Mass Spectrometry & Spectroscopy 13
The sample with the smallest maximum permissible level (ML) was pork fat, with ML of 1.0 ng/kg TEQ. For this reason, a large difference in the quantitation values (i.e., a quantitation value ratio outside the 50% to 200% range) is possible at concentration levels at least 10 times lower than ML. However, no signifi cant difference could be seen in the quantitation performance of GC-MS/MS and GC-HRMS at the concentration level required in analyses.
Evaluation of Durability in Analysis of Actual Samples
As an evaluation of durability in analysis of dioxins in food products, actual samples and standard samples (concentration: 0.05 pg/µL) were analysed alternately, and the number of analyses possible while maintaining sensitivity was evaluated based on the transition of sensitivity for low concentration standard samples. A total of more than 500 analyses of standard samples and actual samples were carried out. Figure 3 shows the results.
for all compounds, indicating that sensitivity could be maintained through the entire test.
Conclusions
In this experiment, dioxins in more than 250 samples of approximately 40 types of food and animal feed products were analysed by GC-MS/MS using BEIS, and the quantitation performance of GC-MS/MS was evaluated by comparing the analysis results by GC-MS/MS and GC-HRMS. The results showed no difference in the quantitation performance of GC-MS/MS and GC-HRMS at the concentration level necessary in analyses.
Durability in analysis of dioxins in actual samples was also evaluated, and no decrease in sensitivity at low concentration levels occurred after more than 500 analyses.
Based on these results, we determined that BEIS with GCMS/MS has the high sensitivity necessary for dioxin analysis comparable to HRMS instruments, while also demonstrating the excellent durability of the GCMS-TQ8050.
Acknowledgement
We wish to take this opportunity to express our sincere thanks to the Laboratoire d‘Etude des Résidus et Contaminants dans les Aliments for cooperation in providing samples, guidance, and other assistance in the preparation of this paper.
Figure 3: Transition of Peak Area in Repeated Analysis.
In Figure 3, the horizontal axis shows the number of analyses and the vertical axis shows the peak area at each analysis number. No large decrease in sensitivity occurred after more than 500 analyses. Next, Table 3 shows the average peak area and repeatability from the 1st to the 530th analysis. Repeatability was less than 20% RSD
References 1.
https://www.epa.gov/dioxin/learn-about-dioxin
2.
https://www.who.int/news-room/fact-sheets/detail/dioxins-and- their-effects-on-human-health
3.
https://rais.ornl.gov/documents/dioxin_tef.pdf
4 EPA Method 1613: Tetra- through Octa-Chlorinated Dioxins and Furans by Isotope Dilution HRGC/HRMS
Table 3: Average Peak Area and Repeatability for Standard Samples Concentration 0.05 pgµL in Durability Test. I.D.
Compound name
1 2 3 4 5 6 7 8 9
10 11 12 13 14 15 16 17
2,3,7,8-Tetrachlorodibenzo-p-dioxin 1,2,3,7,8-Pentachlorodibenzo-p-dioxin 1,2,3,4,7,8-Hexachlorodibenzo-p-dioxin 1,2,3,6,7,8-Hexachlorodibenzo-p-dioxin 1,2,3,7,8,9-Hexachlorodibenzo-p-dioxin 1,2,3,4,6,7,8-Heptachlorodibenzo-p-dioxin Octachlorodibenzo-p-dioxin 2,3,7,8-Tetrachlorodibenzofuran 1,2,3,7,8-Pentachlorodibenzofuran 2,3,4,7,8-Pentachlorodibenzofuran 1,2,3,4,7,8-Hexachlorodibenzofuran 1,2,3,6,7,8-Hexachlorodibenzofuran 2,3,4,6,7,8-Hexachlorodibenzofuran 1,2,3,7,8,9-Hexachlorodibenzofuran 1,2,3,4,6,7,8-Heptachlorodibenzofuran 1,2,3,4,7,8,9-Heptachlorodibenzofuran Octachlorodibenzofuran
Average peak area 73596 60713 55956 58167 56035 51663 84614
105930 80339 88317 67814 74759 75794 67878 67665 62914
103483
STDEV 8321 8803 7025 8034 9095 7452
10814 11847 9592
10631 11761 9636 9605 6056
10199 9356
13911
%RSD(n = 17) 11.31 14.5
12.55 13.81 16.23 14.43 12.78 11.18 11.94 12.04 17.34 12.89 12.67 8.92
15.07 14.87 13.44
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