Nicotine-related impurities in e-cigarette cartridges and refill e-liquids

Flora, Jason W.; Wilkinson, Celeste T.; Sink, Kathleen M.; McKinney, Diana L.; Miller, John H.

doi:10.1080/10826076.2016.1266500

Cited by 22 publications

(31 citation statements)

References 10 publications

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“…e conditions of storage and conservation are also incriminated and can also be responsible for many unknown impurities. A recent study has shown that nicotine impurities increase under long-term storage conditions especially n-nicotine, cotinine, myosmine, and nornicotine [29].…”

Section: Resultsmentioning

confidence: 99%

E-Cigarette Quality Control: Impurity and Nicotine Level Analysis in Electronic Cigarette Refill Liquids

Bennani¹,

Chentoufi²,

Karbane³

et al. 2020

The Scientific World Journal

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This work targets mainly the quality control of electronic cigarette liquids. It relies on an analytical control of a “32-product” sample made of several types of e-cigarette liquids taken from various supermarkets and tobacconist’s offices in Morocco. All along this study, we made sure to check both the conformity of the nicotine level indicated in the packaging of each product and the existence of any other components inside the product, especially toxic or unknown impurities. The method used for this study is known under the name of high-performance liquid chromatography. For statistical analysis, we used Student’s t-test for a single sample in order to analyze the relative differences between nicotine quantity reported in the product and the one measured during our experiment. Finally, we used linear regression test to determine the relationship between the nicotine level accuracy on the packaging and the level of toxic impurities in the products. The differences between the nicotine concentrations reported in the packages and the measured ones varied from −100% to +3.3%. The study showed that 31% of analyzed products have an accurate indication of the level of nicotine on the packaging. However, 47% of the studied products showed more than 20% difference between measure and packaging indication. In all analyzed samples, the level of impurities altered from 0 to 32.6%. Furthermore, the level of the nicotine breakdown products did not exceed 2% of the nicotine content in pretty much all of the samples. The actual nicotine content of electronic cigarette refill liquids is not always as precise as what is stated on the packaging; in addition to the level of impurities detected in several brands and that exceeds the European Pharmacopoeia standards, some may even present a risk of causing toxicological damage.

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Section: Resultsmentioning

confidence: 99%

E-Cigarette Quality Control: Impurity and Nicotine Level Analysis in Electronic Cigarette Refill Liquids

Bennani¹,

Chentoufi²,

Karbane³

et al. 2020

The Scientific World Journal

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“…As shown in Figure 4, after two months, anatabine, anabasine and β-nicotyrine were immeasurable while the yields of cotinine, nornicotine and myosmine, which are usually indicators of the thermal decomposition of nicotine (30)(31)(32), did not show noticeable changes. However, the yields of nicotine-N-oxide, which is the primary oxidation product of nicotine (25), increased quickly, especially under 40 °C / RH 75% storage condition. This experiment suggests that quantifying the yields of nicotine degradation products is an effective way to discern an unstable formulation.…”

Section: Stability Of Nicotine In Highly Flavored E-cigarette Productsmentioning

confidence: 99%

“…Pharmaceutical products are required to be comprehensively evaluated in rigorous stability studies to provide proof on how the quality, safety, and effectiveness of the drug products change with time under the influence of a variety of environmental factors such as temperature, humidity, and light (25,26). The stability studies, including real-time and accelerated tests, have been used to investigate the potential degradation products and impurities that originate from exposure and interaction with excipients, a specific container / closure system, and to ensure that the products retain their fitness for use up to the end of their expiration dates.…”

Section: Stability Of Nicotine In E-cigarette Products Under Various mentioning

confidence: 99%

Analysis of Nicotine and Nicotine-Related Compounds in Electronic Cigarette Liquids and Aerosols by Liquid Chromatography-Tandem Mass Spectrometry

Liu¹,

Joza²,

Rickert³

2017

Beiträge Zur Tabakforschung International/Contributions to Tobacco Research

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SUMMARYThe objective of this study was to develop and validate an analytical method for determining nicotine and nicotine related compounds (i.e., nicotine-N-oxide, cotinine, nornicotine, anatabine, myosmine, anabasine, and β-nicotyrine) in e-cigarette aerosols and e-liquids. Aerosol collection was achieved using a Cambridge collection pad. The sample preparation consisted of adding deuterated internal standards to the collection pad and extracting with 100 mM ammonium acetate solution using a wrist-action shaker. The filtrate was then analyzed by LC-MS/MS using a Gemini NX C 18 column (3 µm, 150 × 3 mm) with a mobile phase gradient system consisting of acetonitrile and 10% acetonitrile in 10 mM ammonium bicarbonate (pH = 8.0) and electrospray ionization (ESI) in the positive mode. The e-liquid was analyzed using the same instrumental parameters, but simplifying the sample preparation procedure by adding deuterated internal standards directly to the 100-mg sample. The sample was then extracted with 100 mM ammonium acetate solution, sonicated, and filtered. In this study, the method's accuracy, robustness, and reliability were enhanced by using deuterated analogues of each compound as internal standards and by applying two ion-transition pairs for each compound for the confirmation and quantification. Validation experiments demonstrated good sensitivity, specificity and reproducibility. All the target compound calibrations exhibited satisfactory linearity from 0.050 to 5.0 mg/mL (r 2 > 0.995). The average recoveries for e-liquids varied from 85.2%(nicotine-N-oxide) to 110% (β-nicotyrine) with recoveries for all compounds exhibiting a coefficient of variation (CV) < 5.0%. Similarly, the average recoveries for e-cigarette aerosols varied from 87.8% (for nicotine-N-oxide) to 111% (for myosmine) with all CV < 8.8%. The LOD and LOQ for e-liquids for all target compounds ranged from 0.234 and 0.781 μg/g (cotinine) to 1.66 and 5.48 μg/g (nicotine-Noxide). For e-cigarette aerosols these limits ranged from 0.094 and 0.312 μg/collection (cotinine) to 0.872 and 2.87 μg/collection (nicotine-N-oxide). This methodology was used to quantitatively determine if any of the target compounds were present in a variety of sample matrices, including e-cigarette solutions and aerosols, and was successfully applied to stability studies, to monitor changes in the target compound levels which might be caused by e-cigarette formulations, components and the storage conditions. [Beitr. Tabakforsch. Int. 27 (2017)

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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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Nicotine-related impurities in e-cigarette cartridges and refill e-liquids

Cited by 22 publications

References 10 publications

E-Cigarette Quality Control: Impurity and Nicotine Level Analysis in Electronic Cigarette Refill Liquids

E-Cigarette Quality Control: Impurity and Nicotine Level Analysis in Electronic Cigarette Refill Liquids

Analysis of Nicotine and Nicotine-Related Compounds in Electronic Cigarette Liquids and Aerosols by Liquid Chromatography-Tandem Mass Spectrometry

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

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