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Segmental analysis of amphetamines in hair using a sensitive UHPLC-MS/MS method.
Drug Test Anal. 2014 Jun; 6 Suppl 1:22-9.DT

Abstract

A sensitive and robust ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated for quantification of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine and 3,4-methylenedioxy methamphetamine in hair samples. Segmented hair (10 mg) was incubated in 2M sodium hydroxide (80°C, 10 min) before liquid-liquid extraction with isooctane followed by centrifugation and evaporation of the organic phase to dryness. The residue was reconstituted in methanol:formate buffer pH 3 (20:80). The total run time was 4 min and after optimization of UHPLC-MS/MS-parameters validation included selectivity, matrix effects, recovery, process efficiency, calibration model and range, lower limit of quantification, precision and bias. The calibration curve ranged from 0.02 to 12.5 ng/mg, and the recovery was between 62 and 83%. During validation the bias was less than ±7% and the imprecision was less than 5% for all analytes. In routine analysis, fortified control samples demonstrated an imprecision <13% and control samples made from authentic hair demonstrated an imprecision <26%. The method was applied to samples from a controlled study of amphetamine intake as well as forensic hair samples previously analyzed with an ultra high performance liquid chromatography time of flight mass spectrometry (UHPLC-TOF-MS) screening method. The proposed method was suitable for quantification of these drugs in forensic cases including violent crimes, autopsy cases, drug testing and re-granting of driving licences. This study also demonstrated that if hair samples are divided into several short segments, the time point for intake of a small dose of amphetamine can be estimated, which might be useful when drug facilitated crimes are investigated.

Authors+Show Affiliations

Department of Forensic Genetics and Forensic Toxicology, National Board of Forensic Medicine, SE-58758, Linköping, Sweden.No affiliation info available

Pub Type(s)

Journal Article
Validation Study

Language

eng

PubMed ID

24817045

Citation

Jakobsson, Gerd, and Robert Kronstrand. "Segmental Analysis of Amphetamines in Hair Using a Sensitive UHPLC-MS/MS Method." Drug Testing and Analysis, vol. 6 Suppl 1, 2014, pp. 22-9.
Jakobsson G, Kronstrand R. Segmental analysis of amphetamines in hair using a sensitive UHPLC-MS/MS method. Drug Test Anal. 2014;6 Suppl 1:22-9.
Jakobsson, G., & Kronstrand, R. (2014). Segmental analysis of amphetamines in hair using a sensitive UHPLC-MS/MS method. Drug Testing and Analysis, 6 Suppl 1, 22-9. https://doi.org/10.1002/dta.1637
Jakobsson G, Kronstrand R. Segmental Analysis of Amphetamines in Hair Using a Sensitive UHPLC-MS/MS Method. Drug Test Anal. 2014;6 Suppl 1:22-9. PubMed PMID: 24817045.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Segmental analysis of amphetamines in hair using a sensitive UHPLC-MS/MS method. AU - Jakobsson,Gerd, AU - Kronstrand,Robert, PY - 2013/10/15/received PY - 2014/01/16/revised PY - 2014/02/14/accepted PY - 2014/5/13/entrez PY - 2014/5/13/pubmed PY - 2015/3/11/medline KW - LC-MS-MS KW - amphetamines KW - forensic KW - hair KW - segmental analysis SP - 22 EP - 9 JF - Drug testing and analysis JO - Drug Test Anal VL - 6 Suppl 1 N2 - A sensitive and robust ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed and validated for quantification of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine and 3,4-methylenedioxy methamphetamine in hair samples. Segmented hair (10 mg) was incubated in 2M sodium hydroxide (80°C, 10 min) before liquid-liquid extraction with isooctane followed by centrifugation and evaporation of the organic phase to dryness. The residue was reconstituted in methanol:formate buffer pH 3 (20:80). The total run time was 4 min and after optimization of UHPLC-MS/MS-parameters validation included selectivity, matrix effects, recovery, process efficiency, calibration model and range, lower limit of quantification, precision and bias. The calibration curve ranged from 0.02 to 12.5 ng/mg, and the recovery was between 62 and 83%. During validation the bias was less than ±7% and the imprecision was less than 5% for all analytes. In routine analysis, fortified control samples demonstrated an imprecision <13% and control samples made from authentic hair demonstrated an imprecision <26%. The method was applied to samples from a controlled study of amphetamine intake as well as forensic hair samples previously analyzed with an ultra high performance liquid chromatography time of flight mass spectrometry (UHPLC-TOF-MS) screening method. The proposed method was suitable for quantification of these drugs in forensic cases including violent crimes, autopsy cases, drug testing and re-granting of driving licences. This study also demonstrated that if hair samples are divided into several short segments, the time point for intake of a small dose of amphetamine can be estimated, which might be useful when drug facilitated crimes are investigated. SN - 1942-7611 UR - https://www.unboundmedicine.com/medline/citation/24817045/Segmental_analysis_of_amphetamines_in_hair_using_a_sensitive_UHPLC_MS/MS_method_ L2 - https://doi.org/10.1002/dta.1637 DB - PRIME DP - Unbound Medicine ER -