Radioimmunoassay of drugs of abuse in hair Part 2: The determination of methadone in the hair of known drug users

doi:10.1016/0731-7085(95)01517-O

Journal of Pharmaceutical and Biomedical Analysis

Volume 13, Issue 7, June 1995, Pages 829-839

https://doi.org/10.1016/0731-7085(95)01517-O Get rights and content

Abstract

This communication addresses the analytical problems associated with the analysis of hair specimens from known users and misusers of the synthetic opioid methadone. An adapted radioimmunoassay and a previously developed preanalytical decontamination procedure have been applied to samples from known drug users. The removal of drugs from the hair surface by washing and the effect of proprietary hair treatments on methadone entrapped in the hair have also been investigated. Pre-analytical washing reduced methadone levels by up to 29%, whilst hair colouration and peroxide bleaching were found to reduce levels by up to 21%, and 50% respectively. Methadone assay of extracts from dated hair segments were shown to provide long term histories of methadone intake, under controlled and non-controlled conditions. Evidence that a dose relationship between hair drug levels and intake may exist is presented. Results of hair analysis, expressed as ng methadone/mg hair, from drug users (range 0.20–10.63) are compared to a pre-determined cut-off of 0.1 ng methadone/mg hair, obtained from the analysis of a known drug free population (n = 23).

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Cited by (18)

Preconcentration of trace amounts of methadone in human urine, plasma, saliva and sweat samples using dispersive liquid-liquid microextraction followed by high performance liquid chromatography
2012, Talanta
Citation Excerpt :
These include several analytical methods based on gas chromatography (GC) coupled with mass spectrometry (MS) [6,7] and flame ionization detection (FID) [8], liquid chromatography (LC) coupled with ultra violet (UV) [9], coulometric [10] and MS [11] detection, capillary electrophoresis [12] coupled with UV [13], MS [14] and electrochemiluminescence detection (ECL) [15], flow-injection analysis (FIA) [16], radioimmunoassay [17] and potentiometry with ion-selective electrode [18]. So far, analysis of methadone was performed in several biological samples such as serum [19], plasma [20], urine [21], hair [22], sweat [23] and saliva [24]. Due to the complex matrix of the real samples and the low concentration of methadone, making efforts to develop a simple and reliable method for preconcentration and determination of the methadone is the main challenge and a very important step for the analysis of it.
A simple, rapid and efficient method for the preconcentration of methadone was developed using dispersive liquid–liquid microextraction (DLLME) followed by high performance liquid chromatography with ultra violet detection (HPLC–UV). The extraction method is based on the fast injection of a mixture of extracting and disperser solvents into the aqueous solution to form a cloudy ternary component solvent (aqueous solution:extracting solvent:disperser solvent) system. The extraction parameters such as nature and volume of extracting and disperser solvents, pH of sample, and extraction time were studied for optimization. Under the optimal conditions (extracting solvent: chloroform, 250 μL; disperser solvent: methanol, 2.5 mL and pH of sample: 10.0) a linear calibration curve was obtained in the range of 0.5–5000 ng mL⁻¹ with r² = 0.9995. To demonstrate analytical performance, figures of merits of the proposed method in four different biological matrices (urine, plasma, saliva and sweat) spiked with methadone were investigated. The limits of detection and quantification in these matrices were ranged from 4.90 to 24.85 ng mL⁻¹ and 16.32 to 82.75 ng mL⁻¹, respectively. The extraction recoveries were above 97% and the preconcentration factors of methadone in distilled water, urine, plasma, saliva, and sweat samples were 196.52, 10.03, 9.93, 1.97 and 1.99, respectively. While the precision for inter-day was ≤6.43 (n = 5), it was ≤2.26 (n = 5) for intra-day assay. Finally, the method was successfully applied in the determination of methadone in the human urine, plasma, saliva and sweat samples.
Determination of methadone and its metabolites EDDP and EMDP in human hair by headspace solid-phase microextraction and gas chromatography-mass spectrometry
2000, Journal of Chromatography B: Biomedical Sciences and Applications
A simple method for analysis of methadone and its two main metabolites EDDP and EMDP in hair was developed using automatic headspace solid-phase microextraction (HS-SPME) at a multipurpose sampler and gas chromatography – mass spectrometry with electron impact ionization and selected ion monitoring (GC–MS-SIM). The washed hair pieces were digested in the closed headspace vial in 1 ml 1 M NaOH containing 0.5 g NaCl and each 10 ng of the internal standards D₉-methadone and D₃-EDDP at 110°C for 20 min. Then the HS-SPME was performed with a 65 μm polydimethylsiloxan/divinylbenzene fiber at the same temperature in the same vial for another 20 min followed by the desorption in the GC injection port. The calibration curves were linear between 0.1 and 3 ng/mg (methadone and EMDP) and 10 ng/mg (EDDP) respectively, at higher concentrations a negative deviation from linearity was found. The detection limits were 0.03 ng/mg (methadone) and 0.05 ng/mg (EDDP and EMDP), and the reproducibility was 9.2% for methadone and 11.2% for EDDP (n=12). The method was applied to hair samples of 26 drug fatalities. 19 cases were positive with 0.36–11.8 ng/mg methadone and 0.19 –10.8 ng/mg EDDP. EMDP was found only in two cases with 0.18 and 0.84 ng/mg. The methadone concentration range was in agreement with previous data, but the EDDP/methadone concentration ratios (0.19–0.67) were definitely higher than those determined by other methods.
Forensic science
1997, Analytical Chemistry
Introducing an Electrochemical Sensor Based on Two Layers of Ag Nanoparticles Decorated Graphene for Rapid Determination of Methadone in Human Blood Serum
2022, Topics in Catalysis
Microextraction by packed sorbent as a novel strategy for sample clean-up in the determination of methadone and EDDP in hair
2020, Journal of Analytical Toxicology
Methadone and metabolites in hair of methadone-assisted pregnant women and their infants
2012, Therapeutic Drug Monitoring

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Full paperRadioimmunoassay of drugs of abuse in hair Part 2: The determination of methadone in the hair of known drug users

Abstract

J. Pharm. Biomed. Anal.

Forensic Sci. Int.

J. Chromatogr.

Forensic Sci. Int.

J. Pharm. Biomed. Anal.

J. Pharm. Biomed. Anal.

Addiction

J. Forensic Sci.

J. Okla, State Med. Assoc.

J. Nucl. Med.

Full paper
Radioimmunoassay of drugs of abuse in hair Part 2: The determination of methadone in the hair of known drug users