Development and validation of a HS/GC–MS method for the simultaneous analysis of diacetyl and acetylpropionyl in electronic cigarette refills

Barhdadi, Sophia; Canfyn, Michaël; Courselle, P.; Rogiers, Vera; Vanhaecke, Tamara; Deconinck, Éric

doi:10.1016/j.jpba.2017.04.050

Cited by 21 publications

(16 citation statements)

References 16 publications

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“…In reaction to this, a prompt response came from e-liquids manufacturers with the replacement of diacetyl with 2,3-pentanedione (acetylpropionyl), an α-diketone showing similar flavor properties, but this option was soon revealed to be unsuccessful when scientific data on acetylpropionyl toxicity started to be published [56]. Our findings, although related to a limited number of samples, are in line with the results obtained in previous investigations highlighting the presence of diacetyl in e-liquids commercially available in EU member states in the pre-TPD implementation period and with characteristic flavors appealing to teenagers and young adults [19,20,30]. Farsalinos et al, 2015 analyzed both liquid and aerosol matrices of a total number of 159 samples purchased from 36 manufacturers and retailers in 7 different countries.…”

Section: Discussion Of Flavoring Additives Resultssupporting

confidence: 86%

“…Similarly to Farsalinos et al, comparison with the NIOSH safety limit was made, revealing that one tobacco flavored e-liquid that resulted diacetyl-positive could lead to exposure higher the recommended limit. Although approximate for estimating risk for e-cig users, the use of occupational exposure limits is affected by several limitations [19,57]. This approach has raised some resistance, mainly because occupational safety limits for toxicants, for instance for diacetyl, have been set for workers not for the general population and are related to inhalation exposure scenarios not applicable to e-cigs users.…”

Section: Discussion Of Flavoring Additives Resultsmentioning

confidence: 99%

“…It is a chemical mentioned in the GRAS list and approved in certain limits for ingestion, therefore it is used as additive in foods [18]. Due to its flavoring properties it is also used in the manufacturing process of e-liquid formulations and its presence has been documented in previous investigations carried out in EU Member States, raising concerns in the scientific community regarding potential health implications [19,20]. In this regard, recently published scientific papers based on epidemiological data collected over recent decades have revealed that inhalation exposure to diacetyl is likely related to increased risk of a specific lung disease called bronchiolitis obliterans [21,22].…”

Section: Flavoring Additivesmentioning

confidence: 99%

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Chemical Characterization of Electronic Cigarette (e-cigs) Refill Liquids Prior to EU Tobacco Product Directive Adoption: Evaluation of BTEX Contamination by HS-SPME-GC-MS and Identification of Flavoring Additives by GC-MS-O

et al. 2020

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The present study focused on the determination of benzene, toluene, ethylbenzene and xylenes (BTEX) concentration levels in 97 refill liquids for e-cigs selected by the Italian National Institute of Health as representative of the EU market between 2013 and 2015 prior to the implementation of the European Union (EU) Tobacco Product Directive (TPD). Most of the e-liquids investigated (85/97) were affected by BTEX contamination, with few exceptions observed (levels below the limit of quantification (LOQ) of headspace-solid phase micro extraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) methodology). Across brands, concentration levels ranged from 2.7 to 30,200.0 µg/L for benzene, from 1.9 to 447.8 µg/L for ethylbenzene, from 1.9 to 1,648.4 µg/L for toluene and from 1.7 to 574.2 µg/L for m,p,o-xylenes. The variability observed in BTEX levels is likely to be related to the variability in contamination level of both propylene glycol and glycerol and flavoring additives included. No correlation was found with nicotine content. Moreover, on a limited number of e-liquids, gas chromatography-mass spectrometry-olfactometry (GC-MS-O) analysis was performed, allowing the identification of key flavoring additives responsible of specific flavor notes. Among them, diacetyl is a flavoring additive of concern for potential toxicity when directly inhaled into human airways. The data reported are eligible to be included in the pre-TPD database and may represent a reference for the ongoing evaluation on e-liquids safety and quality under the current EU Legislation.

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Section: Discussion Of Flavoring Additives Resultssupporting

confidence: 86%

Section: Discussion Of Flavoring Additives Resultsmentioning

confidence: 99%

Section: Flavoring Additivesmentioning

confidence: 99%

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Chemical Characterization of Electronic Cigarette (e-cigs) Refill Liquids Prior to EU Tobacco Product Directive Adoption: Evaluation of BTEX Contamination by HS-SPME-GC-MS and Identification of Flavoring Additives by GC-MS-O

et al. 2020

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“…In one of these procedures (8), a method of the Cooperation Centre for Scientific Research Relative to Tobacco (CORESTA) used for other carbonyl compounds analysis (9) has been expanded to include diacetyl and acetylpropionyl. More recently, the evaluation of diacetyl and acetylpropionyl in e-vapor products became of interest (10,11), and several presentations were made at Tobacco Science Research Conferences (TSRC) (12,13) regarding this topic.…”

mentioning

confidence: 99%

“…The measurements (for diacetyl) were performed on various matrices such as wine (14), beer (15), food (16), urine (17), and environmental air (18). Related to the analysis of diacetyl in e-liquids and tobacco products, the procedures for analysis can be based on gas chromatography followed by mass spectrometry (MS) (11)(12)(13), or on high performance liquid chromatography (HPLC) (9). The HPLC procedure recommended by CORESTA is based on derivatization with dinitrophenylhydrazine and UV detection (8,9).…”

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confidence: 99%

The Determination of Diacetyl and Acetylpropionyl in Aerosols From Electronic Smoking Devices Using Gas Chromatography Triple Quad Mass Spectrometry

Moldoveanu

Hudson

Harrison

2017

Beiträge Zur Tabakforschung International/Contributions to Tobacco Research

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SUMMARYA reliable and sensitive method for the measurement of the level of diacetyl (2,3-butanedione) and acetylpropionyl (2,3-pentanedione) in the aerosol (both the particles and the suspending gas) of electronic smoking devices (e-cigarettes) has been developed. The method uses a gas chromatographic separation on a Carbowax type column with the measurement of the analytes on a triplequadrupole mass spectrometer working in positive MRM mode. The method has been validated using standard requirements regarding selectivity, sensitivity, recovery, accuracy, and repeatability. The limit of quantitation (LOQ) for the method was determined to be 0.41 ng/mL for diacetyl and 0.21 ng/mL for acetylpropionyl as measured for standards. These values translate to an LOQ of 0.082 ng/puff for diacetyl and 0.042 ng/puff for acetylpropionyl as measured for an e-cigarette with 50 puffs placed in 10 mL acetone. The samples analyzed included collected aerosols from several e-cigarettes, and a number of liquids used in electronic cigarettes (e-liquids). 3R4F Kentucky reference cigarette was also analyzed for evaluating the accuracy of the procedure, with good agreement with data from the literature. Diacetyl and acetylpropionyl were distributed in both particulate phase and also in vapor phase. The levels of diacetyl and acetylpropionyl in particulate phase collected from 3R4F cigarettes were found to represent only about 22% for diacetyl and only 31% for acetylpropionyl, while the vapor phase for diacetyl represented 78% and for acetylpropionyl 69% of the total analyte. The levels of diacetyl and acetylpropionyl in the aerosols of most electronic smoking devices were found to be very low, with a few exceptions. The analysis of the two analytes in several e-liquids available on the market showed a very large range of levels. Some of the e-liquids from the market are likely to have diacetyl and/or acetylpropionyl intentionally added. [Beitr. Tabakforsch. Int. 27 (2017) RESUMEUne méthode sensible et fiable fut mise au point afin de mesurer le niveau de diacétyle (butane-2,3-dione) et d'acétylpropionyle (pentane-2,3-dione) présent dans l'aérosol (tant parmi les particules que dans le gaz de suspension) contenu dans les cigarettes électroniques (vapoteuses). La méthode s'appuya sur une séparation par chromatographie gazeuse sur une colonne de type Carbowax, accompagnée de la mesure des analytes sur un spectromètre de masse de type triple quadripôle en mode MRM positif. La méthode fut validée sur la base des normes habituelles concernant la sélectivité, la sensibilité, la récupération, la précision et la répétabilité. La limite de quantification (LOQ) de la méthode fut définie à 0.4 ng/mL pour le diacétyle et à 0.21 ng/mL pour l'acétylpropionyle, telle que mesurée pour les étalons. Ces valeurs se traduisirent par une LOQ de 0.082 ng/bouffée de diacétyle et 0.042 ng/bouffée pour l'acétylpropionyle, telles que mesurées pour une cigarette électronique de 50 bouffées placées dans 10 mL d'acétone. Les échantillons analysés inclurent des aé...

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Profiling flavourings in strawberry‐flavoured e‐liquid using headspace‐gas chromatography–mass spectrometry

Haworth-Duff

Parkes

Reed

2023

Drug Testing and Analysis

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E‐liquids typically contain nicotine and flavourings in a matrix of propylene glycol (PG) and vegetable glycerine (VG). Some nicotine‐free e‐liquids are flavouring only in the aerosol carrier with the option for users to add their own nicotine. It is only the nicotine that is monitored in terms of level, as specified by the manufacturers. Little is known of the toxicological effect for some of the flavourings in the context of vaping as these are only regulated for ingestion and not inhalation. A method was developed to analyse volatile organic compounds (VOCs) evolved when e‐liquids are vaporised based on headspace‐gas chromatography–mass spectrometry (HS‐GC‐MS) for e‐liquids. An in‐house standard was prepared with sample matrix and purchased strawberry flavouring to simulate a simple e‐liquid but with known levels. This standard was then used to optimise the analysis for use with e‐liquid samples but not for full quantification purposes. These were purchased from a range of retailers and with different batches but mainly focussed on strawberry flavour. The results identified three key components indicative of strawberry flavour (ethyl‐3‐methyl butanoate, ethyl 2‐methyl butanoate and ethyl butanoate) and showed considerable variation between both manufacturers and batches. Flavouring VOCs are regulated for ingestion but are not regulated for e‐liquid inhalation, so these could have toxicological implications. In addition, the inconsistency between samples suggests further issues when users add their own nicotine to the e‐liquids as the viscous sample matrix makes homogeneous mixing difficult.

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Development and validation of a HS/GC–MS method for the simultaneous analysis of diacetyl and acetylpropionyl in electronic cigarette refills

Cited by 21 publications

References 16 publications

Chemical Characterization of Electronic Cigarette (e-cigs) Refill Liquids Prior to EU Tobacco Product Directive Adoption: Evaluation of BTEX Contamination by HS-SPME-GC-MS and Identification of Flavoring Additives by GC-MS-O

Chemical Characterization of Electronic Cigarette (e-cigs) Refill Liquids Prior to EU Tobacco Product Directive Adoption: Evaluation of BTEX Contamination by HS-SPME-GC-MS and Identification of Flavoring Additives by GC-MS-O

The Determination of Diacetyl and Acetylpropionyl in Aerosols From Electronic Smoking Devices Using Gas Chromatography Triple Quad Mass Spectrometry

Profiling flavourings in strawberry‐flavoured e‐liquid using headspace‐gas chromatography–mass spectrometry

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