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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

Sigma-Aldrich
Diethylene glycol, puriss. p.a., ≥99.0% (GC), colorless
Sigma-Aldrich
Ammonium formate, BioUltra, ≥99.0% (calc. based on dry substance, NT)
Sigma-Aldrich
Ammonium formate, ≥99.995% trace metals basis
Sigma-Aldrich
Ammonium formate, reagent grade, 97%
Supelco
Ammonium formate, eluent additive for LC-MS, LiChropur, ≥99.0%
Sigma-Aldrich
Sodium hydroxide solution, 1.0 N, BioReagent, suitable for cell culture
Sigma-Aldrich
Sodium hydroxide, beads, 16-60 mesh, reagent grade, 97%
Sigma-Aldrich
Sodium hydroxide, anhydrous, free-flowing, Redi-Dri, reagent grade, ≥98%, pellets
Sigma-Aldrich
Sodium hydroxide, reagent grade, 97%, powder
Sigma-Aldrich
Sodium hydroxide solution, BioUltra, 10 M in H2O
Sigma-Aldrich
Sodium hydroxide, puriss. p.a., ACS reagent, reag. Ph. Eur., K ≤0.02%, ≥98%, pellets
Supelco
Ethylene glycol solution, 80% in DMSO-d6 (99.9 atom % D), NMR tube size 5 mm × 8 in.
Sigma-Aldrich
Ethylene, ≥99.5%
Sigma-Aldrich
3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%
Sigma-Aldrich
Sodium hydroxide, ultra dry, powder or crystals, 99.99% trace metals basis
Sigma-Aldrich
Sodium hydroxide solution, purum, ≥32%
Propylene glycol, European Pharmacopoeia (EP) Reference Standard
Supelco
2,3-Butanediol, analytical standard, mixture of racemic and meso forms
Sigma-Aldrich
Ethylene glycol, anhydrous, 99.8%
Sigma-Aldrich
1,2-Butanediol, 98%
Sigma-Aldrich
1,2-Butanediol, purum, ≥98.0% (GC)
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (v/v) trifluoroacetic acid
Sigma-Aldrich
Ethylene, 99.99%
Sigma-Aldrich
Acetonitrile solution, contains 10.0% acetone, 0.05% formic acid, 40.0% 2-propanol
Supelco
Diethylene glycol, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Ethylene glycol, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (w/v) ammonium formate, 5 % (v/v) water, 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
2,3-Butanediol, 98%