Abstract
We developed a quantitative method for analyzing nicotine and menthol in e-cigarette, or vaping, products (EVPs). These products may adversely impact health through inhalational exposure to addictive and harmful chemicals. The presence of unknown substances in do-it-yourself e-liquids, counterfeits, or unregulated products may increase exposure to harmful chemicals, as underscored by the 2019 EVP use-associated lung injury (EVALI) outbreak. To minimize these risks, it is important to accurately quantify nicotine and menthol in e-liquids and aerosol emissions to evaluate EVP authenticity, verify product label accuracy, and identify potentially hazardous products. We developed a simple, versatile, high-throughput method using isotope-dilution gas chromatography-mass spectrometry for quantifying nicotine and menthol concentrations in both e-liquid contents and machine-generated aerosol emissions of EVPs. Rigorous validation has demonstrated that the method is specific, precise (CV<2.71%), accurate (percent error ≤7.0%), and robust. Linear calibration ranges from 0.01 to 1.00 mg/ml for both analytes was achieved, corresponding to expected analyte levels in e-liquids and machine-generated EVP aerosols. Limits of detection (LODs) in the final 10-ml sample extract were 0.4 μg/ml for nicotine and 0.2 μg/ml for menthol. The method was used to analyze aerosol emissions of 141 EVPs associated with the 2019 EVALI outbreak; detectable levels of nicotine (2.19–59.5 mg/g of aerosol) and menthol (1.09–10.69 mg/g of aerosol) were observed in 28 and 11%, respectively, of the samples analyzed. Nicotine was not detected in any of the tetrahydrocannabinol (THC), cannabidiol (CBD), or oil-based products, while menthol (2.95 mg/g of aerosol) was only detected in one of these products (THC-labeled). The analytical method can be used to quantify nicotine and menthol concentrations in the e-liquids and aerosols from a range of EVPs, and these findings highlight a difference between e-cigarette and other vaping products.
Highlights
E-cigarette, or vaping, product (EVP) use has increased substantially in the United States over the last few years, both for traditional atomizer/cartomizer e-cigarettes designed to deliver nicotine (Wang et al, 2020) and for more recent ceramic-cell vape products designed to deliver cannabinoids (Knapp et al, 2019)
Validation, and application of a new, simple, sensitive, high-throughput, and selective isotope-dilution gas chromatography-mass spectrometry (ID-GC-MS) method for the simultaneous quantitation and characterization of nicotine and menthol in e-liquids and machine-generated aerosol emissions of EVPs
total particulate matter (TPM) deliveries and nicotine/menthol concentrations vary from product-to-product, resulting in variable aerosol LODs that are based on product analyte concentrations and their respective deliveries
Summary
E-cigarette, or vaping, product (EVP) use has increased substantially in the United States over the last few years, both for traditional atomizer/cartomizer e-cigarettes designed to deliver nicotine (Wang et al, 2020) and for more recent ceramic-cell vape products designed to deliver cannabinoids (Knapp et al, 2019). Various methods have been described to measure nicotine concentrations in traditional atomizer/ cartomizer devices and in hydrophilic solvents such as propylene glycol (PG) and glycerol (GLY) (Trehy et al, 2011; Goniewicz et al, 2013; Famele et al, 2015; Lisko et al, 2015; Ogunwale et al, 2017; Gholap et al, 2018; Reilly et al, 2020) These existing methods have not been validated for measuring nicotine and menthol in hydrophobic, oil-based liquids and aerosols that can result from DIY mixing of ingredients and from using different types of liquids in the same device. This is the first report of these analytes quantitatively measured in samples from the EVALI response
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