title: Development and validation of an automated static headspace gas chromatography-mass spectrometry (SHS-GC-MS) method for monitoring the formation of ethyl methane sulfonate from ethanol and methane sulfonic acid.
abstract: An automated sample preparation and analysis procedure was developed to monitor the formation of ethyl methane sulfonate from reaction mixtures containing ethanol and methane sulfonic acid. The system is based on a liquid handling robot combined with a static headspace module. The formed ethyl methane sulfonate is analysed after derivatisation with pentafluorothiophenol using static headspace-gas chromatography-mass spectrometry (SHS-GC-MS). Using the automated reaction-derivatisation-headspace GC-MS system, the formation of ethyl methane sulfonate can be monitored in different reaction mixtures under different reaction conditions, including temperature, water content and pH. Excellent linearity, repeatability and robustness were obtained, allowing the system to be used in kinetic studies.
authors.affiliation: Research Institute for Chromatography, Pres. Kennedypark 26, B-8500, Kortrijk, Belgium.
authors.forename: Karine
authors.initials: K
authors.lastname: Jacq
authors.forename: Ed
authors.initials: E
authors.lastname: Delaney
authors.forename: Andrew
authors.initials: A
authors.lastname: Teasdale
authors.forename: Steve
authors.initials: S
authors.lastname: Eyley
authors.forename: Karen
authors.initials: K
authors.lastname: Taylor-Worth
authors.forename: Andrew
authors.initials: A
authors.lastname: Lipczynski
authors.forename: Van D
authors.initials: VD
authors.lastname: Reif
authors.forename: David P
authors.initials: DP
authors.lastname: Elder
authors.forename: Kevin L
authors.initials: KL
authors.lastname: Facchine
authors.forename: Simon
authors.initials: S
authors.lastname: Golec
authors.forename: Rolf Schulte
authors.initials: RS
authors.lastname: Oestrich
authors.forename: Pat
authors.initials: P
authors.lastname: Sandra
authors.forename: Frank
authors.initials: F
authors.lastname: David
mesh_terms: D000431:Ethanol / Q000737:chemistry*; D005020:Ethyl Methanesulfonate / Q000138:chemical synthesis* / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D008698:Mesylates / Q000737:chemistry*; D015394:Molecular Structure; D012015:Reference Standards; D015203:Reproducibility of Results; D012371:Robotics / Q000379:methods; D013696:Temperature; D013997:Time Factors
chemical_list: D008698:Mesylates; C045880:methanesulfonic acid; D000431:Ethanol; D005020:Ethyl Methanesulfonate