O artykule
Data publikacji: 25 wrz 2020
Zakres stron: 57 - 65
Otrzymano: 25 mar 2020
Przyjęty: 29 maj 2020
DOI: https://doi.org/10.2478/cttr-2020-0007
Słowa kluczowe
© 2020 Serban C. Moldoveanu, published by Sciendo
This work is licensed under the Creative Commons Attribution-NonCommercial-ShareAlike 4.0 International License.
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Parameters for the MS/MS detection.
| Compound | Ion for Q1 | Ion for Q3 | Time (ms) | CE3 (V) |
|---|---|---|---|---|
| α-Tocopherol | 431.4 | 165.1 | 200 | 38.0 |
| α-Tocopheryl acetate | 473.4 | 165.1 | 200 | 52.0 |
| Uvitex-OB (I.S.) | 431.5 | 415.3 | 200 | 49.0 |
The list of standards in μg/mL(the addition of 10 μL I.S. slightly changes the final concentrations from the values in the stock solution).
| Compound | Standard in μg/mL | |||||||||
|---|---|---|---|---|---|---|---|---|---|---|
| Level 1 | Level 2 | Level 3 | Level 4 | Level 5 | Level 6 | Level 7 | Level 8 | Level 9 | Level 10 | |
| α-Tocopherol | 98.63 | 49.31 | 24.66 | 12.33 | 6.16 | 3.08 | 1.54 | 0.77 | 0.39 | 0.19 |
| α-Tocopherol acetate | 96.47 | 48.24 | 24.12 | 12.06 | 6.03 | 3.01 | 1.51 | 0.75 | 0.38 | 0.19 |
Percent recovery of α-tocopherol in a second extraction from total in the sample.
| Experiment | First extraction (μg/g) | Second extraction (μg/g) | % in second extraction |
|---|---|---|---|
| 1 | 749.16 | 15.70 | 2.05 |
| 2 | 812.54 | 18.66 | 2.24 |
| 3 | 768.32 | 14.57 | 1.86 |
| 4 | 808.30 | 16.14 | 1.96 |
j.cttr-2020-0007.tab.011
| Declustering potential DE | = 150 V, |
| Entrance potential | = 13 V, |
| Collision gas (N2) CG | = 6 mL/min, |
| Curtain gas CUR | = 10 mL/min, |
| Ion spray voltage IS | = 4000 V, |
| Temperature TE | = 600 °C, |
| Ion source gas 1 GS1 | = 35 mL/min, |
| Ion source gas 2 GS2 | = 30 mL/min. |
The values for LOQ for α-tocopherol and α-tocopheryl acetate in μg/mL standard solution and per g of sample.
| Compound | LOQ solution (μg/mL) | LOQ sample (μg/g) |
|---|---|---|
| α-Tocopherol | 0.19 | 1.9 |
| α-Tocopheryl acetate | 0.19 | 1.9 |
The TPM in g generated from 5 cigarettes smoked under ISO type conditions and the average results for α-tocopherol in μg/mg in the collected TPM as obtained by the analysis with UV detection.
| Sample No. | Sample acronym |
TPM, Repetition 1 (g) | TPM, Repetition 2 (g) | Average α-tocopherol in TPM (μg/mg) | RSD (%) |
|---|---|---|---|---|---|
| 3 | FC L (2) | 0.0668 | 0.0639 | 3.35 | 0.38 |
| 4 | FC U (2) | 0.0794 | 0.0816 | 3.98 | 1.11 |
| 5 | FC L (3) | 0.0534 | 0.0559 | 4.17 | 3.60 |
| 6 | FC U (3) | 0.0818 | 0.0802 | 3.54 | 1.66 |
| 7 | FC off L | 0.0543 | 0.0561 | 4.08 | 1.99 |
| 8 | FC off U | 0.0714 | 0.0737 | 3.65 | 0.65 |
| 11 | Bu L (2) | 0.0586 | 0.0626 | 2.72 | 0.35 |
| 12 | Bu U (2) | 0.0704 | 0.0703 | 2.84 | 0.07 |
| 13 | Bu L (3) | 0.0679 | 0.0598 | 2.22 | 0.35 |
| 14 | Bu U (3) | 0.0650 | 0.0574 | 2.15 | 4.15 |
| 15 | Bu off L | 0.0701 | 0.0651 | 1.83 | 0.01 |
| 16 | Bu off U | 0.0669 | 0.0729 | 1.52 | 0.44 |
| 19 | Or Sa U | 0.0468 | 0.0463 | 1.68 | 1.13 |
| 20 | Or Iz U | 0.0504 | 0.0464 | 2.76 | 0.57 |
| 21 | Commercial | 0.0509 | 0.0421 | 2.95 | 0.67 |
| 22 | 3R4F | 0.0643 | 0.0701 | 1.80 | 0.74 |
Timetable for the gradient HPLC separation.
| Run time (min) | Solvent A % | Solvent B % | Detection |
|---|---|---|---|
| 0.0 | 85.0 | 15.0 | On |
| 15.0 | 85.0 | 15.0 | On |
| 15.5 | 40.0 | 60.0 | On |
| 16.0 | 40.0 | 60.0 | Off |
| 18.5 | 40.0 | 60.0 | Off |
| 19.0 | 85.0 | 15.0 | Off |
| 25.0 | 85.0 | 15.0 | Off |
Average α-tocopherol levels in μg/g tobacco as measured using the UV detection.
| Sample No. | Sample acronym |
(μg/g) “as is” | (μg/g) “dry base” | RSD (%) |
|---|---|---|---|---|
| 1 | FC L (1) | 731.18 | 778.26 | 0.27 |
| 2 | FC U (1) | 857.27 | 914.80 | 1.92 |
| 3 | FC L (2) | 760.38 | 812.39 | 2.09 |
| 4 | FC U (2) | 823.72 | 884.26 | 1.92 |
| 5 | FC L (3) | 778.92 | 840.15 | 1.93 |
| 6 | FC U (3) | 823.06 | 881.57 | 2.53 |
| 7 | FC off L | 746.77 | 807.48 | 2.86 |
| 8 | FC off U | 764.48 | 833.36 | 2.65 |
| 9 | Bu L (1) | 231.93 | 246.68 | 0.24 |
| 10 | Bu U (1) | 336.85 | 361.00 | 0.81 |
| 11 | Bu L (2) | 396.24 | 423.70 | 0.54 |
| 12 | Bu U (2) | 599.52 | 641.43 | 2.80 |
| 13 | Bu L (3) | 267.59 | 289.24 | 2.54 |
| 14 | Bu U (3) | 284.40 | 308.09 | 0.56 |
| 15 | Bu off L | 327.57 | 354.40 | 0.92 |
| 16 | Bu off U | 255.28 | 276.32 | 0.37 |
| 17 | Or (1) | 296.70 | 316.40 | 0.65 |
| 18 | Or (2) | 267.31 | 283.97 | 0.08 |
| 19 | Or Sa U | 181.74 | 197.00 | 1.31 |
| 20 | Or Iz U | 427.01 | 456.35 | 0.37 |
| 21 | Commercial | 510.19 | 546.97 | 0.53 |
| 22 | 3R4F | 404.30 | 432.03 | 0.31 |
Coefficients for the calibration curves Y = a X + b and of R2 used in UV quantitation.
| Compound | a | b | R2 |
|---|---|---|---|
| α-Tocopherol | 0.022401 | −0.05633 | 1.00 |
| α-Tocopheryl acetate | 0.022655 | −0.05204 | 1.00 |
Coefficients for the calibration curves Y = a X + b and of R2 used in MS/MS quantitation.
| Compound | a | b | R2 |
|---|---|---|---|
| α-Tocopherol | 34.2270 | −1.00506 | 0.9997 |
| α-Tocopheryl acetate | 10.7472 | −1.39160 | 0.9997 |
List of tobaccos evaluated in this study, the moisture in % and the indication if cigarettes were available.
| No. | Sample acronym |
Description | Moisture (%) | Cigarettes available |
|---|---|---|---|---|
| 1 | FC L (1) | Common blend of lower stalk flue-cured | 6.44 | No |
| 2 | FC U (1) | Common blend of upper stalk flue-cured | 6.71 | No |
| 3 | FC L (2) | Eastern NC belt, lower stalk (lug) flue-cured | 6.84 | Yes |
| 4 | FC U (2) | Eastern NC belt, upper stalk (leaf & some tips) flue-cured | 7.35 | Yes |
| 5 | FC L (3) | South Carolina belt, lower stalk (lug) flue-cured | 7.86 | Yes |
| 6 | FC U (3) | South Carolina belt, upper stalk (leaf & some tips) flue-cured | 7.11 | Yes |
| 7 | FC off L | Brazil, lower stalk (lugs & primings) flue-cured | 8.13 | Yes |
| 8 | FC off U | Brazil, upper stalk (leaf & tips) flue-cured | 9.01 | Yes |
| 9 | Bu L (1) | Common blend of lower stalk Burley | 6.36 | No |
| 10 | Bu U (1) | Common blend of upper stalk Burley | 7.17 | No |
| 11 | Bu L (2) | Kentucky & Tennessee, lower stalk (flyings & cutters) Burley | 6.93 | Yes |
| 12 | Bu U (2) | Kentucky & Tennessee, upper stalk (leaf) Burley | 6.99 | Yes |
| 13 | Bu L (3) | North Carolina & Virginia, lower stalk (flyings & cutters) Burley | 8.09 | Yes |
| 14 | Bu U (3) | North Carolina & Virginia, upper stalk (leaf) Burley | 8.33 | Yes |
| 15 | Bu off L | Malawi, lower stalk (flyings & rcutters) Burley | 8.19 | Yes |
| 16 | Bu off U | Malawi, upper stalk (leaf) Burley | 8.24 | Yes |
| 17 | Or (1) | Common blend of Oriental | 6.64 | No |
| 18 | Or (2) | Common blend of Oriental | 6.23 | No |
| 19 | Or Sa U | Turkey, good quality middle to upper stalk, Samsun Oriental | 8.40 | Yes |
| 20 | Or Iz U | Turkey, good quality middle to upper stalk, Izmir Oriental | 6.87 | Yes |
| 21 | Commercial | Tobacco blend | 7.21 | Yes |
| 22 | 3R4F | Tobacco blend | 6.86 | Yes |