Ultrasound-Assisted Solvent Extraction of a Porous Membrane Packed Sample for the Determination of Tobacco-Specific Nitrosamines in the Replacement Liquids for E-Cigarettes
Abstract
:1. Introduction
2. Results
2.1. Detection Parameters and Chromatographic Separation
2.2. Optimization of the Extraction Procedure
2.3. Method Validation
2.4. Analysis of Real Samples
3. Discussion
4. Materials and Methods
4.1. Standards and Solutions Preparations
4.2. Instruments and Analytical Conditions
4.3. Sample Preparation of the Replacement Liquids and Spiked Samples
Supplementary Materials
Funding
Acknowledgments
Conflicts of Interest
References
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Sample Availability: Samples of the compounds are available from the author after personal communication. |
Analyte | Precursor Ion [M + H]+ [m/z] | Product Ions [m/z] | Collision Energy [V] | Q1 Prerod [V] | Q3 Prerod [V] |
---|---|---|---|---|---|
NNK | 208.00 | 79.10 1 | −26 | −40 | −29 |
148.20 | −11 | −12 | −13 | ||
NNN | 178.10 | 120.10 1 | −14 | −19 | −25 |
148.20 | −21 | −13 | −30 | ||
NAT | 190.00 | 79.10 1 | −14 | −29 | −13 |
160.20 | −14 | −11 | −16 | ||
NAB | 192.10 | 162.20 1 | −10 | −14 | −29 |
133.20 | −14 | −19 | −29 | ||
NNK-d4 | 212.20 | 126.20 1 | −10 | −12 | −22 |
152.15 | −10 | −13 | −30 | ||
NNN-d4 | 182.20 | 152.20 1 | −14 | −12 | −14 |
122.10 | −12 | −29 | −12 | ||
NAT-d4 | 194.20 | 164.20 1 | −20 | −12 | −16 |
110.20 | −10 | −17 | −23 | ||
NAB-d4 | 196.20 | 166.20 1 | −14 | −13 | −30 |
137.20 | −19 | −23 | −23 |
Analyte | Calibration Curve Equation (6 Points, n = 3) | Sa | Sb | LOD [ng/g] | LOQ [ng/g] | R2 |
---|---|---|---|---|---|---|
NNK | y = 0.01211x + 0.0045 | 0.00029 | 0.0031 | 0.9 | 2.6 | 0.9931 |
NNN | y = 0.08552x − 0.0014 | 0.00070 | 0.0075 | 0.3 | 0.9 | 0.9992 |
NAT | y = 0.05133x − 0.0016 | 0.00041 | 0.0044 | 0.3 | 0.9 | 0.9992 |
NAB | y = 0.05865x + 0.00022 | 0.00073 | 0.00791 | 0.4 | 1.3 | 0.9981 |
Analyte | Spiking Level | Mean Recovery [ng/g] (%), n = 6 | SD [ng/g] | CV [%] | Repeatability, n = 6 | |||
---|---|---|---|---|---|---|---|---|
Day | Mean Recovery [ng/g] (%) | SD [ng/g] | CV [%] | |||||
NNK | 5 | 4.7 (93) | 0.2 | 3.3 | 1 | 19.0 (95) | 0.7 | 3.6 |
20 | 19.0 (95) | 0.7 | 3.6 | 2 | 19.3 (96) | 0.6 | 2.9 | |
40 | 41.5 (104) | 0.9 | 2.1 | 3 | 18.5 (92) | 0.8 | 4.2 | |
NNN | 5 | 4.9 (97) | 0.2 | 4.0 | 1 | 20.9 (105) | 0.8 | 3.7 |
20 | 20.9 (105) | 0.8 | 3.7 | 2 | 21.2 (106) | 0.9 | 4.1 | |
40 | 41.4 (104) | 0.9 | 2.2 | 3 | 20.5 (103) | 0.7 | 3.2 | |
NAT | 5 | 4.6 (92) | 0.2 | 3.2 | 1 | 18.0 (90) | 0.5 | 2.5 |
20 | 18.0 (90) | 0.5 | 2.5 | 2 | 17.7 (88) | 0.3 | 1.8 | |
40 | 34.8 (87) | 0.7 | 1.9 | 3 | 18.6 (93) | 0.6 | 3.2 | |
NAB | 5 | 4.9 (97) | 0.2 | 4.9 | 1 | 19.4 (97) | 0.4 | 2.2 |
20 | 19.4 (97) | 0.4 | 2.2 | 2 | 18.9 (95) | 0.8 | 4.1 | |
40 | 37.5 (94) | 0.7 | 1.9 | 3 | 18.7 (93) | 0.6 | 3.3 |
No. Sample and Flavour | Amount of Sample [g] | PG/VG Ratio; (Density) [g/cm3] | NNK ± SD [ng/mL] | NNN ± SD [ng/mL] | NAT ± SD [ng/mL] | NAB ± SD [ng/mL] |
---|---|---|---|---|---|---|
Producer 1 | 50/50; (1.15) | |||||
1. Cherry | 1.059 | 1.20 ± 0.05 | - | - | - | |
Producer 2 | 60/40; (1.13) | |||||
2. Fruit mix | 1.102 | 2.6 ± 0.3 | 7.5 ± 0.2 | - | - | |
3. Tobacco | 1.092 | 7.6 ± 0.4 | - | 1.7 ± 0.1 | - | |
4. Vanilla | 1.088 | 7.5 ± 0.6 | 4.1 ± 0.6 | - | - | |
5. Mint | 1.095 | 2.9 ± 0.3 | 15.6 ± 1.3 | - | - | |
Producer 3 | 60/40; (1.13) | |||||
6. Apple | 1.066 | 54.3 ± 3.0 | 4.2 ± 0.2 | - | - | |
7. Mint | 1.057 | - | 4.6 ± 0.2 | - | - | |
Producer 4 | 80/20; (1.08) | |||||
8. Strawberry | 1.047 | 16.1 ± 0.9 | - | - | - | |
9. Tobacco | 1.031 | 35.8 ± 2.0 | 30.2 ± 1.1 | 2.5 ± 0.1 | - |
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Kubica, P. Ultrasound-Assisted Solvent Extraction of a Porous Membrane Packed Sample for the Determination of Tobacco-Specific Nitrosamines in the Replacement Liquids for E-Cigarettes. Molecules 2019, 24, 4618. https://doi.org/10.3390/molecules24244618
Kubica P. Ultrasound-Assisted Solvent Extraction of a Porous Membrane Packed Sample for the Determination of Tobacco-Specific Nitrosamines in the Replacement Liquids for E-Cigarettes. Molecules. 2019; 24(24):4618. https://doi.org/10.3390/molecules24244618
Chicago/Turabian StyleKubica, Paweł. 2019. "Ultrasound-Assisted Solvent Extraction of a Porous Membrane Packed Sample for the Determination of Tobacco-Specific Nitrosamines in the Replacement Liquids for E-Cigarettes" Molecules 24, no. 24: 4618. https://doi.org/10.3390/molecules24244618