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Two Techniques for the Analysis of WS-3 With Potential Application to the Analysis of Other Cooling Agents * Cover

Two Techniques for the Analysis of WS-3 With Potential Application to the Analysis of Other Cooling Agents *

Contributions to Tobacco & Nicotine Research
Volume 32 (2023): Issue 1 (March 2023)
By: Serban C. Moldoveanu and  Robert O. Bussey  
Open Access
|Apr 2023

Figures & Tables

Figure 1.

Chemical structures of four compounds with cooling properties.
Chemical structures of four compounds with cooling properties.

Figure 2.

Typical LC/MS chromatogram for a standard containing 0.78 µg/mL of each analyte and 12.5 µg/mL internal standard (IS).
Typical LC/MS chromatogram for a standard containing 0.78 µg/mL of each analyte and 12.5 µg/mL internal standard (IS).

Figure 3.

Typical GC/MS chromatogram of a standard mixture containing each coolant agent at 25 µg/mL and the internal standard (I.S.) at 12.5 µg/mL.
Typical GC/MS chromatogram of a standard mixture containing each coolant agent at 25 µg/mL and the internal standard (I.S.) at 12.5 µg/mL.

Results of WS-3 analysis by GC/MS in four analyzed nicotine pouches_

SamplesLevel of WS-3 (mg/g)RSD (%)
Sample 1 a0.514
Sample 1 b0.469
Sample 1 c0.490
Average for pouch 10.4914.59

Level of WS-3 per g of tobacco in several cigarettes_

SamplesLevel of WS-3 (mg/g)RSD (%)
Experimental cigarette 1 (LC/MS)  2.8781.93
Experimental cigarette 1 (GC/MS)  2.9914.93
Experimental cigarette 2  1.9543.52
Experimental cigarette 3< LOQ
Experimental cigarette 4  1.4840.02
Commercial cigarette 1< LOQ
Commercial cigarette 2< LOQ

Results for the measurement of WS-3 in cigarette smoke_

SmokingLevel of WS-3 (mg/g)RSD (%)
ISO0.1961.31
HCA0.2400.79

The parameters a, b, and c used for calibration for each cooling agent as well as the corresponding correlation coefficient R2_

CompoundabcR2
WS-23-3.91604E-145.64097E-06-0.055495290.9987
WS-3    4.4729E-131.77042E-06      0.1974420.9989
Evercool 190-5.22754E-142.58027E-06-0.023076810.9990
Evercool 180  1.61678E-126.22688E-060.0075957380.9982

Results of WS-3 analysis by LC/MS in four analyzed nicotine pouches_

SamplesLevel of WS-3 (mg/g)RSD (%)
Sample 1 a  0.496
Sample 1 b  0.513
Sample 1 c  0.496
Average for pouch 1  0.5021.99
Sample 2 a< LOQ
Sample 2 b< LOQ
Sample 2 c< LOQ
Average for pouch 2< LOQ—
Sample 3 a< LOQ
Sample 3 b< LOQ
Sample 3 c< LOQ
Average for pouch 3< LOQ—
Sample 4 a0.105
Sample 4 b0.103
Sample 4 c0.104
Average for pouch 40.1040.84

Results for WS-3 levels in some flavor solutions_

SampleWS-3 (mg/g)RSD (%)
Flavor 1125.694.33
Flavor 2117.560.63
Flavor 3123.722.74
Flavor 4112.272.59
Flavor 5119.503.82
Flavor 6118.360.24
Flavor 7121.132.95
Flavor 8123.001.82
Flavor 9113.891.84

The LOQ values for the GC/MS method of analysis of cooling agents_

CompoundLOQ (μg/mL)
WS-231.56
WS-31.56
Evercool 1903.13
Evercool 1806.25

The recovery of WS-3 from a tobacco sample spiked with three levels of analyte and the corresponding recovery levels_

Taken (mg/g)Analyzed (mg/g)Recovery (%)RSD (%)
2.02.018100.93.316
1.01.004100.43.444
0.50.500100.01.375

Gradient conditions for coolants HPLC separation_

Time (min)A (%)B (%)
0.0955
0.5955
2.04060
4.04060
5.0955
6.0955

Samples analyzed in this study_

Sample typeMaterial typeAnalytical procedure
Experimental cigarette 1 aTobacco from cigaretteLC/MS, GC/MS
Experimental cigarette 2 aTobacco from cigaretteLC/MS
Experimental cigarette 3 aTobacco from cigaretteLC/MS
Experimental cigarette 4 aTobacco from cigaretteLC/MS
Commercial cigarette 1 bTobacco from cigaretteLC/MS
Commercial cigarette 2 bTobacco from cigaretteLC/MS
Nicotine pouch 1 bNicotine pouchLC/MS, GC/MS
Nicotine pouch 2 bNicotine pouchLC/MS
Nicotine pouch 3 bNicotine pouchLC/MS
Nicotine pouch 4 bNicotine pouchLC/MS
Experimental cigarette 1 aSmoke ISOLC/MS
Experimental cigarette 1 aSmoke HCALC/MS
Flavor (1) to flavor (9) aFlavor solutionLC/MS

Ion used to generate the extracted peak, the parameters a and b used for calibration for each cooling agent as well as the corresponding correlation coefficient R2_

Compoundm/z for peak areaabR2
I.S. (nicotinamide)122,1 -
WS-23129,100,2188010,9998
WS-3211,20-0,178140,9995
Evercool 190288,102,6045580,999
Evercool 180298,103,443240,9986

Typical parameters for the GC/MS analysis_

ParameterDescriptionParameterDescription
Initial oven temperature37 °CCarrier gasHelium
Initial time1.0 minInjection volume1 μL
Oven ramp rate30 °C/minFlow modeConstant flow
Oven temperature70 °CFlow rate1.1 mL/min
Final time first ramp0 minNominal initial pressure7.95 psi
Oven ramp rate20 °C/minGC outletMSD
Oven final temperature300 °CMSD transfer line temperature270 °C
Final time6.4 minIon source temperature230 °C
Total run time20.0 minQuadrupole temperature150 °C
Inlet temperature280 °CMSD Gain1
Inlet modeSplitMSD solvent delay5.0 min
Split ratio10:1Mass range33–350 a.u.
DOI: https://doi.org/10.2478/cttr-2023-0004 | Journal eISSN: 2719-9509
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Language: English
Page range: 26 - 33
Submitted on: Jun 21, 2022
Accepted on: Mar 9, 2023
Published on: Apr 4, 2023
Published by: Institut für Tabakforschung GmbH
In partnership with: Paradigm Publishing Services
Publication frequency: 4 issues per year
Keywords:
WS-3,
WS-23,
Evercool 180,
Evercool 190
Related subjects:
General interest,
Life sciences,
Life sciences, other,
Physics,
Physics, other

© 2023 Serban C. Moldoveanu, Robert O. Bussey, published by Institut für Tabakforschung GmbH
This work is licensed under the Creative Commons Attribution-NonCommercial-ShareAlike 4.0 License.

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