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A New Gas Chromatography–Mass Spectrometry Method for Detecting and Quantifying Low Levels of Dimethyl Sulfate in Palm Oil‐Based Sulfonated Methyl Esters
Author(s) -
Ping Bonnie Tay Yen,
Aziz Haliza Abdul
Publication year - 2019
Publication title -
journal of surfactants and detergents
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.349
H-Index - 48
eISSN - 1558-9293
pISSN - 1097-3958
DOI - 10.1002/jsde.12269
Subject(s) - chemistry , chromatography , repeatability , palm oil , hexane , reproducibility , mass spectrometry , detection limit , gas chromatography–mass spectrometry , gas chromatography , selected ion monitoring , analytical chemistry (journal) , food science
Dimethyl sulfate (DMS) is a potential carcinogen that may be formed during the production of α‐sulfonated methyl ester (α‐SME). To date, there have been no published analytical methods for quantification of DMS in palm oil‐based α‐SME. The objective of the method development was to establish a simple and reliable method for quantifying and monitoring DMS from palm oil‐based α‐SME. The sample preparation prior to analysis involved extracting DMS from α‐SME using hexane. The gas chromatography–mass spectrometry (GC–MS) separation was performed on an Agilent MS‐HP5 column (30 m × 320 μm × 0.25 μm). The MS signal was obtained in the selected ion monitoring (SIM) mode. The method was validated according to the International Conference on Harmonization (ICH) guidelines. The accuracy of the method was measured via percentage recoveries of DMS from spiked α‐SME samples at spiking levels of (25, 125, 250, and 500) μg mL −1 . The percentage recoveries for all spiking levels were found to be in the range of 88.6–97.4%. The repeatability and interday reproducibility were found to be satisfactory as the relative standard deviations (RSD) were within 11%. The method also has a good linear relationship as indicated by the coefficient of determination of 0.9996 over the range of 1.0–30 μg mL −1 . The limits of detection (LOD) and quantification (LOQ) corresponded to 0.8 and 2.3 μg mL −1 , respectively. The developed method demonstrated sufficient linearity, intraday and interday precision, sensitivity, and accuracy for determination of DMS in palm oil‐based α‐SME.