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

Serban C. Moldoveanu
Serban C. Moldoveanu
 et 
Robert O. Bussey
Robert O. Bussey
   | 04 avr. 2023
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Publié en ligne: 04 avr. 2023
Pages: 26 - 33
Reçu: 21 juin 2022
Accepté: 09 mars 2023
DOI: https://doi.org/10.2478/cttr-2023-0004
© 2023 Serban C. Moldoveanu et al., published by Sciendo
This work is licensed under the Creative Commons Attribution-NonCommercial-ShareAlike 4.0 International License.

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.

Samples Level of WS-3 (mg/g) RSD (%)
Sample 1 a 0.514
Sample 1 b 0.469
Sample 1 c 0.490
Average for pouch 1 0.491 4.59

Level of WS-3 per g of tobacco in several cigarettes.

Samples Level of WS-3 (mg/g) RSD (%)
Experimental cigarette 1 (LC/MS)   2.878 1.93
Experimental cigarette 1 (GC/MS)   2.991 4.93
Experimental cigarette 2   1.954 3.52
Experimental cigarette 3 < LOQ
Experimental cigarette 4   1.484 0.02
Commercial cigarette 1 < LOQ
Commercial cigarette 2 < LOQ

Results for the measurement of WS-3 in cigarette smoke.

Smoking Level of WS-3 (mg/g) RSD (%)
ISO 0.196 1.31
HCA 0.240 0.79

The parameters a, b, and c used for calibration for each cooling agent as well as the corresponding correlation coefficient R2.

Compound a b c R2
WS-23 -3.91604E-14 5.64097E-06 -0.05549529 0.9987
WS-3     4.4729E-13 1.77042E-06       0.197442 0.9989
Evercool 190 -5.22754E-14 2.58027E-06 -0.02307681 0.9990
Evercool 180   1.61678E-12 6.22688E-06 0.007595738 0.9982

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

Samples Level 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   0.502 1.99
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 a 0.105
Sample 4 b 0.103
Sample 4 c 0.104
Average for pouch 4 0.104 0.84

Results for WS-3 levels in some flavor solutions.

Sample WS-3 (mg/g) RSD (%)
Flavor 1 125.69 4.33
Flavor 2 117.56 0.63
Flavor 3 123.72 2.74
Flavor 4 112.27 2.59
Flavor 5 119.50 3.82
Flavor 6 118.36 0.24
Flavor 7 121.13 2.95
Flavor 8 123.00 1.82
Flavor 9 113.89 1.84

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

Compound LOQ (μg/mL)
WS-23 1.56
WS-3 1.56
Evercool 190 3.13
Evercool 180 6.25

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 (%)
2.0 2.018 100.9 3.316
1.0 1.004 100.4 3.444
0.5 0.500 100.0 1.375

Gradient conditions for coolants HPLC separation.

Time (min) A (%) B (%)
0.0 95 5
0.5 95 5
2.0 40 60
4.0 40 60
5.0 95 5
6.0 95 5

Samples analyzed in this study.

Sample type Material type Analytical procedure
Experimental cigarette 1 a Tobacco from cigarette LC/MS, GC/MS
Experimental cigarette 2 a Tobacco from cigarette LC/MS
Experimental cigarette 3 a Tobacco from cigarette LC/MS
Experimental cigarette 4 a Tobacco from cigarette LC/MS
Commercial cigarette 1 b Tobacco from cigarette LC/MS
Commercial cigarette 2 b Tobacco from cigarette LC/MS
Nicotine pouch 1 b Nicotine pouch LC/MS, GC/MS
Nicotine pouch 2 b Nicotine pouch LC/MS
Nicotine pouch 3 b Nicotine pouch LC/MS
Nicotine pouch 4 b Nicotine pouch LC/MS
Experimental cigarette 1 a Smoke ISO LC/MS
Experimental cigarette 1 a Smoke HCA LC/MS
Flavor (1) to flavor (9) a Flavor solution LC/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.

Compound m/z for peak area a b R2
I.S. (nicotinamide) 122,1 -
WS-23 129,1 0 0,218801 0,9998
WS-3 211,2 0 -0,17814 0,9995
Evercool 190 288,1 0 2,604558 0,999
Evercool 180 298,1 0 3,44324 0,9986

Typical parameters for the GC/MS analysis.

Parameter Description Parameter Description
Initial oven temperature 37 °C Carrier gas Helium
Initial time 1.0 min Injection volume 1 μL
Oven ramp rate 30 °C/min Flow mode Constant flow
Oven temperature 70 °C Flow rate 1.1 mL/min
Final time first ramp 0 min Nominal initial pressure 7.95 psi
Oven ramp rate 20 °C/min GC outlet MSD
Oven final temperature 300 °C MSD transfer line temperature 270 °C
Final time 6.4 min Ion source temperature 230 °C
Total run time 20.0 min Quadrupole temperature 150 °C
Inlet temperature 280 °C MSD Gain 1
Inlet mode Split MSD solvent delay 5.0 min
Split ratio 10:1 Mass range 33–350 a.u.
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