Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) Determination of Perfluorooctane Sulfonate (PFOS) and Perfluorooctanoic Acid (PFOA) in the Yolk of Poultry Eggs in Malaysia
Abstract
:1. Introduction
2. Results
2.1. Selection of Deprotonated Ions
2.2. Assay Specificity and Selectivity
2.3. Calibration Curve and Sensitivity
2.4. Precision and Accuracy
2.5. Stability
2.6. Concentration of Perfluorinated Compounds in Yolk Samples
3. Discussion
3.1. Sample Preparation for LC-MS/MS Analysis
3.2. LC-MS/MS Method Validation
3.3. Concentration of Perfluorinated Compounds in Egg Yolk Samples
4. Materials and Methods
4.1. Chemicals
4.2. Instrumentation
4.3. Sample Collection and Preparation
4.4. Preparation of Standards and Quality Control Materials
4.5. Sample Extraction
4.6. Method Validation
4.6.1. Selectivity
4.6.2. Calibration Curve and Sensitivity
4.6.3. Accuracy and Precision
4.6.4. Recovery
4.6.5. Stability
4.7. Statistical Analysis
5. Conclusions
Author Contributions
Funding
Conflicts of Interest
References
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Sample Availability: Samples of the compounds are not available from the authors. |
Analyte | Concentration (ng g−1) | Intra-Assay (n = 5) | Inter-Assay (n = 15) | ||||
---|---|---|---|---|---|---|---|
Observed Concentration (ng g−1) | Accuracy | RSD (% CV) | Observed Concentration (ng g−1) | Accuracy | RSD (% CV) | ||
PFOS | 0.50 | 0.54 ± 0.03 | 108 | 5.01 | 0.54 ± 0.03 | 108 | 6.35 |
0.75 | 0.81 ± 0.02 | 108 | 2.03 | 0.81 ± 0.05 | 108 | 6.05 | |
7.50 | 6.85 ± 0.12 | 91.3 | 1.77 | 7.28 ± 0.50 | 97.1 | 6.91 | |
12.5 | 11.5 ± 0.28 | 92.3 | 2.42 | 11.8 ± 0.40 | 94.3 | 3.38 | |
PFOA | 0.10 | 0.11 ± 0.01 | 110 | 6.79 | 0.11 ± 0.01 | 110 | 6.25 |
0.75 | 0.67 ± 0.01 | 89.3 | 1.82 | 0.69 ± 0.03 | 92.0 | 5.06 | |
7.50 | 7.38 ± 0.82 | 98.4 | 11.1 | 8.93 ± 0.68 | 101 | 4.08 | |
12.5 | 12.3 ± 0.51 | 98.4 | 4.19 | 12.4 ± 0.51 | 99.1 | 4.08 |
Analyte | QC Concentration (ng g−1) | Time | Mean Measured Concentration, ng g−1 (n = 5) | Accuracy (%) | RSD (% CV) |
---|---|---|---|---|---|
PFOS | 0.75 | 0 hr | 0.81 ± 0.02 | 109 | 2.03 |
12 hr | 0.80 ± 0.07 | 106 | 9.29 | ||
24 hr | 0.83 ± 0.04 | 111 | 5.13 | ||
12.5 | 0 hr | 11.5 ± 0.28 | 92.3 | 2.42 | |
12 hr | 11.8 ± 0.42 | 94.2 | 3.57 | ||
24 hr | 12.1 ± 0.36 | 96.5 | 3.02 | ||
PFOA | 0.75 | 0 hr | 0.67 ± 0.01 | 89.7 | 1.82 |
12 hr | 0.73 ± 0.06 | 97.8 | 8.13 | ||
24 hr | 0.70 ± 0.03 | 93.0 | 4.82 | ||
12.5 | 0 hr | 12.3 ± 0.51 | 98.4 | 4.19 | |
12 hr | 12.2 ± 0.57 | 97.6 | 4.67 | ||
24 hr | 12.7 ± 0.40 | 101 | 3.14 |
Type | Source | Number of Yolk (n) | Concentration (ng g−1 ww) | |
---|---|---|---|---|
PFOS | PFOA | |||
Chicken Eggs (Home Produced) | ||||
1 | 3 | 0.64 | <0.10 a | |
2 | 3 | <0.50 | <0.10 | |
3 | 3 | 0.50 | <0.10 a | |
4 | 3 | <0.50 a | <0.10 a | |
5 | 3 | 1.01 | <0.10 | |
6 | 3 | 0.53 | <0.10 a | |
7 | 3 | <0.50 a | <0.10 a | |
8 | 3 | <0.50 a | <0.10 | |
9 | 3 | 0.52 | <0.10 | |
10 | 3 | <0.50 | <0.10 | |
Duck eggs | ||||
1 | 2 | <0.50 a | <0.10 | |
2 | 2 | <0.50 a | <0.10 | |
3 | 2 | <0.50 a | <0.10 a | |
Quail eggs | ||||
1 | 5 | <0.50 a | <0.10 | |
2 | 5 | 0.69 | <0.10 | |
3 | 5 | <0.50 a | <0.10 a | |
4 | 5 | <0.50 a | <0.10 a |
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Tahziz, A.; Mohamad Haron, D.E.; Aziz, M.Y. Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) Determination of Perfluorooctane Sulfonate (PFOS) and Perfluorooctanoic Acid (PFOA) in the Yolk of Poultry Eggs in Malaysia. Molecules 2020, 25, 2335. https://doi.org/10.3390/molecules25102335
Tahziz A, Mohamad Haron DE, Aziz MY. Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) Determination of Perfluorooctane Sulfonate (PFOS) and Perfluorooctanoic Acid (PFOA) in the Yolk of Poultry Eggs in Malaysia. Molecules. 2020; 25(10):2335. https://doi.org/10.3390/molecules25102335
Chicago/Turabian StyleTahziz, Atiqah, Didi Erwandi Mohamad Haron, and Mohd Yusmaidie Aziz. 2020. "Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) Determination of Perfluorooctane Sulfonate (PFOS) and Perfluorooctanoic Acid (PFOA) in the Yolk of Poultry Eggs in Malaysia" Molecules 25, no. 10: 2335. https://doi.org/10.3390/molecules25102335