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  • Analysis of ecstasy in oral fluid by ion mobility spectrometry and infrared spectroscopy after liquid-liquid extraction.

Analysis of ecstasy in oral fluid by ion mobility spectrometry and infrared spectroscopy after liquid-liquid extraction.

Journal of chromatography. A (2015-02-11)
Sergio Armenta, Salvador Garrigues, Miguel de la Guardia, Judit Brassier, Manel Alcalà, Marcelo Blanco
ABSTRACT

We developed and evaluated two different strategies for determining abuse drugs based on (i) the analysis of saliva by ion mobility spectrometry (IMS) after thermal desorption and (ii) the joint use of IMS and infrared (IR) spectroscopy after liquid-liquid microextraction (LLME) to enable the sensitivity-enhanced detection and double confirmation of ecstasy (MDMA) abuse. Both strategies proved effective for the intended purpose. Analysing saliva by IMS after thermal desorption, which provides a limit of detection (LOD) of 160μgL(-1), requires adding 0.2M acetic acid to the sample and using the truncated negative second derivative of the ion mobility spectrum. The joint use of IMS and IR spectroscopy after LLME provides an LOD of 11μgL(-1) with the former technique and 800μgL(-1) with the latter, in addition to a limit of confirmation (LOC) of 1.5mgL(-1). Using IMS after thermal desorption simplifies the operational procedure, and using it jointly with IR spectroscopy after LLME allows double confirmation of MDMA abuse with two techniques based on different principles (viz., IMS drift times and IR spectra). Also, it affords on-site analyses, albeit at a lower throughput.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Acetic acid-12C2, 99.9 atom % 12C
Supelco
Sodium hydroxide concentrate, 0.1 M NaOH in water (0.1N), Eluent concentrate for IC
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Hydrogen chloride solution, 3 M in cyclopentyl methyl ether (CPME)
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Acetic acid, ≥99.5%, FCC, FG
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Acetic acid, natural, ≥99.5%, FG
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Chloroform, anhydrous, contains amylenes as stabilizer, ≥99%
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Hydrogen chloride – ethanol, ~1.25 M HCl, derivatization grade (GC derivatization), LiChropur
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Acetic acid, suitable for luminescence, BioUltra, ≥99.5% (GC)
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Hydrogen chloride – 2-propanol solution, ~1.25 M HCl (T), derivatization grade (GC derivatization), LiChropur
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Hydrochloric acid solution, ~6 M in H2O, for amino acid analysis
Supelco
Sodium hydroxide solution, 49-51% in water, eluent for IC
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Sodium hydroxide solution, BioUltra, Molecular Biology, 10 M in H2O
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Potassium bromide, BioUltra, ≥99.5% (AT)
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Potassium bromide, anhydrous, powder, 99.95% trace metals basis
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Isopropyl alcohol, ≥99.7%, FCC, FG
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Potassium bromide, anhydrous, powder, 99.999% trace metals basis
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Hydrogen chloride – methanol solution, ~1.25 m HCl (T), derivatization grade (GC derivatization), LiChropur
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3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%
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Potassium bromide, BioXtra, ≥99.0%
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Hydrochloric acid solution, volumetric, 0.1 M HCl (0.1N), endotoxin free
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Hydrochloric acid, 36.5-38.0%, BioReagent, Molecular Biology
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Sodium hydroxide, BioUltra, suitable for luminescence, ≥98.0% (T), pellets
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Hydrochloric acid solution, 32 wt. % in H2O, FCC
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Chloroform, ≥99%, PCR Reagent, contains amylenes as stabilizer
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Hydrochloric acid solution, 1.0 N, BioReagent, suitable for cell culture
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Sodium hydroxide, BioXtra, ≥98% (acidimetric), pellets (anhydrous)
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Chloroform, biotech. grade, ≥99.8%, contains 0.5-1.0% ethanol as stabilizer
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Chloroform, contains amylenes as stabilizer, ACS reagent, ≥99.8%
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Chloroform, contains ethanol as stabilizer, meets analytical specification of BP, 99-99.4% (GC)
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Sodium hydroxide solution, 1.0 N, BioReagent, suitable for cell culture