Screening Efficiency
A direct comparison of calculated WHO-PCDD/F-TEQ
in pg/g fat (or wet weight for fish) was made by analyzing
the same sample extracts on both the TSQ Quantum XLS
Ultra and the DFS HRMS. The data obtained are given
in Figure 6. Very good correlation with HRMS data was
observed in the real calculated values down to ca. 0.5
(WHO-PCDD/F-TEQ) pg/g level indicating that a highly
efficient screening method is possible with TSQ Quantum
XLS Ultra. The sensitivity and selectivity obtained with the
technique made this possible. This means, in addition to
a very low false negative rate, very few compliant samples
are likely to be directed to subsequent confirmatory analysis.
Conclusions
•
The Thermo Scientific TSQ Quantum XLS Ultra is a highly
applicable screening tool for PCDD/Fs in food and feed.
•
Strong correlation, between the results of GC-MS/MS
and GC-HRMS within acceptable limits were observed
around the level of interest for a high percentage of the
food and feed samples tested.
•
Measured ion ratios for identity confirmation are
predictable and can therefore be tested against
theoretical values.
•
A different approach for LOQ calculation (from the
signal/noise ratio, employed on HRMS systems) is
required due to the inherent low noise of the GC-MS/MS
system. For this, the lowest calibrated concentration
was used.
References
1. European Food Safety Authority; Results of the monitoring of dioxin
levels in food and feed. EFSA Journal 2010; 8(3):1385 [36 pp.].
doi:10.2903/j.efsa.2010.1385. Available online:
2. Commission Regulation (EC) No 152/2009 of 27 January 2009 (OJ L 54,
26.2.2009, p. 1–130), Commission Regulation (EC) No 1883/2006 of 19
December 2006 (OJ L 364, 20.12.2006, p. 32–43)
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Mean Recovery (%)
Relative Standard Deviation (%)
2,3,7,8-TCDF
83
11
1,2,3,7,8-PeCDF
105
12
2,3,4,7,8-PeCDF
101
13
1,2,3,4,7,8-HxCDF
106
14
1,2,3,6,7,8-HxCDF
107
15
2,3,4,6,7,8-HxCDF
104
17
1,2,3,7,8,9-HxCDF
97
17
1,2,3,4,6,7,8-HpCDF
105
18
1,2,3,4,7,8,9-HpCDF
99
18
OCDF
90
26
2,3,7,8-TCDD
87
12
1,2,3,7,8-PeCDD
105
13
1,2,3,4,7,8-HxCDD
110
13
1,2,3,6,7,8-HxCDD
108
14
1,2,3,7,8,9-HxCDD
104
16
1,2,3,4,6,7,8-HpCDD
104
17
OCDD
94
24
Table 5: Recoveries of
13
C-labeled internal PCDD/F standards for food
samples (n = 42)
Figure 5: Theoretically calculated ion ratios for SRM analysis of tetra thru
octa PCDD/F congeners in addition to the real values obtained from a
calibration sequence using the TSQ Quantum XLS Ultra. Error bars show typi-
cal ±15% QC tolerance.
Figure 6: Deviations of WHO-PCDD/F-TEQ of GC-MS/MS results of
GC-HRMS (%) for food and human milk samples
