Assessment of a New GC-MS/MS System for the Confirmatory Measurement of PCDD/Fs and (N)DL-PCBs in Food under EU Regulation
Abstract
:1. Introduction
2. Materials and Methods
2.1. Standards and Chemicals
2.2. Samples and Certified Reference Material
2.3. Sample Preparation
2.4. Instrumentation and Measurements
2.5. Method Validation Criteria
3. Results and Discussion
3.1. Gas Chromatography-Triple Quadrupole Mass Spectrometry (GC-QQQMS/MS) Method Development
3.2. Method Validation and Regulatory EU 2017/664-771 Compliance
3.3. Quality Controls and Performance Comparison with a Routine Gas Chromatography-High Resolution Mass Spectrometry (GC-HRMS) Method
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Native Congeners | Retention Time (min) | Lowest Cali. Point (pg/μL) | Lowest Cali. Point RSD (%) | Highest Cali. Point (pg/μL) | Determination Coef. (R2) | Average RRF | Difference (%) RRF (Lowest Point)-RRF (All) | iLOQ (pg/μL) |
---|---|---|---|---|---|---|---|---|
PCDDs | ||||||||
2,3,7,8-TCDD | 29.41 | 0.05 | 1.9 | 10 | 0.99998 | 1.35 | 8.7 | 0.028 |
1,2,3,7,8-PeCDD | 34.61 | 0.05 | 15 | 10 | 0.9999 | 1.07 | 4.5 | 0.046 |
1,2,3,4,7,8-HxCDD | 41.11 | 0.1 | 11.6 | 20 | 0.99996 | 1.16 | 22.7 | 0.168 |
1,2,3,6,7,8-HxCDD | 41.3 | 0.1 | 15 | 20 | 0.9993 | 1.18 | −3.6 | 0.094 |
1,2,3,7,8,9-HxCDD | 41.76 | 0.1 | 8.3 | 20 | 0.99999 | 1.19 | 6.3 | 0.103 |
1,2,3,4,6,7,8-HpCDD | 45.5 | 0.1 | 15 | 20 | 0.99998 | 1.38 | −25.5 | 0.06 |
OCDD | 49.97 | 0.25 | 12.3 | 50 | 0.9999 | 1.04 | 8.3 | 0.164 |
PCDFs | ||||||||
2,3,7,8-TCDF | 28.81 | 0.05 | 11.4 | 10 | 0.9998 | 1.24 | −12.7 | 0.032 |
1,2,3,7,8-PeCDF | 32.99 | 0.05 | 10.9 | 10 | 0.99999 | 1.09 | 1.8 | 0.051 |
2,3,4,7,8-PeCDF | 34.24 | 0.05 | 10.2 | 10 | 0.99997 | 1.1 | 6.4 | 0.033 |
1,2,3,4,7,8-HxCDF | 39.33 | 0.1 | 9.9 | 20 | 0.99999 | 1.03 | −5.2 | 0.09 |
1,2,3,6,7,8-HxCDF | 39.61 | 0.1 | 10.2 | 20 | 0.99998 | 1.07 | −3 | 0.053 |
2,3,4,6,7,8-HxCDF | 40.84 | 0.1 | 6 | 20 | 0.99999 | 1.23 | 7.6 | 0.066 |
1,2,3,7,8,9-HxCDF | 42.33 | 0.1 | 8 | 20 | 0.999 | 1.03 | −8.5 | 0.11 |
1,2,3,4,6,7,8-HpCDF | 44.1 | 0.1 | 11.9 | 20 | 0.9999 | 1.29 | 3.9 | 0.075 |
1,2,3,4,7,8,9-HpCDF | 46.3 | 0.1 | 9.5 | 20 | 0.99996 | 1.2 | 7.1 | 0.1 |
OCDF | 50.33 | 0.25 | 8.2 | 50 | 0.9988 | 1.13 | 1.6 | 0.273 |
NO-PCBs | ||||||||
PCB 77 | 24.76 | 0.5 | 4.8 | 20 | 0.9997 | 1.1 | −5.2 | 0.118 |
PCB 81 | 25.33 | 0.5 | 6.5 | 20 | 0.9997 | 1.17 | −7.5 | 0.057 |
PCB 126 | 29.72 | 0.5 | 4.3 | 20 | 0.9999 | 1.37 | −0.3 | 0.253 |
PCB 169 | 34.41 | 0.5 | 8 | 20 | 0.9999 | 1.12 | −3.2 | 0.397 |
MO-PCBs | ||||||||
PCB 123 | 26.37 | 0.4 | 3.7 | 140 | 0.9913 | 1.2 | 14.1 | 0.774 |
PCB 118 | 26.57 | 0.4 | 2.5 | 140 | 0.9908 | 1.26 | 15.8 | 0.233 |
PCB114 | 27.16 | 0.4 | 6.3 | 140 | 0.995 | 1.19 | 6.6 | 0.756 |
PCB 105 | 27.98 | 0.4 | 6.8 | 140 | 0.9976 | 1.25 | 14.6 | 0.226 |
PCB 167 | 30.68 | 0.4 | 5.1 | 140 | 0.9926 | 1.15 | 15.1 | 0.121 |
PCB 156 | 32.01 | 0.4 | 9.2 | 140 | 0.9928 | 1.13 | 15.5 | 0.255 |
PCB 157 | 32.31 | 0.4 | 13.7 | 140 | 0.9998 | 1.21 | 11.7 | 0.494 |
PCB 189 | 37.16 | 0.4 | 10.1 | 140 | 0.9998 | 1.14 | 14.1 | 0.119 |
NDL-PCBs | ||||||||
PCB 28 | 17.95 | 0.4 | 7.5 | 500 | 0.9963 | 0.78 | 17 | 0.21 |
PCB 52 | 19.23 | 0.4 | 8 | 500 | 0.9914 | 1.21 | 14.3 | 0.176 |
PCB 101 | 23.29 | 0.4 | 7.8 | 500 | 0.9961 | 1.31 | 19.8 | 0.13 |
PCB 153 | 27.64 | 0.4 | 14.9 | 500 | 0.9906 | 1.05 | −4.9 | 0.434 |
PCB 138 | 29.13 | 0.4 | 4.5 | 500 | 0.9908 | 0.98 | 2.5 | 0.235 |
PCB 180 | 32.92 | 0.4 | 12 | 500 | 0.9927 | 0.99 | −12.5 | 0.249 |
plant origins ng WHO2005TEQ/kg | |||||||
PCDD/Fs | Regulation | Average | SD | RSD % | Target | Bias % | MSE |
ML | 0.75 | 0.573 | 0.018 | 3.21 | 0.584 | −1.88 | 0.00035 |
ML/2 | 0.38 | 0.126 | 0.003 | 2.41 | 0.117 | 7.69 | 0.00009 |
2ML | 1.5 | 1.166 | 0.012 | 1.06 | 1.168 | −0.15 | 0.00011 |
animal origins (fat) ng WHO2005TEQ/kg | |||||||
PCDD/Fs | Regulation | Average | SD | RSD % | Target | Bias % | MSE |
ML | 1.5 | 1.72 | 0.055 | 3.21 | 1.75 | −1.95 | 0.00308 |
ML/2 | 0.75 | 0.378 | 0.009 | 2.41 | 0.35 | 7.87 | 0.00084 |
2ML | 3 | 3.52 | 0.037 | 1.06 | 3.5 | 0.34 | 0.00115 |
plant origins ng WHO2005TEQ/kg | |||||||
DL-PCBs and PCDD/Fs | Regulation | Average | SD | RSD % | Target | Bias % | MSE |
ML | 1.25 | 1.375 | 0.014 | 1.02 | 1.372 | 0.28 | 0.00014 |
ML/2 | 0.625 | 0.654 | 0.019 | 2.85 | 0.665 | −1.77 | 0.00024 |
2ML | 2.5 | 6.152 | 0.103 | 1.67 | 6.247 | −1.52 | 0.00714 |
animal origins (fat) ng WHO2005TEQ/kg | |||||||
DL-PCBs and PCDD/Fs | Regulation | Average | SD | RSD % | Target | Bias % | MSE |
ML | 2 | 1.961 | 0.056 | 2.846 | 1.996 | −1.77 | 0.00407 |
ML/2 | 1 | 0.493 | 0.01 | 2.016 | 0.47 | 4.82 | 0.00048 |
2ML | 4 | 4.126 | 0.042 | 1.017 | 4.115 | 0.28 | 0.00129 |
Analytes | Measured Values | SD | RSD (%) | Certified Values * | Accuracy (%) |
---|---|---|---|---|---|
2,3,7,8-TCDD | 0.26 | 0.025 | 10 | 0.25(0.03) | 105 |
1,2,3,7,8-PeCDD | 0.85 | 0.057 | 7 | 0.79(0.04) | 107 |
1,2,3,4,7,8-HxCDD | 0.34 | 0.018 | 5 | 0.42(0.07) | 81 |
1,2,3,6,7,8-HxCDD | 0.65 | 0.071 | 11 | 0.98(0.11) | 66 |
1,2,3,7,8,9-HxCDD | 0.28 | 0.024 | 8 | 0.34(0.05) | 83 |
2,3,7,8-TCDF | 0.04 | 0.004 | 10 | 0.05(0.03) | 82 |
1,2,3,7,8-PeCDF | 0.06 | 0.005 | 8 | 0.054(0.013) | 114 |
2,3,4,7,8-PeCDF | 1.49 | 0.152 | 10 | 1.81(0.13) | 82 |
1,2,3,4,7,8-HxCDF | 0.91 | 0.073 | 8 | 0.94(0.04) | 97 |
1,2,3,6,7,8-HxCDF | 1.06 | 0.074 | 7 | 1.01(0.09) | 105 |
2,3,4,6,7,8-HxCDF | 0.97 | 0.051 | 5 | 1.07(0.05) | 90 |
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Franchina, F.A.; Lazzari, E.; Scholl, G.; Focant, J.-F. Assessment of a New GC-MS/MS System for the Confirmatory Measurement of PCDD/Fs and (N)DL-PCBs in Food under EU Regulation. Foods 2019, 8, 302. https://doi.org/10.3390/foods8080302
Franchina FA, Lazzari E, Scholl G, Focant J-F. Assessment of a New GC-MS/MS System for the Confirmatory Measurement of PCDD/Fs and (N)DL-PCBs in Food under EU Regulation. Foods. 2019; 8(8):302. https://doi.org/10.3390/foods8080302
Chicago/Turabian StyleFranchina, Flavio Antonio, Eliane Lazzari, George Scholl, and Jean-François Focant. 2019. "Assessment of a New GC-MS/MS System for the Confirmatory Measurement of PCDD/Fs and (N)DL-PCBs in Food under EU Regulation" Foods 8, no. 8: 302. https://doi.org/10.3390/foods8080302