Abstract
Emerging chemicals of concern (ECCs), including phthalate plasticizers, flame retardants, and phenolic compounds, are likely present in electronic nicotine delivery system (ENDS) replacement solutions (e-liquids) which are often packaged, stored in, and/or can contact with, plastic, glass, and metal materials. Developing and validating an efficient analytical method for concurrent quantification of ECCs in e-liquids are thus needed to inform evidence-based safety evaluation of ENDS products. In this study, we developed and validated a “dilute-and-shoot” method using high-performance liquid chromatography coupled with tandem mass spectrometry to simultaneously measure organophosphate flame retardants (OPFRs), phthalate plasticizers, and tetrabromobisphenol A (TBBPA) in e-liquids. We analyzed samples in positive electrospray ionization mode (ESI+) for OPFRs and phthalates and negative ESI– for TBBPA. The method has a total runtime of 10 min. The optimized procedure was able to deliver broad dynamic linearity ranges with coefficients of determination (R2) above 0.995, limits of detection ranging from 0.020 to 10 ng/mL, average accuracy within ±15%, and imprecision ≤ 15.0% for all analytes. To our knowledge, this is the first multianalysis method for measuring ECCs in e-liquid samples, and the validation results show that it is sensitive, accurate, precise, and efficient.
Highlights
Electronic cigarettes are engineered to heat a liquid solutionCO, and metals.[13−17]For this, investigation of the types and concentrations of Emerging chemicals of concern (ECCs) in e-liquids is needed to provide scientific data for a better evaluation of the safety of the electronic nicotine delivery system (ENDS) products
To differentiate the potential carryover from the system background residual levels, multiple samples containing highpurity methanol and water were injected and analyzed prior to analyzing the samples with high concentration levels. In this assay, when the samples were diluted by 10 times, we did not identify the background residual levels for TEP, TPrP, tris(2chloroethyl)phosphate (TCEP), dihexyl phthalate (DHP), tris(2,3-dibromopropyl)phosphate (TDBPP), dimethyl phthalate (DMP), diamyl phthalate (DAP), resorcinol bis(diphenyl phosphate) (RDP), TDBPP, and tetrabromobisphenol A (TBBPA)
Most of organophosphate flame retardants (OPFRs) and phthalates are lipophilic compounds, their polarity and solubility vary in broad ranges, resulting in a wide retention ability on SPEs
Summary
Electronic cigarettes are engineered to heat a liquid solutionCO, and metals.[13−17]For this, investigation of the types and concentrations of ECCs in e-liquids is needed to provide scientific data for a better evaluation of the safety of the ENDS products. Shin developed a method for measuring diethyl phthalate (DEP) and diethylhexyl phthalate (DEHP) in replacement liquid.[18] Several other phthalates of interest were not included in their method This method employed liquid−liquid extraction which is relatively time-consuming and required a volume of 0.5 mL for sample preparation to achieve the lowest limits of detection (LODs) that were 0.003 and 0.004 μg/mL for DEP and DEHP, respectively. To differentiate the potential carryover from the system background residual levels, multiple samples containing highpurity methanol and water were injected and analyzed prior to analyzing the samples with high concentration levels. “Cost-effectiveness” is usually a factor that needs to be considered when developing analytical assays which have a high-frequency application potential
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