A high-throughput method based on microwave-assisted extraction and liquid chromatography-tandem mass spectrometry for simultaneous analysis of amphetamines, ketamine, opiates, and their metabolites in hair

Anal Bioanal Chem. 2014 Apr;406(9-10):2445-55. doi: 10.1007/s00216-014-7669-z. Epub 2014 Mar 7.

Abstract

A total sample-preparation and analysis time of 50 min is required for the high-throughput method of hair analysis proposed in this paper. The method is applicable to analysis of drugs commonly used in Asia, and their metabolites--methamphetamine (MA), amphetamine (AMP), methylenedioxymethamphetamine (MDMA), methylenedioxyamphetamine (MDA), ketamine (K), norketamine (NK), dehydronorketamine (DHNK), 6-acetylmorphine (6-AM), morphine (MOR), and codeine (COD). Cut and weighed hair (10 mg) was incubated for 3 min with methanol-trifluoroacetic acid (TFA) during microwave-assisted extraction (MAE) at 700 W. The incubation solution was evaporated, the residue was reconstituted in deionized water-methanol, 99:1 (v/v), and 20 μL was injected on to a core-shell column (50 × 4.6 mm, 2.6 μm particle size) for liquid chromatographic-tandem mass spectrometric (LC-MS-MS) analysis. Gradient elution separation was performed in 8 min at a flow rate of 1 mL min(-1). No signal interfering with any of the analytes was found in fourteen blank hair samples from different sources. The limits of detection and quantification were 0.5 pg mg(-1) and 2.0 pg mg(-1), respectively, for MA, AMP, MDMA, MDA, K, NK, and DHNK, and 2.0 pg mg(-1) and 5.0 pg mg(-1), respectively, for 6-AM, MOR and COD. The linear range was between the LOQ and 1000 pg mg(-1), and the correlation coefficients were all greater than 0.999. Investigation of matrix effects revealed that all the analytes were suppressed by less than 20% and the standard deviation (SD) was always less than 7%. Recovery was always greater than 90% and the SD for each compound was less than 6%. Precision and accuracy for each analyte were within 15%. Eight authentic hair specimens from known drug abusers were successfully analyzed. Compared with traditional overnight incubation methods, the rapid 3-min extraction time achieved similar or greater extraction yields. Sample preparation by MAE was a reliable procedure for extraction of the analytes from hair but substantially simpler and faster than other methods.

Publication types

  • Evaluation Study
  • Research Support, Non-U.S. Gov't

MeSH terms

  • Amphetamines / analysis*
  • Amphetamines / isolation & purification
  • Amphetamines / metabolism
  • Analgesics, Opioid / analysis*
  • Analgesics, Opioid / isolation & purification
  • Analgesics, Opioid / metabolism
  • Chromatography, High Pressure Liquid / methods*
  • Hair / chemistry*
  • High-Throughput Screening Assays / methods*
  • Humans
  • Illicit Drugs / analysis*
  • Illicit Drugs / isolation & purification
  • Illicit Drugs / metabolism
  • Ketamine / analysis*
  • Ketamine / isolation & purification
  • Ketamine / metabolism
  • Microwaves
  • Substance Abuse Detection / methods
  • Tandem Mass Spectrometry / methods*

Substances

  • Amphetamines
  • Analgesics, Opioid
  • Illicit Drugs
  • Ketamine