Online In-Tube Solid-Phase Microextraction Coupled to Liquid Chromatography–Tandem Mass Spectrometry for the Determination of Tobacco-Specific Nitrosamines in Hair Samples
Abstract
:1. Introduction
2. Results and Discussion
2.1. Optimization of In-Tube Solid-Phase Microextraction and Desorption of TSNAs
2.2. LC–MS/MS Analysis of TSNAs and Their Stable Isotope-Labeled Compounds
2.3. Analytical Method Validation
2.4. Application to the Analysis of Hair Samples
3. Materials and Methods
3.1. Reagents and Standard Solutions
3.2. Preparation of Hair Samples
3.3. LC–MS/MS Analysis
3.4. In-Tube SPME
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
Sample Availability
References
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TSNA | Linearity | LOD 2 (pg mL–1) | LOQ 3 (pg mg–1) | ||
---|---|---|---|---|---|
Range (pg mL–1) | Linearity 1 (R2) | Direct Injection | In-Tube SPME | In-Tube SPME | |
NNK | 0.5–100 | 0.9999 | 1 | 0.05 | 0.03 |
NNN | 0.5–100 | 1 | 1.8 | 0.04 | 0.03 |
NAT | 0.5–100 | 0.9999 | 1.1 | 0.02 | 0.02 |
NBT | 0.5–100 | 0.9998 | 3.5 | 0.07 | 0.04 |
NNAL | 5–1000 | 0.9999 | 12.9 | 1.14 | 0.75 |
TSNA | Nominal Concentration (pg mL–1) | Precision (CV 1%) (n = 5) | Accuracy (%) (n = 5) | ||
---|---|---|---|---|---|
Intra-Day | Inter-Day | Intra-Day | Inter-Day | ||
NNK | 2 | 3.6 | 6.4 | 100.5 | 102.5 |
20 | 2.7 | 3.7 | 100.7 | 100.3 | |
NNN | 2 | 7.3 | 9.2 | 104.5 | 104.5 |
20 | 2.7 | 4.6 | 104.7 | 104.2 | |
NAT | 2 | 4.4 | 5.2 | 113.5 | 112.0 |
20 | 2.1 | 3.0 | 103.9 | 105.2 | |
NBT | 2 | 3.1 | 8.0 | 114.5 | 118.5 |
20 | 3.0 | 7.7 | 94.2 | 99.3 | |
NNAL | 20 | 4.2 | 7.6 | 95.0 | 96.3 |
200 | 4.2 | 7.0 | 94.3 | 99.2 |
TSNA | Concentration (pg mg–1 Hair) | Recovery | |
---|---|---|---|
Spiked | Mean ± SD (n = 3) | (%) | |
NNK | 0 | ND 1 | |
2 | 1.85 ± 0.12 | 92.3 | |
20 | 20.0 ± 0.4 | 100.2 | |
NNN | 0 | ND | - |
2 | 1.95 ± 0.09 | 97.3 | |
20 | 19.0 ± 0.8 | 94.9 | |
NAT | 0 | ND | - |
2 | 1.97 ± 0.07 | 98.4 | |
20 | 20.1 ± 0.2 | 100.4 | |
NAB | 0 | ND | - |
2 | 1.92 ± 0.05 | 96.2 | |
20 | 19.7 ± 0.2 | 98.3 | |
NNAL | 0 | ND | - |
20 | 18.7 ± 0.9 | 93.7 | |
200 | 205.4 ± 0.8 | 102.7 |
TSNA | Smokers (n = 24) | Non-Smokers (n = 29) | ||||||||
---|---|---|---|---|---|---|---|---|---|---|
Detection Frequency (%) | Content (pg mg–1 Hair) | Detection Frequency (%) | Content (pg mg–1 Hair) | |||||||
Mean ± SD | Min.1 | Med. 1 | Max. 1 | Mean ± SD | Min. | Med. | Max. | |||
NNK | 100 | 0.95 ± 0.96 2 | 0.08 | 0.68 | 3.97 | 34 | 0.05 ± 0.08 2 | 0.00 | 0.00 | 0.25 |
NNN | 100 | 0.43 ± 0.85 3 | 0.02 | 0.22 | 4.44 | 14 | 0.02 ± 0.06 3 | 0.00 | 0.00 | 0.24 |
NAT | 68 | 0.09 ± 0.09 | 0.00 | 0.08 | 0.35 | 0 | ND | 0.00 | 0.00 | 0.00 |
NBT | 88 | 0.13 ± 0.27 | 0.00 | 0.06 | 1.09 | 0 | ND | 0.00 | 0.00 | 0.00 |
NNAL | 0 | ND 4 | ND | ND | ND | 0 | ND | 0.00 | 0.00 | 0.00 |
Total | 100 | 1.61 ±1.55 5 | 0.11 | 1.08 | 6.72 | 34 | 0.08 ± 0.11 5 | 0.00 | 0.00 | 0.31 |
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Ishizaki, A.; Kataoka, H. Online In-Tube Solid-Phase Microextraction Coupled to Liquid Chromatography–Tandem Mass Spectrometry for the Determination of Tobacco-Specific Nitrosamines in Hair Samples. Molecules 2021, 26, 2056. https://doi.org/10.3390/molecules26072056
Ishizaki A, Kataoka H. Online In-Tube Solid-Phase Microextraction Coupled to Liquid Chromatography–Tandem Mass Spectrometry for the Determination of Tobacco-Specific Nitrosamines in Hair Samples. Molecules. 2021; 26(7):2056. https://doi.org/10.3390/molecules26072056
Chicago/Turabian StyleIshizaki, Atsushi, and Hiroyuki Kataoka. 2021. "Online In-Tube Solid-Phase Microextraction Coupled to Liquid Chromatography–Tandem Mass Spectrometry for the Determination of Tobacco-Specific Nitrosamines in Hair Samples" Molecules 26, no. 7: 2056. https://doi.org/10.3390/molecules26072056