Comprehensive determination of flavouring additives and nicotine in e-cigarette refill solutions. Part I: Liquid chromatography-tandem mass spectrometry analysis

Aszyk, Justyna; Kubica, Paweł; Kot‐Wasik, Agata; Namieśnik, Jacek; Wasik, Andrzej

doi:10.1016/j.chroma.2017.08.056

Cited by 37 publications

(25 citation statements)

References 18 publications

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“…In published studies, concentrations of ethyl maltol in vaping liquids range between undetectable to 4,200 μg/ml ( Aszyk et al, 2017 ; Behar et al, 2018 ), compared to average maximum concentration ranges of 12.4–152 μg/ml in non-alcoholic beverages and baked goods, respectively, on which Flavor Extract Manufacturers Association ( FEMA, The Flavor and Extract Manufacturers Association of the United States, 2021 ) Expert Panel based its’ judgments that this substance is safe for ingestion ( Oser and Ford 1977 ). Although generally recognized as safe for ingestion, the health effects of ethyl maltol, and more broadly the majority of flavour compounds, have not been assessed for the inhalation route ( Flavor and Extract Manufacturers Association, 2021 ).…”

Section: Resultsmentioning

confidence: 99%

Open Characterization of Vaping Liquids in Canada: Chemical Profiles and Trends

et al. 2021

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Currently, there is a lack of comprehensive data on the diversity of chemicals present in vaping liquids. To address this gap, a non-targeted analysis of 825 vaping liquids collected between 2017 and 2019 from Canadian retailers was conducted. Prior to mass spectrometry analysis, samples were diluted 1:500 v/v with methanol or acetonitrile. Chemical compound separation and analysis was carried out using gas chromatography and triple quadrupole mass spectrometry (GC-MS/MS) systems operated in the full scan mode and mass range of 35–450 m/z. Mass spectrum for each sample was obtained in electron ionization at 70 eV and processed. Non-targeted identification workflow included use of automated mass spectral deconvolution and identification system (AMDIS), where required, as well as a number of commercially available spectral libraries. In order to validate identities, an in-house database of expected compounds previously detected in vaping liquids was used along with genuine analytical standards for compounds of interest. This resulted in a dataset of over 1,500 unique detected chemicals. Approximately half of these chemical compounds were detected only once in a single product and not in multiple products analyzed. For any sample analyzed, on average, 40% of the chemical constituents appeared to have flavouring properties. The remainder were nicotine and related alkaloids, processing, degradation or indirect additives, natural extractives and compounds with unknown roles. Data published here from the project on the Open Characterization of vaping liquids is unique as it offers a detailed understanding of products’ flavour chemical profiles, the presence and frequency of chemicals of potential health concern, as well as trends and changes in products’ chemical complexity over a three-year period. Non-targeted chemical surveillance such as this present valuable tools to public health officials and researchers in responding to emergent issues such as vaping associated lung injury or informing chemical based strategies which may be aimed at addressing product safety or appeal.

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Section: Resultsmentioning

confidence: 99%

Open Characterization of Vaping Liquids in Canada: Chemical Profiles and Trends

et al. 2021

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“…Considering the addictive nature of nicotine, e-liquids need to be regulated for the total nicotine content as well as free base nicotine yield. ere are published methods for determining total nicotine content in e-liquids using gas chromatography and liquid chromatography coupled with mass detectors [27][28][29]. Recently, we have proposed a HPLC method based on peak purity criteria for accurate quantification of total nicotine content [19].…”

Section: Discussionmentioning

confidence: 99%

An Analytical Perspective on Determination of Free Base Nicotine in E-Liquids

Gholap

Heyder

Kośmider

et al. 2020

Journal of Analytical Methods in Chemistry

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In electronic cigarette users, nicotine delivery to lungs depends on various factors. One of the important factors is e-liquid nicotine concentration. Nicotine concentration in e-liquids ranges from 0 to >50 mg/mL. Furthermore, nicotine exists in protonated and unprotonated (“free base”) forms. The two forms are believed to affect the nicotine absorption in body. Therefore, in addition to total nicotine concentration, e-liquids should be characterized for their free base nicotine yield. Two approaches are being used for the determination of free base nicotine in e-liquids. The first is applying a dilution to e-liquids followed by two methods: Henderson–Hasselbalch theory application or a Liquid-Liquid Extraction. The second is the without-dilution approach followed by 1H NMR method. Here, we carried out controlled experiments using five e-liquids of different flavors using these two approaches. In the dilution approach, the Henderson–Hasselbalch method was tested using potentiometric titration. The accuracy was found to be >98% for all five e-liquid samples (n = 3). A Liquid-Liquid Extraction was carried out using toluene or hexane as extraction solvent. The Liquid-Liquid Extraction technique was found to be limited by solvent interactions with flavors. Solvent extractions resulted in flavor dependent inaccuracies in free base nicotine determination (5 to 277% of calculated values). The without-dilution approach was carried out using 1H NMR as described by Duell et al. This approach is proposed to offer an independent and alternative scale. None of the methods have established a strong correlation between pre- and postvaporization free base nicotine yield. Here we present comparative results of two approaches using analytical techniques. Such a comparison would be helpful in establishing a standardized method for free base nicotine determination of e-liquids.

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“…All analyses were performed using an LC-MS-8060 triple quadrupole mass spectrometer (Shimadzu, Japan) equipped with an electrospray ionization source (ESI) working in positive multiple reaction mode (MRM). The parameters of the ion source were set as in Aszyk et al [27], while the optimization of MRM conditions was performed via an infusion of a 100 ng/mL solution of each substance by flow injection analysis (FIA). The MRM transitions were monitored only for specific detection time (± 1 min of t R of analyte) to increase sensitivity.…”

Section: Methodsmentioning

confidence: 99%

Stabilities of bisphenol A diglycidyl ether, bisphenol F diglycidyl ether, and their derivatives under controlled conditions analyzed using liquid chromatography coupled with tandem mass spectrometry

et al. 2019

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Bisphenol A diglycidyl ether (BADGE), bisphenol F diglycydyl ether (BFDGE), and their related compounds are widely used as precursors in production of epoxy resins. The high reactivity of these compounds makes the development of analytical methodologies that ensure appropriate metrological accuracy crucial. Consequently, we aimed to determine whether and to what extent the composition of the solution and storage conditions affect the stability of selected BADGE and BFDGE derivatives. The stabilities of these compounds were studied using liquid chromatography–tandem mass spectrometry with electrospray ionization (HPLC-ESI–MS/MS). The chromatographic method elaborated here has allowed for separation of the analytes in time shorter than 6 min, for both methanol and acetonitrile-based mobile phases. The obtained calibration curves for all analytes were linear in the range tested. The values of limit of detection (LODs) were in the range of 0.91–2.7 ng/mL, while values of limit of quantitation (LOQs) were in the range of 2.7–5.7 ng/mL. The chosen experimental conditions were compared in terms of the content of organic solvent in solution, storage temperature, and time. Our results show that the content of BADGE, BADGE·HCl, BFDGE, three-ring NOGE decreased with increasing water content (> 40% v / v ). For BADGE and three-ring NOGE, significant changes in concentration were noted as early as 24 h after the test solutions had been prepared. In addition, a reduction in the storage temperature (4 to − 20 °C) reduced the rate of transformation of the monitored analytes. Our study will increase quality control in future research and may increase the reliability of the obtained results. Graphical abstract Electronic supplementary material The online version of this article (10.1007/s00216-019-02016-5) contains supplementary material, which is available to authorized users.

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Comprehensive determination of flavouring additives and nicotine in e-cigarette refill solutions. Part I: Liquid chromatography-tandem mass spectrometry analysis

Cited by 37 publications

References 18 publications

Open Characterization of Vaping Liquids in Canada: Chemical Profiles and Trends

Open Characterization of Vaping Liquids in Canada: Chemical Profiles and Trends

An Analytical Perspective on Determination of Free Base Nicotine in E-Liquids

Stabilities of bisphenol A diglycidyl ether, bisphenol F diglycidyl ether, and their derivatives under controlled conditions analyzed using liquid chromatography coupled with tandem mass spectrometry

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