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TSRC, Tob. Sci. Res. Conf., 2021, 74, abstr. 56 (also presented as presentation at CORESTA SSPT2021)

Determination of organic acids by GC-FID: on cartridge derivatization by silylating reagent (MTBSTFA)

PENNINGTON A.
Enthalpy Analytical, Durham, NC, USA

Organic acids are compounds that, when used in ENDS devices and e-liquids, can alter the perception and uptake of nicotine by the consumer. Traditional means of analysis by suppressed IC (Ion Chromatography) can lead to long runtimes in excess of 70 minutes and can contain coelutions or partial coelutions of some analytes, namely Lactic Acid and Levulinic Acid which coelute completely and Benzoic Acid, Malic Acid, and Succinic Acid which coelute partially. This may be overcome by the analysis of organic acids by GC-FID. By using a weak anion SPE (sample preparatory exchange) cartridge, the organic acids may be trapped and then undergo silylation derivatization with MTBSTFA (N-tert-Butyldimethylsilyl-N-methyltrifluoroacetamide) and eluted with acetonitrile. Standards prepared in the same fashion have shown to have quantitative recovery from the cartridge that has allowed for a production of a quadratic curve from 0.4 µg/mL to 1000 µg/mL with recoveries of 90 to 115% for all compounds. By performing the derivatized analysis by GC-FID, coeluting compounds in IC are completely resolved, analytical runtime is decreased to 25 minutes, and comparable method detection limits to that of IC are maintained. Notably, the method detection limits for the 15 organic acids analyzed were between 0.02 µg/mL and 0.08 µg/mL. This process eliminated the need for multiple dilutions in order to analyze effectively the levels of organic acids in percent level nicotine salt e-liquids and vapor. Derivatitzation and GC-FID analysis has added the benefit of a reduced runtime as well as provided resolution to coelution of known compounds.