PY - 2007/01/15/revised PY - 2007/01/18/accepted PY - 2007/2/27/pubmed PY - 2007/9/28/medline PY - 2007/2/27/entrez SP - 3 EP - 12 JF - Journal of chromatography. A JO - J Chromatogr A VL - 1160 IS - 1-2 N2 - A rapid, sensitive and fully automated on-line solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC-MS/MS) method was developed and validated for the direct analysis of 14 antidepressants and their metabolites in plasma. Integration of the sample extraction and LC separation into a single system permitted direct injection of the plasma without prior sample pre-treatment. The applied gradient ensured the elution of all the examined drugs within 14 min and produced chromatographic peaks of acceptable symmetry. The total process time was 20 min and only 50 microL of plasma was required. Selectivity of the method was achieved by a combination of retention time and two precursor-product ion transitions for the non-deuterated compounds. The use of SPE was demonstrated to be highly effective and led to significant decreases in the interferences present in the matrix. Extraction was found to be both reproducible and efficient with recoveries >99% for all the analytes. The method showed excellent intra-assay and inter-assay precision (relative standard deviation (RSD) and bias <20%) for quality control (QC) samples spiked at a concentration of 40, 200 and 800 microg/L and the r2>0.99 over the range investigated (10-1000 microg/L). Limits of quantification (LOQs) were estimated to be 10 microg/L. Furthermore, the processed samples were demonstrated to be stable for at least 48 h, except for clomipramine and norclomipramine, where a slight negative trend was observed, but did not compromise the quantification. The method was subsequently applied to authentic samples previously screened by a routine HPLC method with diode array detection (DAD). SN - 0021-9673 UR - https://www.unboundmedicine.com/medline/citation/17321530/High_throughput_on_line_solid_phase_extraction_liquid_chromatography_tandem_mass_spectrometry_method_for_the_simultaneous_analysis_of_14_antidepressants_and_their_metabolites_in_plasma_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0021-9673(07)00122-7 DB - PRIME DP - Unbound Medicine ER -