Quantification of Carbonyl Compounds Generated from Ozone-Based Food Colorants Decomposition Using On-Fiber Derivatization-SPME-GC-MS
Abstract
:1. Introduction
Study | Matrix | Analysis Method | Internal Standard | (Range of Carbon Number of) Target Carbonyls | (Range of) LOD/ppb(v) | Description of the Study |
---|---|---|---|---|---|---|
Beránek et al., 2008 [26] | Aqueous particulate matter extracts of wood smoke and diesel exhaust | GC-MS (TIC) | butanal-d2 and benzaldehyde-d6 | C1-C12 | 0.1–55 | A SPME-GC-MS method for trace analysis of a wide range of carbonyls was developed. Headspace and direct extractions from liquid phase with on-fiber derivatization were tested. Effects of extraction time and temperature were tested. |
Ethanal | 3.7 | |||||
Benzaldehyde | 2.3 | |||||
2-Furfural | 35 | |||||
Hexanal | 0.7 | |||||
Saison et al., 2008 [27] | Beer | GC-MS (TIC) | 2-heptanol and guaiacol or p-fluorobenzaldehyde | C3-C10 | 0.003–310 | Two SPME-GC-MS procedures for analysis of volatiles in beer were developed. Effects of time and temperature of PFBHA doping and derivatization, salt addition, and matrix effects were studied. |
Hexanal | 0.028 | |||||
Benzaldehyde | 0.078 | |||||
2-Furfural | 6.0 | |||||
Trenholm et al., 2008 [32] | Municipal wastewater | GC-MS (TIC/SIM) | acetone-d6 | C1 | 3.7 | A rapid and automated SPME-GC-MS method utilizing SPME autosampler was developed for formaldehyde analysis. Reproducibility and background contamination were reported. |
Tsai et al., 2003 [34] | Water (bi-distilled water, well water, chlorinated tap water) | GC-MS-(TIC) | decafluorobiphenyl | C1-C5 | 0.12–0.34 | A SPME-GC-MS method for the analysis of short chain aliphatic aldehydes was developed. Effects of time for PFBHA doping and derivatization were tested. |
Deng et al., 2004 [23] | Human blood | GC-MS (TIC/SIM) | None | C2-C7 | 0.44 × 10−4–6.0 × 10−4 | A SPME-GC-MS method was developed for the analysis of short chain aliphatic aldehydes in human blood as a diagnostic measure of cancer status. Effects of derivatization time and temperature were tested. |
Ethanal | 0.44 × 10−4 | |||||
Hexanal | 6.0 × 10−4 | |||||
Wang et al., 2005 [33] | Particle board, wine and fish | GC-MS/FID | None | C1-C9 | 2–25 | An automated SPME-GC-MS method was developed for the analysis of low-molecular mass aldehydes in the given sample. PFPH was compared with PFBHA. Limiting factor was determined to be diffusion of analytes from sample to headspace. |
Ethanal | 0.5 | |||||
Hexanal | 0.5 | |||||
This study | Wastewater (ozonated fruit leather) solution / suspension) | GC-MS (TIC/SIM) | None | C2-C7 | 0.016–0.030 | A SPME-GC-MS method was developed for the analysis of carbonyls from ozone-based food colorant decomposition. Effects of dopant concentration, derivatization temperature and time were studied. Inaccuracy from competitive derivatization was minimized with a short derivatization time. |
Ethanal | 0.030 | |||||
Hexanal | 0.029 | |||||
Benzaldehyde | 0.016 | |||||
2-Furfural | 0.016 |
2. Experimental Section
2.1. Reagents and Materials
2.2. Response Factor Calculation
2.3. On-fiber Derivatization HS-SPME
2.4. GC-MS Condition for Carbonyls Analysis
2.5. Validation of the Method
2.6. Analyses of Ozonated Fruit Leather Solution / Suspension Samples
3. Results and Discussion
3.1. Doping of PFBHA
Chemical | 2 min derivatization | 5 min derivatization | 15 min derivatization | |||
---|---|---|---|---|---|---|
P value | Significant Difference | P value | Significant Difference | P value | Significant Difference | |
Ethanal | 0.011 | N | 0.052 | N | 0.003 | Y |
Propanal | 0.003 | Y | 0.003 | Y | 0.000 | Y |
Butanal | 0.001 | Y | 0.001 | Y | 0.000 | Y |
Pentanal | 0.000 | Y | 0.084 | N | 0.008 | Y |
Hexanal | 0.399 | N | 0.021 | N | 0.000 | Y |
Octanal | 0.001 | Y | 0.002 | Y | 0.002 | Y |
Acetone | 0.016 | N | 0.018 | N | 0.002 | Y |
2-Heptanone | 0.671 | N | 0.180 | N | 0.036 | N |
2-Furfural | 0.015 | N | 0.000 | Y | 0.057 | N |
Benzaldehyde | 0.001 | Y | 0.013 | N | 0.050 | N |
3.2. Effects of Derivatization Temperature
3.3. Effects of Derivatization Time and Displacement of 2-Furfural
Chemical | Henry’s Law Constant/(M/atm) | RF | Extraction-time Linearity (R2) | Average Uptake of Carbonyls/ng e | Average RSD (%) | ||||
---|---|---|---|---|---|---|---|---|---|
2–60 min | 2–20 s | 60 min | 5 s | 2–60 min | 2–20 s | 5 s | |||
Ethanal | 15 a | 86,600 | 0.932 | 0.932 | 6.49 ± 1.82 | 1.14 ± 0.16 f | 12.7 | 10.2 | 14.4 |
Propanal | 13 a | 60,200 | 0.942 | ND | 14.01 ± 3.10 | ND | 13.7 | ND | ND |
Butanal | 8.7 a | 342,000 | 0.930 | 0.969 | 5.93 ± 1.02 | 0.05 ± 0.01 | 11.1 | 8.94 | 10.4 |
Pentanal | 6.8 a | 73.40 | 0.973 | ND | 7.39 ± 2.27 | ND | 24.6 | ND | ND |
Hexanal | 4.7 a | 64,200 | 0.973 | 0.957 | 4.50 ± 0.74 | 0.24 ± 0.02 | 12.3 | 15.9 | 7.90 |
Octanal | 1.9 a | 31,400 | 0.941 | 0.930 | 5.87 ± 1.15 | 0.34 ± 0.06 | 10.5 | 24.4 | 17.7 |
Acetone | 25 a | 112,000 | 0.968 | 0.562 | 5.29 ± 1.29 | 1.11 ± 0.05 | 8.64 | 8.43 | 4.19 |
2-Heptanone | 7.0 a | 125,300 | 0.988 | 0.825 | 1.56 ± 0.18 | 0.04 ± 0.01 | 10.8 | 25.0 | 17.3 |
2-Furfural | 263.2 b | 100,800 | 0.874 | 0.963 d | 0.51 ± 0.05 | 0.08 ± 0.00 | 29.1 | 14.3 | 1.61 |
Benzaldehyde | 42 c | 130,900 | 0.776 | 0.999 d | 3.32 ± 1.94 | 0.17 ± 0.02 | 17.1 | 14.4 | 9.34 |
3.4. Method Validation
Compound | Calibration Curve | R2 | LOD (µg/L) |
---|---|---|---|
Ethanal | y = 1.2 × 103x + 70324 | 0.9831 | 0.030 |
Hexanal | y = 9.2 × 102x + 29024 | 0.9959 | 0.029 |
2-Furfural * | y = 3.7 × 104x + 35313 | 0.9579 | 0.016 |
Benzaldehyde | y = 4.1 × 104x + 38523 | 0.9874 | 0.016 |
3.5. Ozonated Fruit Leather Solution/Suspension Sample Analysis
4. Conclusions
Acknowledgments
Author Contributions
Conflicts of Interest
References
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Zhu, W.; Koziel, J.A.; Cai, L.; Özsoy, H.D.; Van Leeuwen, J. Quantification of Carbonyl Compounds Generated from Ozone-Based Food Colorants Decomposition Using On-Fiber Derivatization-SPME-GC-MS. Chromatography 2015, 2, 1-18. https://doi.org/10.3390/chromatography2010001
Zhu W, Koziel JA, Cai L, Özsoy HD, Van Leeuwen J. Quantification of Carbonyl Compounds Generated from Ozone-Based Food Colorants Decomposition Using On-Fiber Derivatization-SPME-GC-MS. Chromatography. 2015; 2(1):1-18. https://doi.org/10.3390/chromatography2010001
Chicago/Turabian StyleZhu, Wenda, Jacek A. Koziel, Lingshuang Cai, H. Duygu Özsoy, and J. (Hans) Van Leeuwen. 2015. "Quantification of Carbonyl Compounds Generated from Ozone-Based Food Colorants Decomposition Using On-Fiber Derivatization-SPME-GC-MS" Chromatography 2, no. 1: 1-18. https://doi.org/10.3390/chromatography2010001