Validation of an online, real time, soft photon ionisation (SPI) time of flight mass spectrometer for mainstream tobacco smoke analysis
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1 European Aerosol Conference Prague, September 2013 Session :Instrumentation 1 Validation of an online, real time, soft photon ionisation (SPI) time of flight mass spectrometer for mainstream tobacco smoke analysis 1
2 Jenni Hawke 1 and Matthias Bente von Frowein 2 1. British American Tobacco, Group R&D Centre, Southampton SO15 8TL, United Kingdom 2. Photonion GmbH, Hagenower Str. 73, Schwein, Germany 2
3 Introduction Tobacco smoke Tobacco smoke generated by combination of combustion, pyrolysis and distillation Complex and dynamic system influenced by aging Particulate & Vapour phases Particles Size nm CMD Concentration particles per puff Whole smoke Identified > 6000 chemicals in tobacco smoke 3
4 Challenges Faced Most analytical approaches employ off-line techniques that limit the understanding of the processes leading to smoke formation. Mass spectrometry techniques in this area typically cause fragmentation and thereby difficulties in identification of spectra Mass Spectra with EI 70 ev. 4
5 LM2X-TOFMS Overview The LM2X-TOFMS (Borgwaldt GmbH, Germany) is a coupling of a smoke engine & TOF mass spectrometer capable of analysing whole smoke online & in real time Ionisation Method : Soft Photoionisation (SPI) (126nm / 9.8 ev) Quantification of seven analytes acetaldehyde, acetone, benzene, 1,3-butadiene, 2-butanone, Isoprene, Toluene Data : total (µg/cigarette) &/or puff by puff (µg/puff) Mass range Dynamic range Resolution Mass accuracy Gas flow into ion volume Calibration Gas Th > 10^5 (in 500 ms) > 500 Th/Th (with EI) <10mTh (with internal mass calibration) approx. 0.7mL/min 100 ppm toluene in N2 5
6 Tobacco smoke mass spectrum LM2X-TOF-MS SPI-TOFMS 9.8 ev EI-TOFMS 70 ev 6
7 Objectives Validate the LM2X-TOFMS to ensure confidence of data using International Committee Harmonisation (ICH) guidelines Step One Robustness Testing Step Two Linearity and Bias Repeatability Limits of detection / quantification Step Three ISO Smoking HCI Smoking 7
8 Robustness The ability for a system to remain unaffected by small but deliberate changes Changes identified: capillary length, ferrule, day time of day Variables : temperature humidity Parameters 3R4F research cigarette ISO puff parameters 3 days Identified Change Capillary Ferrule DAY Time New New 1 am Cut_1 Same 1 am Cut_2 Same 1 am Cut_3 Same 1 am No Cut Same 1 am New New 1 pm Cut_1 Same 1 pm Cut_2 Same 1 pm Cut_3 Same 1 pm No Cut Same 1 pm
9 Robustness Results Identified Changes Vapour Phase Analyte Capillary Ferrule Day Time (AM vs. PM) Treatment Acetaldehyde ,3-Butadiene Acetone * Isoprene < 0.001* Butanone Benzene * Toluene * Statistically significant values (p value <0.05) are marked with an * 9
10 Robustness Results 10
11 Linearity, Bias, Repeatability & Accuracy Linearity & Bias 3 L gas bag measurements Six concentration mixtures Blanks - nitrogen 3 days 140 puffs per analyte ISO puffing regime ( ) Bottle [ppm] Analyte Acetaldehyde Butadiene Acetone Isoprene Butanone Benzene Toluene Repeatability Gas bag & cigarette smoking 3 cigarette types Commercial (1mg) 3R4F (Univ Kentucky, 7mg) CM6 (CORESTA, 14 mg) 5 days Day Day One Day Two Day Three Time AM PM AM PM AM PM Gas Bottle Number 4 4 BLANK BLANK BLANK BLANK 1 BLANK 1 1 BLANK 6
12 Linearity Results Yield [µg/puff] y = x R² = 1 Measured Toluene Calculated Toluene Concentration [ppm] Yield [µg/puff] y = x R² = Measured Benzene Calculated Benzene Concentration [ppm] Yield [µg/puff] y = x R² = Measured 1,3- butadiene Calculated 1,3- butadiene Concentration [ppm] Yield [µg/puff] y = x R² = Concentration [ppm] Measured Acetaldehyde Calculated Acetaldehyde 12
13 Bias Results Relative error = (concentration measured concentration expected) / concentration expected Relative Error (%) Analyte Average (n=140) Min Max Acetaldehyde Butadiene Acetone Isoprene Butanone Benzene Toluene Allows optimisation of instrument per analyte 13
14 Repeatability & Accuracy 14
15 Precision & Accuracy Inter & Intra Day Precision and Accuracy RSD, min -max (%) Analyte Concentration Range [ppm] Intra day (D1; n=40) Inter day (x3 days; n=140) Accuracy (%) (range) Acetaldehyde ( ) 14.7 ( ) 100 (±2) Acetone ( ) 7.2 ( ) 100 (±1) 1,3-Butadiene ( ) 10.6 ( ) 95 (±13) 2-Butanone ( ) 10.3 ( ) 100 (±3) Benzene ( ) 8.6 ( ) 100 (±1) Isoprene ( ) 3.8 ( ) 99 (±3) Toluene ( ) 7.0 ( ) 100 (±2) 15
16 Gas Bag -Rep Xbar-S Chart of Benzene B5 5.6 UCL= Mean Measured Yield (µg/puff) Sample Mean Sample _ X= LC L= UCL= Sample StDev _ S= LC L= Sample
17 Gas Bag Puff By Puff I-MR Chart of Benzene_1 by Puff_ Measured Yield (µg/puff) Individual Value UCL=2.088 _ X=1.652 LCL= Observation Difference Moving Range UCL= MR= LCL= Observation
18 Why this is important Yield (µg/cigarette) C D1 C D2 C D3 C D4 C D5 3R4F D1 3R4F D2 3R4F D3 3R4F D4 3R4F D5 CM6 D1 CM6 D2 CM6 D3 CM6 D4 CM6 D Acetaldehyde Butadiene Acetone Isoprene 2-Butanone Benzene Toluene Vapour Phase Analyte 18
19 ISO 3R4F Puff By Puff 80 Yield (µg/puff) Puff One Puff Two Puff Three Puff Four Puff Five Puff Six Puff Seven Puff Eight Acetaldehyde Butadiene Acetone Isoprene 2-Butanone Benzene Toluene Analyte 19
20 Summary Based on current data : The system is robust All seven analytes demonstrate linearity Bias is generally consistent for all analytes Good repeatability and accuracy Reproducibility need another instrument Variation mostly due to cigarettes not system 20
21 Acknowledgements Borgwaldt GmbH, Hamburg Mark Barber Caner Yurteri Graham Errington Jasper van Heemst John McAughey 21
22 Thank you for your time Any questions? 22
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