Quantification of dimethylamine in low concentration particulate matter by reducing the concentration of 9-fluorenylmethyl chloroformate

Abstract

This study presents a refined method that uses liquid chromatography with a fluorescence detector (LC-FD) to quantify trace amounts of dimethylamine in particulate matter (PM). This method was optimized to prioritize simplicity, cost-effectiveness and practicality. To ensure accurate and reliable analysis, strict protocols and procedures were followed to minimize cross-contamination. Separate workspaces were designated for preparing control blanks and sample treatments in one area and standard solutions in another, thus mitigating the risk of cross-contamination. An evaluation was conducted on different concentrations of 9-fluorenylmethyl chloroformate to derivatize dimethylamine. The results showed that a concentration of 3 μg mL⁻¹ was effective in derivatizing dimethylamine concentrations up to 300 ng mL⁻¹. Increasing the concentration of the derivatization reagent from 2.9 to 7.3 μg mL⁻¹ resulted in slightly elevated dimethylamine levels in blank measurements. Also, during the preparation of standards at low concentrations, high analytical coefficients of variation were observed. This highlights the importance of checking for potential sources of contamination. Method precision and quantification limits were evaluated through blank analysis, yielding values of approximately 20% and 20 ng mL⁻¹, respectively, consistent with chromatographic determination for environmental analysis. The suitability of the method for environmental analysis was demonstrated by analyzing eight PM_2.5 samples. The concentrations of methylamine and dimethylamine were found to range from 0.8 to 3 ng m⁻³ and 1.4 to 7.1 ng m⁻³, respectively, in accordance with the literature. Comparison with concurrent carbonyl measurements revealed similar concentration profiles. Both types of analyses can be performed using affordable methodologies that involve prior derivatization using a reduced concentration of the derivatization reagent.