Simultaneous quantitative determination of amphetamines, ketamine, opiates and metabolites in human hair by gas chromatography/mass spectrometry

Abstract

A gas chromatography/mass spectrometry (GC/MS) method was developed and validated for the determination of common drugs of abuse in Asia. The method was able to simultaneously quantify amphetamines (amphetamine; AP, methamphetamine; MA, methylenedioxy amphetamine; MDA, methylenedioxymeth mphetamine; MDMA, methylenedioxy ethylamphetamine; MDEA), ketamine (ketamine; K, norketamine; NK), and opiates (morphine; MOR, codeine; COD, 6-acetylmorphine; 6-AM) in human hair. Hair samples (25 mg) were washed, cut, and incubated overnight at 25 degrees C in methanol/trifluoroacetic acid (methanol/TFA). The samples were extracted by solid-phase extraction (SPE), derivatized using heptafluorobutyric acid anhydride (HFBA) at 70 degrees C for 30 min, and the derivatives were analyzed by electron ionization (EI) GC/MS in selected ion monitoring mode. Confirmation was accomplished by comparing retention times and the relative abundances of selected ions with those of standards. Deuterated analogs of the analytes were used as internal standards for quantification. Calibration curves for ten analytes were established in the concentration range 0.1-10 ng/mg with high correlation coefficients (r2 > 0.999). The intra-day and inter-day precisions were within 12.1% and 15.8%, respectively. The intra-day and inter-day accuracies were between -8.7% and 10.7%, and between -5.9% and 13.8%, respectively. The limit of detection (LOD) and limit of quantification (LOQ) obtained were 0.03 and 0.05 ng/mg for AP, MA, MDA, MDMA and MDEA; 0.05 and 0.08 ng/mg for K, NK, MOR and COD; and 0.08 and 0.1 ng/mg for 6-AM. The recoveries were above 88.6% for all the compounds, except K and NK which were in the range of 71.7-72.7%. Eight hair samples from known polydrug abusers were examined by this method. These results show that the method is suitable for broad-spectrum drug testing in a single hair specimen.

Evaluation of hair roots for detection of methamphetamine and 3,4-methylenedioxymethamphetamine abuse by use of an HPLC–chemiluminescence method

“…The LOQ at S/N010 ranged from 0.017-0.191 ng mg −1 , Table 1). The sensitivity of the method was comparable with that of current conventional GC-MS methods [5][6][7] but was a factor of 10 lower than that of LC-MS-MS [11]. However, the amount of hair needed for assay by this method (1 mg) was substantially less than that required by the other methods (20-50 mg).…”

“…Gas chromatography-mass spectrometry (GC-MS) [5][6][7], high-performance liquid chromatography-fluorescence (HPLC-FL) detection [8][9][10], liquid chromatography-mass spectrometry (LC)-MS (or MS-MS) [11], and capillary zone electrophoresis-MS [12] have been used. However, there are few methods for determination of MP and related drugs in hair roots.…”

Electrochemiluminescence detection of methamphetamine based on a Ru(bpy)32+‐doped silica nanoparticles/Nafion composite film modified electrode

“…As a result, the determination of METH has attracted attention. So far, many methods have been used, including gas chromatography, [30] HPLC, [31] gas chromatographymass spectrometry (GC-MS), [32] chromatography-mass spec-trometry (LC-MS), [33] solid-phase microextraction-capillary zone electrophoresis [34] and capillary electrophoresis electrochemical/ electrochemiluminescence [35] for quantifying METH in hair, [29] plasma [31] or urine. [36] However, for these methods, expensive equipment and a long testing time are needed.…”

Simultaneous and group determination methods for designated substances by HPLC with multi‐channel electrochemical detection and their application to real samples

“…However, the number of simultaneous determination methods, which are simple and sensitive, for various tryptamine, phenethylamine and piperazine analogs is quite limited. HPLC-FL (Nakamura et al, 2007;Tomita et al, 2006), GC-MS (Awad et al, 2005;Theobald and Maurer 2006;Theobald et al, 2005;Lin et al, 2003;Balikova, 2005;Kikura-Hanajiri et al, 2005 and LC-MS (Leung et al, 2007;Gottardo et al, 2007;Nakashima 2005;Nishida et al, 2006;Jimenez et al, 2006;Carrera et al, 2007;Appollonio et al, 2006;Wu et al, 2008) are the most convenient methods for distinguishing the drugs. In our previous reports, fluorescence labeling methods by LC separation and TOF-MS detection were developed for the designated substances (Min et al, 2008(Min et al, , 2009).…”