Determination of glycerol in oils and fats using liquid chromatography chloride attachment electrospray ionization mass spectrometry

- Selective method for the quantitative analysis of glycerol.
- Chloride anion attachment as ionization mechanism.
- Stable isotope labelled internal standard used for signal normalization.
- Method validation is presented.

Existing liquid chromatography - mass spectrometry method for the analysis of short chain carboxylic acids was expanded and validated to cover also the measurement of glycerol from oils and fats. The method employs chloride anion attachment and two ions, [glycerol +35Cl]− and [glycerol +37Cl]−, as alternative quantifiers for improved selectivity of glycerol measurement. The averaged within run precision, between run precision and accuracy ranged between 0.3 − 7%, 0.4 − 6% and 94 − 99%, respectively, depending on the analyte ion and sample matrix. Selected renewable diesel feedstocks were analyzed with the method.