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Quantitative analysis of multiple illicit drugs in preserved oral fluid by solid-phase extraction and liquid chromatography-tandem mass spectrometry.
Forensic Sci Int. 2005 Jun 10; 150(2-3):227-38.FS

Abstract

We present a validated method for the simultaneous analysis of basic drugs which comprises a sample clean-up step, using mixed-mode solid-phase extraction (SPE), followed by LC-MS/MS analysis. Deuterated analogues for all of the analytes of interest were used for quantitation. The applied HPLC gradient ensured the elution of all the drugs examined within 14 min and produced chromatographic peaks of acceptable symmetry. Selectivity of the method was achieved by a combination of retention time, and two precursor-product ion transitions for the non-deuterated analogues. Oral fluid was collected with the Intercept, a FDA approved sampling device that is used on a large scale in the US for workplace drug testing. However, this collection system contains some ingredients (stabilizers and preservatives) that can cause substantial interferences, e.g. ion suppression or enhancement during LC-MS/MS analysis, in the absence of suitable sample pre-treatment. The use of the SPE was demonstrated to be highly effective and led to significant decreases in the interferences. Extraction was found to be both reproducible and efficient with recoveries >76% for all of the analytes. Furthermore, the processed samples were demonstrated to be stable for 48 h, except for cocaine and benzoylecgonine, where a slight negative trend was observed, but did not compromise the quantitation. In all cases the method was linear over the range investigated (2-200 microg/L) with an excellent intra-assay and inter-assay precision (coefficients of variation <10% in most cases) for QC samples spiked at a concentration of 4, 12 and 100 microg/L. Limits of quantitation were estimated to be at 2 microg/L with limits of detection ranging from 0.2 to 0.5 microg/L, which meets the requirements of SAMHSA for oral fluid testing in the workplace. The method was subsequently applied to the analysis of Intercept samples collected at the roadside by the police, and to determine MDMA and MDA levels in oral fluid samples from a controlled study.

Authors+Show Affiliations

Waters Corporation, MS Technologies Centre, Manchester, UK.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

Language

eng

PubMed ID

15944064

Citation

Wood, Michelle, et al. "Quantitative Analysis of Multiple Illicit Drugs in Preserved Oral Fluid By Solid-phase Extraction and Liquid Chromatography-tandem Mass Spectrometry." Forensic Science International, vol. 150, no. 2-3, 2005, pp. 227-38.
Wood M, Laloup M, Ramirez Fernandez Mdel M, et al. Quantitative analysis of multiple illicit drugs in preserved oral fluid by solid-phase extraction and liquid chromatography-tandem mass spectrometry. Forensic Sci Int. 2005;150(2-3):227-38.
Wood, M., Laloup, M., Ramirez Fernandez, M. d. e. l. . M., Jenkins, K. M., Young, M. S., Ramaekers, J. G., De Boeck, G., & Samyn, N. (2005). Quantitative analysis of multiple illicit drugs in preserved oral fluid by solid-phase extraction and liquid chromatography-tandem mass spectrometry. Forensic Science International, 150(2-3), 227-38.
Wood M, et al. Quantitative Analysis of Multiple Illicit Drugs in Preserved Oral Fluid By Solid-phase Extraction and Liquid Chromatography-tandem Mass Spectrometry. Forensic Sci Int. 2005 Jun 10;150(2-3):227-38. PubMed PMID: 15944064.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Quantitative analysis of multiple illicit drugs in preserved oral fluid by solid-phase extraction and liquid chromatography-tandem mass spectrometry. AU - Wood,Michelle, AU - Laloup,Marleen, AU - Ramirez Fernandez,Maria del Mar, AU - Jenkins,Kevin M, AU - Young,Michael S, AU - Ramaekers,Jan G, AU - De Boeck,Gert, AU - Samyn,Nele, Y1 - 2005/04/18/ PY - 2004/10/04/received PY - 2004/11/13/revised PY - 2004/11/14/accepted PY - 2005/6/10/pubmed PY - 2005/9/9/medline PY - 2005/6/10/entrez SP - 227 EP - 38 JF - Forensic science international JO - Forensic Sci Int VL - 150 IS - 2-3 N2 - We present a validated method for the simultaneous analysis of basic drugs which comprises a sample clean-up step, using mixed-mode solid-phase extraction (SPE), followed by LC-MS/MS analysis. Deuterated analogues for all of the analytes of interest were used for quantitation. The applied HPLC gradient ensured the elution of all the drugs examined within 14 min and produced chromatographic peaks of acceptable symmetry. Selectivity of the method was achieved by a combination of retention time, and two precursor-product ion transitions for the non-deuterated analogues. Oral fluid was collected with the Intercept, a FDA approved sampling device that is used on a large scale in the US for workplace drug testing. However, this collection system contains some ingredients (stabilizers and preservatives) that can cause substantial interferences, e.g. ion suppression or enhancement during LC-MS/MS analysis, in the absence of suitable sample pre-treatment. The use of the SPE was demonstrated to be highly effective and led to significant decreases in the interferences. Extraction was found to be both reproducible and efficient with recoveries >76% for all of the analytes. Furthermore, the processed samples were demonstrated to be stable for 48 h, except for cocaine and benzoylecgonine, where a slight negative trend was observed, but did not compromise the quantitation. In all cases the method was linear over the range investigated (2-200 microg/L) with an excellent intra-assay and inter-assay precision (coefficients of variation <10% in most cases) for QC samples spiked at a concentration of 4, 12 and 100 microg/L. Limits of quantitation were estimated to be at 2 microg/L with limits of detection ranging from 0.2 to 0.5 microg/L, which meets the requirements of SAMHSA for oral fluid testing in the workplace. The method was subsequently applied to the analysis of Intercept samples collected at the roadside by the police, and to determine MDMA and MDA levels in oral fluid samples from a controlled study. SN - 0379-0738 UR - https://www.unboundmedicine.com/medline/citation/15944064/Quantitative_analysis_of_multiple_illicit_drugs_in_preserved_oral_fluid_by_solid_phase_extraction_and_liquid_chromatography_tandem_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S0379-0738(05)00131-3 DB - PRIME DP - Unbound Medicine ER -