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Hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) determination of cocaine and its metabolites benzoylecgonine, ecgonine methyl ester, and cocaethylene in hair samples.
Anal Bioanal Chem. 2010 Mar; 396(5):1703-12.AB

Abstract

This study reports the development and validation of a method using hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) for the analysis of cocaine and its metabolites benzoylecgonine (BE), ecgonine methyl ester (EME), and cocaethylene (CE) in hair samples. Decontamination was performed as follows: Firstly, the aliquot of hair was briefly rinsed with 2 mL dichloromethane, then was washed three times with 10 mL 0.01 M phosphate buffer, pH 6, for 15 min, followed by 2 mL 2-propanol for less than 2 min, and, finally, a last rinse with 2 mL dichloromethane was again done. Cocaine compounds were extracted from 10 mg of hair by incubation with 2 mL 0.1 M HCl at 50 °C for 12 h and purified by solid phase extraction with Oasis MCX cartridges. Analysis was performed by LC-MS/MS using an Atlantis HILIC silica chromatographic column. The method was fully validated. Linearity was established over the concentration range 0.020-10.0 ng/mg for cocaine (COC), 0.010-10.0 ng/mg for BE and CE, and 0.005-2.0 ng/mg for EME, and the correlation coefficients were all >0.99. Extraction efficiency was >70% for all analytes. Limits of detection were 0.0005 ng/mg for CE and 0.001 ng/mg for the other analytes (COC, BE, and EME). Lower limits of quantification were the lowest points of the calibration curves with acceptable accuracy and precision (coefficient of variation ≤20%). Intra- and inter-day imprecision ranged between 1.5% and 9.5% and 0.7% and 12.6%, respectively. Intra- and inter-day inaccuracy ranged from 0.5% to 12.3% and from 0.7% to 7.1%, respectively. With regard to matrix effects, suppression was <27.5% in all cases. The method was applied to the analysis of several samples derived from forensic cases.

Authors+Show Affiliations

Forensic Toxicology Service, Institute of Legal Medicine, University of Santiago de Compostela, San Francisco s/n, 15782, Santiago de Compostela, Spain. oscar.quintela@usc.esNo 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

20052577

Citation

Quintela, Oscar, et al. "Hydrophilic Interaction Liquid Chromatography-tandem Mass Spectrometry (HILIC-MS/MS) Determination of Cocaine and Its Metabolites Benzoylecgonine, Ecgonine Methyl Ester, and Cocaethylene in Hair Samples." Analytical and Bioanalytical Chemistry, vol. 396, no. 5, 2010, pp. 1703-12.
Quintela O, Lendoiro E, Cruz A, et al. Hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) determination of cocaine and its metabolites benzoylecgonine, ecgonine methyl ester, and cocaethylene in hair samples. Anal Bioanal Chem. 2010;396(5):1703-12.
Quintela, O., Lendoiro, E., Cruz, A., de Castro, A., Quevedo, A., Jurado, C., & López-Rivadulla, M. (2010). Hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) determination of cocaine and its metabolites benzoylecgonine, ecgonine methyl ester, and cocaethylene in hair samples. Analytical and Bioanalytical Chemistry, 396(5), 1703-12. https://doi.org/10.1007/s00216-009-3393-5
Quintela O, et al. Hydrophilic Interaction Liquid Chromatography-tandem Mass Spectrometry (HILIC-MS/MS) Determination of Cocaine and Its Metabolites Benzoylecgonine, Ecgonine Methyl Ester, and Cocaethylene in Hair Samples. Anal Bioanal Chem. 2010;396(5):1703-12. PubMed PMID: 20052577.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) determination of cocaine and its metabolites benzoylecgonine, ecgonine methyl ester, and cocaethylene in hair samples. AU - Quintela,Oscar, AU - Lendoiro,Elena, AU - Cruz,Angelines, AU - de Castro,Ana, AU - Quevedo,Alfredo, AU - Jurado,Carmen, AU - López-Rivadulla,Manuel, Y1 - 2010/01/06/ PY - 2009/09/18/received PY - 2009/12/08/accepted PY - 2009/11/30/revised PY - 2010/1/7/entrez PY - 2010/1/7/pubmed PY - 2011/2/10/medline SP - 1703 EP - 12 JF - Analytical and bioanalytical chemistry JO - Anal Bioanal Chem VL - 396 IS - 5 N2 - This study reports the development and validation of a method using hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) for the analysis of cocaine and its metabolites benzoylecgonine (BE), ecgonine methyl ester (EME), and cocaethylene (CE) in hair samples. Decontamination was performed as follows: Firstly, the aliquot of hair was briefly rinsed with 2 mL dichloromethane, then was washed three times with 10 mL 0.01 M phosphate buffer, pH 6, for 15 min, followed by 2 mL 2-propanol for less than 2 min, and, finally, a last rinse with 2 mL dichloromethane was again done. Cocaine compounds were extracted from 10 mg of hair by incubation with 2 mL 0.1 M HCl at 50 °C for 12 h and purified by solid phase extraction with Oasis MCX cartridges. Analysis was performed by LC-MS/MS using an Atlantis HILIC silica chromatographic column. The method was fully validated. Linearity was established over the concentration range 0.020-10.0 ng/mg for cocaine (COC), 0.010-10.0 ng/mg for BE and CE, and 0.005-2.0 ng/mg for EME, and the correlation coefficients were all >0.99. Extraction efficiency was >70% for all analytes. Limits of detection were 0.0005 ng/mg for CE and 0.001 ng/mg for the other analytes (COC, BE, and EME). Lower limits of quantification were the lowest points of the calibration curves with acceptable accuracy and precision (coefficient of variation ≤20%). Intra- and inter-day imprecision ranged between 1.5% and 9.5% and 0.7% and 12.6%, respectively. Intra- and inter-day inaccuracy ranged from 0.5% to 12.3% and from 0.7% to 7.1%, respectively. With regard to matrix effects, suppression was <27.5% in all cases. The method was applied to the analysis of several samples derived from forensic cases. SN - 1618-2650 UR - https://www.unboundmedicine.com/medline/citation/20052577/Hydrophilic_interaction_liquid_chromatography_tandem_mass_spectrometry__HILIC_MS/MS__determination_of_cocaine_and_its_metabolites_benzoylecgonine_ecgonine_methyl_ester_and_cocaethylene_in_hair_samples_ L2 - https://dx.doi.org/10.1007/s00216-009-3393-5 DB - PRIME DP - Unbound Medicine ER -