Solid phase microextraction and gas chromatography-mass spectrometry methods for residual solvent assessment in seized cocaine and heroin.
Anal Bioanal Chem
; 408(23): 6393-402, 2016 Sep.
Article
in En
| MEDLINE
| ID: mdl-27405875
ABSTRACT
A simple sample pre-treatment method based on solid phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) has been optimized and validated for the assessment of 15 residual solvents (2-propanol, 2-methylpentane, 3-methylpentane, acetone, ethyl acetate, benzene, hexane, methylcyclohexane, methylcyclopentane, m-xylene, propyl acetate, toluene, 1,2,4-trimethylbenzene, dichloromethane, and ethylbenzene) in seized illicit cocaine and heroin. DMSO and DMF as sample diluents were found to offer the best residual solvent transference to the head space for further adsorption onto the SPME fiber, and the developed method therefore showed high sensitivity and analytical recovery. Variables affecting SPME were fully evaluated by applying an experimental design approach. Best conditions were found when using an equilibration time of 5 min at 70 °C and headspace sampling of residual solvents at the same temperature for 15 min. Method validation, performed within the requirements of international guidelines, showed excellent sensitivity, as well as intra- and inter-day precision and accuracy. The proposed methodology was applied to 96 cocaine samples and 14 heroin samples seized in Galicia (northwestern Spain) within 2013 and 2014.
Key words
Full text:
1
Collection:
01-internacional
Database:
MEDLINE
Main subject:
Illicit Drugs
/
Cocaine
/
Heroin
/
Solid Phase Microextraction
/
Anesthetics, Local
/
Gas Chromatography-Mass Spectrometry
/
Narcotics
Type of study:
Evaluation_studies
/
Guideline
Language:
En
Journal:
Anal Bioanal Chem
Year:
2016
Document type:
Article
Affiliation country:
Spain