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Merck

Analysis of eight glycols in serum using LC-ESI-MS-MS.

Journal of analytical toxicology (2014-09-05)
Laurent Imbert, Elodie Saussereau, Christian Lacroix
ABSTRACT

A liquid chromatography coupled with electrospray tandem mass spectrometry method was developed for the analysis of ethylene glycol, diethylene glycol, triethylene glycol, 1,4-butanediol, 1,2-butanediol, 2,3-butanediol, 1,2-propanediol and 1,3-propanediol, in serum after a Schotten-Baumann derivatization by benzoyl chloride. Usual validation parameters were tested: linearity, repeatability and intermediate precision, limits of detection and quantification, carry over and ion suppression. Limits of detection were between 0.18 and 1.1 mg/L, and limits of quantification were between 0.4 and 2.3 mg/L. Separation of isomers was possible either chromatographically or by selecting specific multiple reaction monitoring transitions. This method could be a useful tool in case of suspected intoxication with antifreeze agents, solvents, dietary supplements or some medical drug compounds.

MATERIALS
Product Number
Brand
Product Description

Supelco
Sodium hydroxide concentrate, 0.1 M NaOH in water (0.1N), Eluent concentrate for IC
Sigma-Aldrich
Methanol, NMR reference standard
USP
Ethylene glycol, United States Pharmacopeia (USP) Reference Standard
Supelco
Ethylene glycol, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Diethylene glycol, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Propylene glycol, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Ethylene glycol, analytical standard
Sigma-Aldrich
1,2-Butanediol, purum, ≥98.0% (GC)
Supelco
Ethylene glycol solution, NMR reference standard, 80% in DMSO-d6 (99.9 atom % D), NMR tube size 5 mm × 8 in.
Sigma-Aldrich
Sodium hydroxide, BioUltra, for luminescence, ≥98.0% (T), pellets
Sigma-Aldrich
Sodium hydroxide solution, BioUltra, for molecular biology, 10 M in H2O
Supelco
Diethylene glycol, analytical standard
Supelco
Sodium hydroxide solution, 49-51% in water, eluent for IC
Sigma-Aldrich
Diethylene glycol, ReagentPlus®, 99%
Supelco
Methanol, analytical standard
Sigma-Aldrich
Ammonium formate, ≥99.995% trace metals basis
Sigma-Aldrich
Ethylene glycol, anhydrous, 99.8%
Sigma-Aldrich
Benzoyl chloride, ReagentPlus®, ≥99%
Sigma-Aldrich
Ethylene, ≥99.5%
Sigma-Aldrich
Benzoyl chloride, 99%
Sigma-Aldrich
Methanol, anhydrous, 99.8%
Sigma-Aldrich
1,2-Butanediol, 98%
Sigma-Aldrich
Propylene glycol, ≥99.5% (GC), FCC, FG
Sigma-Aldrich
3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%
Sigma-Aldrich
2,3-Butanediol, 98%
Sigma-Aldrich
Diethylene glycol, puriss. p.a., ≥99.0% (GC), colorless
Supelco
Ammonium formate, eluent additive for LC-MS, LiChropur, ≥99.0%
Sigma-Aldrich
Ethylene glycol, BioUltra, ≥99.5% (GC)
Sigma-Aldrich
Diethylene glycol, BioUltra, ≥99.0% (GC)
Sigma-Aldrich
Ammonium formate, BioUltra, ≥99.0% (calc. based on dry substance, NT)