Nicotine Assay of Titan Black Cartridges Medium Strength Tabacco
Report Number: F252A
Mike Ellicott
6th September 2010
LPD Lab Services Limited
D Building Philips Site,
Philips Road
Blackburn
Lancashire, BB1 5RZ
United Kingdom
www.lpdlabservices.co.ukenquiries@lpdlabservices.co.ukTel 01254-676 074
Fax 01254-278 845
Jason Cropper – Pillbox38 (UK) and (USA) Ltd
Unit 1 Brook Mill Complex
Branch Road
Lower Darwen
Lancashire BB3 0PR
This report shall not be reproduced except in full, without written approval of the laboratory
Description
One type of electronic cigarette ‘Cartridge’ was supplied to confirm the nicotine concentration found within the electronic cigarette ‘Cartridge’, and suggest a classification for the products under the current CHIP Regulations.
The product was as follows: -
• Titan Cartridges Medium Tabacco Strength (20 cigarettes) 14mg
The electronic cigarette which replicates the action of smoking, producing a tobacco aromatised smoke which when inhaled quickly delivers the nicotine to the lung.
The Electronic Cigarettes do not contain “Tobacco” as such, but are formulated using a refined tobacco leaf extract, where the extract used in manufacture may typically contain >= 95% Nicotine. The EC cartridges should therefore be exempt from the current Tobacco Legislation.
Nicotine is classified as a poison and is on the “Poisons List A”, however, there are “No special restrictions to any purchasing group”. It is therefore appropriate to deal with the electronic cigarettes under the CHIP Regulations.
An electronic cigarette ‘Cartridge’ was removed from a protective cellophane sachet ready to be dismantled. A small amount of liquid droplets were identified within the cellophane sachet presumably indicating some of the nicotine solution had leaked with time from the cartridge. The outside of the cartridge was wiped dry with tissues and the ‘Cartridge’ weighed before extraction of the nicotine solution.
The electronic cigarette ‘Cartridge’ was then dismantled by carefully removing the translucent rubber end cap, and then carefully pulling out the felt loaded with the nicotine solution using a pair of tweezers from the black plastic body of the cartridge.
Following extraction of the nicotine solution using the technique described in section 1 below, the cartridge components were dried at 100oC for 1 hour, cooled, and then reweighed. The weight of nicotine solution in the cartridge was thus calculated by difference.
The Nicotine Assay
1. Sample Extraction for GC Nicotine Assay - Cartridge
All equipment was washed at least three times with pure acetone then air dried before use; this included the 50 ml graduated flask, glass filter funnel with integral glass sintered support plate, and steel tweezers.
A single cartridge was slowly disassembled and each sub-component rinsed in turn with pure Propan-1-ol solvent, with all washing being collected using a glass funnel in a 50 ml graduated flask.
The nicotine solution was efficiently extracted from the ‘felt’ by careful washing with pure Propan-1-ol solvent 10 times, and subsequently collecting the washings in a 50 ml graduated flask and made up to the mark with pure Propan-1-ol. The flask was shaken 10 times to mix the contents prior to analysis.
2. Calibration of GC Nicotine Assay Method
A nicotine drug standard was obtained from Sigma-Aldrich with a concentration of 1.05 mg/ml of (-) Nicotine in methanol.
Part Number: N5511
Lot No: 077K5003
Concentration: 1.05 mg Nicotine/ ml
Expiration Date: December 2010
3. GC Nicotine Assay Method
The samples were analysed at LPD Lab Services Ltd to determine the nicotine concentration present by GC (Gas Chromatography).
Column: Heliflex AT-1 Dimethylpolysiloxane Capillary Column
– 30 m x 0.53 µm x 5 µm
Temperature: 150oC for 1 min, ramp 10oC/min to 250oC, 250oC for
19 min, 15 min equilibration
Analysis Time: 30min
Injection: Split less
Carrier gas: Helium
The GC method employed was of the ‘external standard type’ where the detector response for the nicotine component was calibrated based on peak area, after injecting a set volume of standard (0.5 µl). The detector response factor for Nicotine is evaluated and stored in the calibration file on the Chromatographic data processor.
The syringe used for injecting the samples was cleaned between samples using pure acetone.
Each ‘unknown’ sample is analysed by injecting an identical volume onto the GC system (0.5 µl as when calibrating) and the integrated peak area is used to calculate the nicotine content of the cartridge by applying the detector response factor and the dilution factor to the integrated peak area for nicotine.
Provided that the weight of the nicotine solution extracted from each cartridge is calculated, the nicotine content can be further expressed as either: -
• mg nicotine / cartridge, or mg nicotine / g nicotine solution
• or % w/w nicotine in the nicotine solution
4. GC Nicotine Assay Results
The nicotine standard was injected neat on to the GC system without any form of dilution. Each sample cartridge was subject to a dilution factor of fifty times prior to analysis.
Table 1 – Summary of GC nicotine Assay Data
Type Nicotine peak area Conc. mg nicotine
/ml Dilution Dilution Factor Conc. Of original Nicotine Solution
mg Nicotine
/cigarette cartridge Wt. Nicotine solution in cigarette cartridge
(g) Conc.
mg Nicotine/g of nicotine Solution % Nicotine in Nicotine Solution
(%)
1.05 mg/ml std 2068.004 1.05 N/A N/A N/A N/A N/A
Titan Cartridge 233.807 0.1187 50 5.9356 0.5675 10.4592 1.05
A detector response factor for nicotine of 0.5077 was used in the calculation of the concentration of nicotine in the dilution.
5. Discussion
The nicotine solution in the electronic cigarette ‘Cartridge’ has been investigated by LPD Lab Services Ltd, in order to confirm the quantity of nicotine currently found within the nicotine solution formulation, and suggest a classification of the preparation according to the hazards identified.
• The nicotine solution in the Titan Black Atomised Cartridge has been determined as 1.05%, and it is suggested that this cartridge should be classified as “Toxic”.
6. CHIP Regulations
The nicotine levels have been determined for each e-cigarette ‘Cartridge’, and the classification has been suggested below.
Suggested Classification: -
“Toxic” - for preparations containing nicotine at concentrations is >=1% but < 7%
For any product containing nicotine for use by the general public such as e-cigarettes, it is recommended that an ‘expert packaging company’ that has a full understanding of the current CHIP regulations and any possible forthcoming changes to regulations be consulted so that the e-cigarettes are packaged and labelled correctly for Trading Standards purposes prior to going on sale.
Such an ‘expert packaging company’ may be found at: -
www.chemsoft.co.uk or via
neil.smith@chemsoft.co.uk 7. References
a) Chemicals (Hazard Information and Packaging for Supply) Regulations 2009
Analysts Name: Mike Ellicott
Function:
Signature: (hard copy only)________________
End of Report
