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Identification and Quantitation of Nicotine Polacrilex in Nicotine Pouches and Other Oral Nicotine Delivery Products


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Figure 1.

Window 30 min to 40 min for the extracted ion chromatogram for m/z = 117 from the pyrogram of a sample of nicotine pouches that contains nicotine polacrilex.
Window 30 min to 40 min for the extracted ion chromatogram for m/z = 117 from the pyrogram of a sample of nicotine pouches that contains nicotine polacrilex.

Figure 2.

Peak areas of ion m/z = 178 eluting at 58.33 min corresponding to phenanthrene for several standards and samples.
Peak areas of ion m/z = 178 eluting at 58.33 min corresponding to phenanthrene for several standards and samples.

Figure 3.

Window 40 min to 50 min for the extracted ion chromatogram for m/z = 162 from the pyrogram of a sample of nicotine pouches that contains nicotine polacrilex.
Window 40 min to 50 min for the extracted ion chromatogram for m/z = 162 from the pyrogram of a sample of nicotine pouches that contains nicotine polacrilex.

Levels of % nicotine polacrilex, % nicotine, and of (nicotine)/(nicotine polacrilex) ratio % in several commercially available nicotine pouches.

Sample No. of replicates Found nicotine polacrilex (%) RSD% Found nicotine (%) Ratio (%)
Sample 1 2 7.38 0.29 0.70 9.53
Sample 2 4 8.59 1.24 0.80 9.30
Sample 3 2 11.54 0.67 1.32 11.42
Sample 4 1 11.8 1.17 9.91
Sample 5 1 5.25 0.63 12.10
Sample 6 1 5.11 0.59 11.45
Sample 7 1 6.35 0.83 13.06
Sample 8 1 3.70 0.66 17.81
Sample 9 1 4.76 0.83 17.42
Sample 10 1 6.70 0.97 14.47
Sample 11 1 8.71 0.90 10.34
Sample 12 2 not detected 1.28
Sample 13 1 not detected 2.37
Sample 14 1 not detected 1.73

Levels of % nicotine polacrilex, % nicotine, and of (nicotine)/(nicotine polacrilex) ratio % in several nicotine pouches samples with known composition.

Sample No. of replicates Expected nicotine polacrilex (%) Found nicotine polacrilex (%) RSD% (of found) Expected nicotine (%) (by HPLC) Found nicotine (%) Ratio (%)
Sample 1 6 9.72 8.92 1.61 1.94 1.70 19.09
Sample 2 2 5.56 5.55 0.89 1.11 1.03 18.56
Sample 3 3 5.56 5.13 2.34 1.11 0.98 19.10
Sample 4 3 2.78 2.84 1.47 0.56 0.53 18.66

Parameters for the GC/MS on-line analysis of pyrolysates on a DB-1701 type column.

Parameter Description
GC column DB-1701
Column dimensions 60 m long, 0.25 mm id.
Film thickness 1.0 μm
Initial oven temperature 37 °C
Initial time 4.0 min
Oven ramp rate 2 °C/min
Oven final first ramp 60 °C
Final time first ramp 0 min
Oven ramp rate 5 °C/min
Oven final temperature 280 °C
Final time 20 min
Total run time 75.5 min
Inlet temperature 280 °C
Inlet mode Split
Carrier gas Helium
Flow mode Constant flow
Flow rate 1.1 mL/min
Nominal initial pressure 17.5 psi
Split ratio 70:1
Split flow 76.0 mL/min
GC outlet MSD
Outlet pressure Vacuum
MSD transfer line temperature 280 °C
Ion source temperature 230 °C
Quadrupole temperature 150 °C
MSD EM offset 250 V
MSD solvent delay 2.0 min
MSD acquisition mode TIC
Mass range 29–550 a.u.

Levels of % nicotine polacrilex, % nicotine, and of (nicotine)/(nicotine polacrilex) ratio % in a tablet, a lozenge, and two gums.

Sample No. of replicates Found nicotine polacrilex (%) RSD% Found nicotine (%) Ratio (%)
Tablet 2 10.51 0.24 0.96 9.13
Lozenge 2 4.16 0.74 0.38 9.13
Gum 1 2 not detected 0.12
Gum 2 2 1.84 0.27 0.22 11.96
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Allgemein, Biologie, andere, Physik