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GC-TOF MS Application: Drugs of Abuse in Urine

Drugs testing urine using the high sensitivity BenchTOF-dx™ and powerful data interrogation software

Prohibited drugsIntroduction

Gas chromatography/mass spectrometry (GC/MS) is a technique commonly used for identifying drugs of abuse (DOA) in urine. The recently-introduced BenchTOF-dx demonstrates breakthrough capability to provide exceptional sensitivity with spectra that are unaffected by spectral skew and exactly match ‘classical’, quadrupole-generated spectra.

The instrument’s associated software incorporates background-compensation, deconvolution and data-mining, which enhance and automate the identification of specific target compounds in a very complex sample like urine.

Experimental

Results

  • A urine sample was collected from a methadone substitution program.

  • Glucuronide separation was followed by sorptive extraction (SPE) using SPEC DAU cation exchangers to extract the organic compounds from the urine.

  • The underivatised sample was then evaporated and concentrated in 50 µL MeOH and a 1 µL aliquot used for GC/TOF-MS analysis.

  • Conditions:
    • Column: Optima 5 Accent 10 m x 0.2 mm x 0.35 µm
    • Run time: 10 min Transfer line: 250°C
    • Mass range: m/z 35–635
    • Scan rate/scanset rate: 10 kHz/2 H
    •  Ion source: 260°C

  • A target library of the compounds of interest was created in the BenchTOF-dx software package. The GC/MS data for the urine sample was then imported and searched for targets.

Chromatogram of urine

Drugs of abuse table

Section of report listing drugs of abuse found in the urine sample

The TIC is affected by high levels of background interference, expected of the nature of the sample. The TIC was imported into the BenchTOF-dx software which applies background compensation and deconvolution algorithms to the data followed by chemometric analysis of ‘clean’ peak spectra to identify target compounds.

The high S/N and quality of spectra derived from the BenchTOF-dx enhance the capabilities of the data interrogation software, ensuring reliable identification of compounds down to the lowest concentrations, e.g. alprazolam, and in underivatised forms.

Overlaid chromatograms showing amisulpride and alprazolam co-eluting

Overlaid chromatograms showing amisulpride and alprazolam co-eluting

The similarity of spectra is excellent despite the large matrix interference

The similarity of spectra is excellent despite the large matrix interference


Conclusion

The overall sample complexity may pose a problem for many analytical detection systems, but the BenchTOF-dx is able to record high quality mass spectra over a wide concentration range.

The ability of the BenchTOF-dx to deliver NIST-searchable spectra means that proprietary libraries may be employed without modification.

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