Mycotoxin Program

2014 AAFCO Check Sample
Mycotoxins Program
Samples Engineered to Contain Relevant
Concentrations of Significant Mycotoxins.
The Samples
Source the base feed.
70,000 lb
Masters Collection
 Carefully sourced feeds naturally
contaminated with Mycotoxins.
Materials thoroughly
processed with regard to
particle size and blending.
 Incubated to raise concentration.
 Homogenous Samples for
distribution.
 Certificate of Analysis and
homogeneity data.
In Sacramento Last Summer:
I reported on Sample 201461, Poultry Feed.
Our First Sample!
Two More Samples Completed Last Year:
•
201462, Swine Feed (Issue Date: August 31st)
•
201463, Cattle Feed (Issue Date: October 31st)
All 3 Samples Reported:
•
Using a Reference Lab Assigned Value for Measure of Location
•
Horwitz %RSD – Measure of Dispersion
We will talk about the “Learning Curve”
3 Samples so Far in 2014
Number of Labs Participating
Poultry Feed
Swine Feed
Cattle Feed
Code
Analyte (ppb)
201461 (23 Labs)
201462 (25 Labs)
201463 (26 Labs)
600
Total Aflatoxin
17
20
23
601
AB1
8
11
7
602
AB2
8
10
7
603
AG1
7
11
7
604
AG2
7
9
7
610
Deoxynivalenol
17
20
10
620
Total Fumonisin
13
13
14
621
FB1
8
5
6
622
FB2
8
5
6
623
FB3
3
2
3
630
Ochratoxin A
9
13
15
640
T-2
8
9
9
650
Zearalenone
14
16
18
3 Samples so Far in 2014
Assigned Values (Reference Lab)
Poultry Feed
Swine Feed
Cattle Feed
201461 (23 Labs)
201462 (25 Labs)
201463 (26 Labs)
Code
Analyte (ppb)
600
Total Aflatoxin
20.1
21.5
42.6
601
AB1
18.5
20.0
40.2
602
AB2
1.6
1.5
1.7
603
AG1
ND (0.5)
ND (0.5)
0.7
604
AG2
ND (0.5)
ND (0.5)
ND (0.5)
610
Deoxynivalenol
1,200
830
2,700
620
Total Fumonisin
1,900
2,100
1,800
621
FB1
1,300
1,500
1,400
622
FB2
400
400
270
623
FB3
200
200
140
630
Ochratoxin A
44.0
85.7
188.9
640
T-2
236.8
46.9
244.6
650
Zearalenone
242.3
183.9
250.6
Tracking Z Scores:
Reference Lab vs
Participant Consensus
Measure of Location XA
Sample 201461 (218 Detects)
Reference
Consensus
Compliant Z
68.8%
67.9%
Warning Z
12.4%
12.8%
Actionable Z
18.8%
19.3%
Sample 201462 (237 Detects)
Z=
X LAB − X A
σ ffp
Reference
Consensus
Compliant Z
69.6%
72.6%
Warning Z
13.5%
13.1%
Actionable Z
16.9%
14.3%
Sample 201463 (252 Detects)
Horwitz Used as the
Measure of Dispersion
σffp in Both Cases
Reference
Consensus
Compliant Z
55.2%
68.7%
Warning Z
17.1%
10.3%
Actionable Z
27.8%
21.0%
Sample 201463 Cattle Feed
Detail Tracking Z Scores For The Mycotoxins:
Reference Lab vs Participant Consensus, Measure of Location
Participant Consensus
Reference Lab
Detects
Value
Compliant
Warning
Actionable
Value
Compliant
Warning
Actionable
Total Aflatoxin
46
36
91.3%
4.3%
4.3%
43
89.1%
8.7%
2.2%
AB1
14
34
85.7%
0.0%
14.3%
40
85.7%
0.0%
14.3%
AB2
12
1.9
83.3%
16.7%
0.0%
1.7
75.0%
16.7%
8.3%
AG1
2
100.0%
0.0%
0.0%
1
100.0%
0.0%
0.0%
AG2
0
Deoxynivalenol
44
2,114
56.8%
9.1%
34.1%
2,700
52.3%
13.6%
34.1%
Total Fumonisin
28
2,428
60.7%
10.7%
28.6%
1,800
32.1%
10.7%
57.1%
FB1
12
1,860
75.0%
16.7%
8.3%
1,400
66.7%
0.0%
33.3%
FB2
12
560
83.3%
16.7%
0.0%
270
0.0%
33.3%
66.7%
FB3
6
279
83.3%
16.7%
0.0%
140
33.3%
0.0%
66.7%
Ochratoxin A
30
162
53.3%
13.3%
33.3%
189
46.7%
23.3%
30.0%
T-2
14
161
42.9%
14.3%
42.9%
245
28.6%
28.6%
42.9%
Zearalenone
32
216
59.4%
12.5%
28.1%
251
46.9%
40.6%
12.5%
ND (0.5)
Let’s Look at Some Data Distribution Charts
For Sample 201463, Cattle Feed
Reference Lab vs Participant Consensus
Compare Measure of Location
Relative to Data Detects
0.009
Reference Lab Normal
0.008
Consensus Normal
0.007
0.006
0.005
0.004
0.003
0.002
Ref.
LAB
Consensus
0.001
0
-8
-7
-6
-5
-4
-3
-2
-1
0
1
2
3
4
5
6
7
8
Total Aflatoxin (ppb) Code: 600 - In Sample # 201463, Cattle Feed
Kernel Density Envelope Detected Values Relative to Normal Horwitz Curve
Issue Date: 10/31/2014
0.06
Robust Normal
Kernel Envelope
Data
Reference Lab Normal
Reference Lab Location
0.05
0.04
0.03
0.02
0.01
0
Z
ppb
-8
-7
-27.28
-6
-5
-11.49
-4
4.30
-3
-2
20.09
-1
0
35.88
1
# Methods Used
Assigned Value 35.884 (ppb)
Horwitz SD
7.90 (ppb)
Reference Lab 42.600 (ppb)
Horwitz SD
9.37 (ppb)
Kernel Bandwidth
Number of Non-Detects
Number of Detects
Participating Labs
Note: Area Under the Kernel Envelope is Identical to Area Under Horwitz Normal Curve within the chart.
2
51.67
3
4
67.46
5
6
83.25
7
10
5.92 (ppb)
0
46
18
Unique LOD's at:
8
99.04
AB1 (ppb) Code: 601 - In Sample # 201463, Cattle Feed
Kernel Density Envelope Detected Values Relative to Normal Horwitz Curve
Issue Date: 10/31/2014
0.06
Robust Normal
Kernel Envelope
Data
Reference Lab Normal
Reference Lab Location
0.05
0.04
0.03
0.02
0.01
0
Z
ppb
-8
-7
-25.79
-6
-5
-10.86
-4
4.07
-3
-2
19.00
-1
0
33.93
1
# Methods Used
Assigned Value 33.932 (ppb)
Horwitz SD
7.47 (ppb)
Reference Lab 40.200 (ppb)
Horwitz SD
8.84 (ppb)
Kernel Bandwidth
Number of Non-Detects
Number of Detects
Participating Labs
Note: Area Under the Kernel Envelope is Identical to Area Under Horwitz Normal Curve within the chart.
2
48.86
3
4
63.79
5
6
78.72
7
3
5.60 (ppb)
0
14
7
Unique LOD's at:
8
93.65
AB2 (ppb) Code: 602 - In Sample # 201463, Cattle Feed
Kernel Density Envelope Detected Values Relative to Normal Horwitz Curve
Issue Date: 10/31/2014
1.2
Robust Normal
Kernel Envelope
Data
Reference Lab Normal
Reference Lab Location
1
0.8
0.6
0.4
0.2
0
Z
ppb
-8
-7
-1.46
-6
-5
-0.62
-4
-3
0.23
-2
1.08
-1
0
1.92
1
# Methods Used
Assigned Value 1.922 (ppb)
Horwitz SD
0.42 (ppb)
Reference Lab 1.700 (ppb)
Horwitz SD
0.37 (ppb)
Kernel Bandwidth
Number of Non-Detects
Number of Detects
Participating Labs
Note: Area Under the Kernel Envelope is Identical to Area Under Horwitz Normal Curve within the chart.
2
2.77
3
4
3.61
5
6
4.46
7
8
5.31
3
0.32 (ppb)
2
12
7
Unique LOD's at:
1 (ppb)
Deoxynivalenol (ppb) Code: 610 - In Sample # 201463, Cattle Feed
Kernel Density Envelope Detected Values Relative to Normal Horwitz Curve
Issue Date: 10/31/2014
0.0014
Robust Normal
Kernel Envelope
Data
Reference Lab Normal
Reference Lab Location
0.0012
0.001
0.0008
0.0006
0.0004
0.0002
0
Z
ppb
-8
-303.60
-7
-6
300.80
-5
-4
905.20
-3
-2
-1
1,509.60
0
1
2,114.00
# Methods Used
Assigned Value 2114 (ppb)
Horwitz SD
302.20 (ppb)
Reference Lab 2700 (ppb)
Horwitz SD
371.94 (ppb)
Kernel Bandwidth
Number of Non-Detects
Number of Detects
Participating Labs
Note: Area Under the Kernel Envelope is Identical to Area Under Horwitz Normal Curve within the chart.
2
3
2,718.40
4
5
3,322.80
6
7
3,927.20
7
226.65 (ppb)
0
44
22
Unique LOD's at:
8
4,531.60
Total Fumonisin (ppb) Code: 620 - In Sample # 201463, Cattle Feed
Kernel Density Envelope Detected Values Relative to Normal Horwitz Curve
Issue Date: 10/31/2014
0.0016
Robust Normal
Kernel Envelope
Data
Reference Lab Normal
Reference Lab Location
0.0014
0.0012
0.001
0.0008
0.0006
0.0004
0.0002
0
Z
ppb
-8
-291.20
-7
-6
388.60
-5
-4
-3
1,068.40
-2
-1
1,748.20
0
1
2,428.00
# Methods Used
Assigned Value 2428 (ppb)
Horwitz SD
339.90 (ppb)
Reference Lab 1800 (ppb)
Horwitz SD
263.56 (ppb)
Kernel Bandwidth
Number of Non-Detects
Number of Detects
Participating Labs
Note: Area Under the Kernel Envelope is Identical to Area Under Horwitz Normal Curve within the chart.
2
3
3,107.80
4
5
3,787.60
6
7
4,467.40
5
254.93 (ppb)
0
28
14
Unique LOD's at:
8
5,147.20
FB1 (ppb) Code: 621 - In Sample # 201463, Cattle Feed
Kernel Density Envelope Detected Values Relative to Normal Horwitz Curve
Issue Date: 10/31/2014
0.002
Robust Normal
Kernel Envelope
Data
Reference Lab Normal
Reference Lab Location
0.0018
0.0016
0.0014
0.0012
0.001
0.0008
0.0006
0.0004
0.0002
0
Z
ppb
-8
-308.00
-7
-6
234.00
-5
-4
776.00
-3
-2
-1
1,318.00
0
1
1,860.00
# Methods Used
Assigned Value 1860 (ppb)
Horwitz SD
271.00 (ppb)
Reference Lab 1400 (ppb)
Horwitz SD
212.90 (ppb)
Kernel Bandwidth
Number of Non-Detects
Number of Detects
Participating Labs
Note: Area Under the Kernel Envelope is Identical to Area Under Horwitz Normal Curve within the chart.
2
3
2,402.00
4
5
2,944.00
6
7
3,486.00
2
203.25 (ppb)
0
12
6
Unique LOD's at:
8
4,028.00
FB2 (ppb) Code: 622 - In Sample # 201463, Cattle Feed
Kernel Density Envelope Detected Values Relative to Normal Horwitz Curve
Issue Date: 10/31/2014
0.008
Robust Normal
Kernel Envelope
Data
Reference Lab Normal
Reference Lab Location
0.007
0.006
0.005
0.004
0.003
0.002
0.001
0
Z
ppb
-8
-7
-221.92
-6
-26.57
-5
-4
-3
168.79
-2
-1
364.14
0
559.50
1
# Methods Used
Assigned Value 559.5 (ppb)
Horwitz SD
97.68 (ppb)
Reference Lab 270.0 (ppb)
Horwitz SD
52.60 (ppb)
Kernel Bandwidth
Number of Non-Detects
Number of Detects
Participating Labs
Note: Area Under the Kernel Envelope is Identical to Area Under Horwitz Normal Curve within the chart.
2
754.86
3
4
950.21
5
6
7
1,145.57
2
73.26 (ppb)
0
12
6
Unique LOD's at:
8
1,340.92
FB3 (ppb) Code: 623 - In Sample # 201463, Cattle Feed
Kernel Density Envelope Detected Values Relative to Normal Horwitz Curve
Issue Date: 10/31/2014
0.014
Robust Normal
Kernel Envelope
Data
Reference Lab Normal
Reference Lab Location
0.012
0.01
0.008
0.006
0.004
0.002
0
Z
ppb
-8
-7
-153.79
-6
-45.49
-5
-4
62.80
-3
-2
-1
171.10
0
279.40
1
# Methods Used
Assigned Value 279.4 (ppb)
Horwitz SD
54.15 (ppb)
Reference Lab 140.0 (ppb)
Horwitz SD
30.11 (ppb)
Kernel Bandwidth
Number of Non-Detects
Number of Detects
Participating Labs
Note: Area Under the Kernel Envelope is Identical to Area Under Horwitz Normal Curve within the chart.
2
387.70
3
4
496.00
5
6
604.29
7
1
40.61 (ppb)
0
6
3
Unique LOD's at:
8
712.59
Ochratoxin A (ppb) Code: 630 - In Sample # 201463, Cattle Feed
Kernel Density Envelope Detected Values Relative to Normal Horwitz Curve
Issue Date: 10/31/2014
0.014
Robust Normal
Kernel Envelope
Data
Reference Lab Normal
Reference Lab Location
0.012
0.01
0.008
0.006
0.004
0.002
0
Z
ppb
-8
-7
-110.50
-6
-42.50
-5
-4
25.50
-3
-2
93.50
-1
0
161.50
1
# Methods Used
Assigned Value 161.5 (ppb)
Horwitz SD
34.00 (ppb)
Reference Lab 188.9 (ppb)
Horwitz SD
38.83 (ppb)
Kernel Bandwidth
Number of Non-Detects
Number of Detects
Participating Labs
Note: Area Under the Kernel Envelope is Identical to Area Under Horwitz Normal Curve within the chart.
2
229.50
3
4
297.50
5
6
365.50
7
4
25.50 (ppb)
0
30
14
Unique LOD's at:
8
433.50
T-2 (ppb) Code: 640 - In Sample # 201463, Cattle Feed
Kernel Density Envelope Detected Values Relative to Normal Horwitz Curve
Issue Date: 10/31/2014
0.009
Robust Normal
Kernel Envelope
Data
Reference Lab Normal
Reference Lab Location
0.008
0.007
0.006
0.005
0.004
0.003
0.002
0.001
0
Z
ppb
-8
-7
-109.98
-6
-42.34
-5
-4
25.31
-3
-2
92.95
-1
0
160.60
1
# Methods Used
Assigned Value 160.6 (ppb)
Horwitz SD
33.82 (ppb)
Reference Lab 244.6 (ppb)
Horwitz SD
48.36 (ppb)
Kernel Bandwidth
Number of Non-Detects
Number of Detects
Participating Labs
Note: Area Under the Kernel Envelope is Identical to Area Under Horwitz Normal Curve within the chart.
2
228.25
3
4
295.89
5
6
363.54
7
8
431.18
3
25.37 (ppb)
4
14
9
Unique LOD's at:
200 (ppb)
1000 (ppb)
Zearalenone (ppb) Code: 650 - In Sample # 201463, Cattle Feed
Kernel Density Envelope Detected Values Relative to Normal Horwitz Curve
Issue Date: 10/31/2014
0.01
Robust Normal
Kernel Envelope
Data
Reference Lab Normal
Reference Lab Location
0.009
0.008
0.007
0.006
0.005
0.004
0.003
0.002
0.001
0
Z
ppb
-8
-7
-132.11
-6
-45.08
-5
-4
41.94
-3
-2
-1
128.97
0
216.00
1
# Methods Used
Assigned Value 216 (ppb)
Horwitz SD
43.51 (ppb)
Reference Lab 251 (ppb)
Horwitz SD
49.37 (ppb)
Kernel Bandwidth
Number of Non-Detects
Number of Detects
Participating Labs
Note: Area Under the Kernel Envelope is Identical to Area Under Horwitz Normal Curve within the chart.
2
303.03
3
4
390.06
5
6
477.08
7
8
564.11
5
32.64 (ppb)
4
32
18
Unique LOD's at:
0 (ppb)
500 (ppb)
Now the Question is:
“What do we want our Z Score to tell us?”
0.009
Reference Lab Normal
0.008
1.
Should we be assessed
against a single Reference
Lab Assigned Value?
Consensus Normal
0.007
0.006
0.005
2.
Should we be assessed
against our best estimate of
the center of all the data?
0.004
Lab
DATA
0.003
Ref.
LAB
0.002
Consensus
0.001
0
-8
-7
-6
-5
-4
-3
-2
-1
0
Z
1
2
3
4
5
6
7
8
2014 Mycotoxin CSP
Ochratoxin Methods (Bias?)
Ochratoxin A (ppb) Code: 630 - In Sample # 201463, Cattle Feed
Kernel Density Envelope Detected Values Relative to Normal Horwitz Curve
Issue Date: 10/31/2014
0.014
Robust Normal
Kernel Envelope
Data
Reference Lab Normal
Reference Lab Location
Bimodal Data Distribution
0.012
0.01
0.008
0.006
0.004
0.002
0
Z
ppb
-8
-7
-110.50
-6
-42.50
-5
-4
25.50
-3
-2
93.50
-1
0
161.50
1
# Methods Used
Assigned Value 161.5 (ppb)
Horwitz SD
34.00 (ppb)
Reference Lab 188.9 (ppb)
Horwitz SD
38.83 (ppb)
Kernel Bandwidth
Number of Non-Detects
Number of Detects
Participating Labs
Note: Area Under the Kernel Envelope is Identical to Area Under Horwitz Normal Curve within the chart.
2
229.50
3
4
297.50
5
6
365.50
7
4
25.50 (ppb)
0
30
14
Unique LOD's at:
8
433.50
Issue Date: 10/31/2014
Mycotoxin Proficiency Testing
Analytes for Sample # 201463 Cattle Feed
Lab #
0660
0958
0959
0957
2050
0964
2060
2033
0003
0001
0227
0918
0553
2023
0964
Code
630.01
630.01
630.01
630.01
630.01
630.01
630.23
630.23
630.01
630.23
630.01
630.23
630.23
630.20
630.21
Analyte
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Method
Neogen Veratox for Ochratoxin
Neogen Veratox for Ochratoxin
Neogen Veratox for Ochratoxin
Neogen Veratox for Ochratoxin
Neogen Veratox for Ochratoxin
Neogen Veratox for Ochratoxin
LC-MS/MS
LC-MS/MS
Neogen Veratox for Ochratoxin
LC-MS/MS
Neogen Veratox for Ochratoxin
LC-MS/MS
LC-MS/MS
LC
LC post-col photochem der. Fl
Result 1
39.7
41
52.2
95.3
86.1
97.8
155.4
180
203
211
222
228
206.1
317
285.5
Result 2
34.1
41.8
69.3
44.9
88.8
100.2
170.7
190
203
210
209
218
241
272
333.5
Detect ?
D1 D2
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Probability
LOD
of Detection
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
Z Score
-3.67
-3.53
-2.96
-2.69
-2.18
-1.84
0.04
0.69
1.22
1.44
1.59
1.81
1.82
3.91
4.35
Robust
Value
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
Horwitz
34
34
34
34
34
34
34
34
34
34
34
34
34
34
34
Issue Date: 08/31/2014
Mycotoxin Proficiency Testing
Analytes for Sample # 201462 Swine Feed
Lab #
0660
0958
0957
0959
2033
0001
0964
2060
0218
0918
2023
0964
0227
Code
630.01
630.01
630.01
630.01
630.23
630.23
630.01
630.23
630.23
630.23
630.20
630.21
630.01
Analyte
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Method
Neogen Veratox for Ochratoxin
Neogen Veratox for Ochratoxin
Neogen Veratox for Ochratoxin
Neogen Veratox for Ochratoxin
LC-MS/MS
LC-MS/MS
Neogen Veratox for Ochratoxin
LC-MS/MS
LC-MS/MS
LC-MS/MS
LC
LC post-col photochem der. Fl
Neogen Veratox for Ochratoxin
Result 1
23.9
28.6
32.4
42.7
42.25
63.44
64.9
80.7
83
96.9
154
128
195
Result 2
32.7
32.6
30.6
38.6
43.55
60.27
75.2
77.1
87
89.5
117
187
161
Detect ?
D1 D2
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Probability
LOD
of Detection
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
Z Score
-2.64
-2.49
-2.43
-1.81
-1.66
-0.39
0.16
0.76
1.17
1.72
4.56
6.04
7.42
Robust
Value
67.646
67.646
67.646
67.646
67.646
67.646
67.646
67.646
67.646
67.646
67.646
67.646
67.646
Horwitz
14.882
14.882
14.882
14.882
14.882
14.882
14.882
14.882
14.882
14.882
14.882
14.882
14.882
Issue Date: 05/31/2014
Mycotoxin Proficiency Testing
Analytes for Sample # 201461 Poultry Feed
Lab #
0660
0964
0957
2060
2033
0918
0218
0553
0001
Code
630.01
630.01
630.01
630.23
630.23
630.23
630.23
630.23
630.23
Analyte
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Method
Neogen Veratox for Ochratoxin
Neogen Veratox for Ochratoxin
Neogen Veratox for Ochratoxin
LC-MS/MS
LC-MS/MS
LC-MS/MS
LC-MS/MS
LC-MS/MS
LC-MS/MS
Result 1
22.9
26.1
29.6
27.757
36
41.7
49.38
47.96
Result 2
24.4
27.3
25.9
30.97
39.21
40.5
49.77
51.28
51.23
Detect ?
D1 D2
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
N
Y
Probability
LOD
of Detection
50
100%
100%
100%
100%
100%
100%
100%
100%
3.36%
Z Score
-1.53
-1.14
-1.01
-0.80
0.25
0.70
1.78
1.78
1.99
Robust
Value
35.646
35.646
35.646
35.646
35.646
35.646
35.646
35.646
35.646
Horwitz
7.842
7.842
7.842
7.842
7.842
7.842
7.842
7.842
7.842
2014 Mycotoxin CSP
Analyte Report Ordered by Z Score
Issue Date: 10/31/2014
Mycotoxin Proficiency Testing
Analytes for Sample # 201463 Cattle Feed
Lab #
0202
0004
0027
0003
0958
0033
0964
0010
0010
0957
0297
0227
0010
2050
0660
2033
0964
0959
0042
2072
0035
0035
0010
0553
0001
0964
2033
2023
2060
0918
0001
2023
0964
2060
0918
Code
600.12
600.14
600.01
600.01
600.01
600.01
600.21
600.20
600.21
600.01
600.01
600.01
600.01
600.01
600.01
600.24
600.01
600.10
600.20
600.99
600.13
600.20
600.98
601.23
601.23
601.21
601.23
601.24
601.23
601.23
602.23
602.24
602.21
602.23
602.23
Analyte
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
Total Aflatoxin (ppb)
AB1 (ppb)
AB1 (ppb)
AB1 (ppb)
AB1 (ppb)
AB1 (ppb)
AB1 (ppb)
AB1 (ppb)
AB2 (ppb)
AB2 (ppb)
AB2 (ppb)
AB2 (ppb)
AB2 (ppb)
Method
r-Biopharm Ridascreen FAST Aflat
Vicam Aflatest
Neogen Veratox Aflatoxin
Neogen Veratox Aflatoxin
Neogen Veratox Aflatoxin
Neogen Veratox Aflatoxin
LC post-col photochem der. Fl
LC
LC post-col photochem der. Fl
Neogen Veratox Aflatoxin
Neogen Veratox Aflatoxin
Neogen Veratox Aflatoxin
Neogen Veratox Aflatoxin
Neogen Veratox Aflatoxin
Neogen Veratox Aflatoxin
LC-MS/MS
Neogen Veratox Aflatoxin
TLC
LC
Miscellaneous technique
r-Biopharm Ridascreen FAST Aflat
LC
Other Rapid Test Kit
LC-MS/MS
LC-MS/MS
LC post-col photochem der. -Fl
LC-MS/MS
Vicam Aflatest, LC-Fl
LC-MS/MS
LC-MS/MS
LC-MS/MS
Vicam Aflatest, LC-Fl
LC post-col photochem der.-Fl
LC-MS/MS
LC-MS/MS
Result 1
20.4
24
31.9
28.3
31.7
30.4
33.814
32
33
31.7
34.8
36
39
37.4
37.4
34.7
40.85
40
45
40.9
49.2
51.599
70
4.31
29.8
32.114
31.8
34.3
41
45.2
1.6
1.5
1.7
2.4
2.79
Page 1 of 4
Result 2
20.4
22
24.4
28
31.8
33.4
32.358
36
35
38.1
35.9
36
33
35.2
36.9
40.3
35.95
39
38
50.5
54.328
55.48
77
6.67
26.9
30.931
37.7
36.5
35
45.8
1.4
1.6
1.427
1.7
2.29
Detect ?
D1 D2
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Probability
LOD
of Detection
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
Z Score
-1.96
-1.63
-0.98
-0.98
-0.52
-0.50
-0.35
-0.24
-0.24
-0.12
-0.07
0.01
0.01
0.05
0.16
0.20
0.32
0.46
0.71
1.24
2.01
2.24
4.76
-3.81
-0.75
-0.32
0.11
0.20
0.54
1.55
-1.00
-0.88
-0.85
0.30
1.46
Robust
Value
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
35.884
33.932
33.932
33.932
33.932
33.932
33.932
33.932
1.922
1.922
1.922
1.922
1.922
Horwitz
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.895
7.465
7.465
7.465
7.465
7.465
7.465
7.465
0.423
0.423
0.423
0.423
0.423
Lab #
2033
0553
0918
0964
0001
0553
2033
2060
2023
0964
0001
0553
0918
2033
2060
2023
2050
0202
0218
0958
0297
2023
2052
2060
0001
0553
2033
0964
0003
0918
0957
0027
0033
0959
0035
0227
0660
2072
0004
2050
0202
0958
0027
Code
602.23
602.23
603.23
603.21
603.23
603.23
603.23
603.23
603.24
604.21
604.23
604.23
604.23
604.23
604.23
604.24
610.01
610.06
610.25
610.01
610.01
610.20
610.23
610.23
610.23
610.23
610.23
610.01
610.01
610.23
610.01
610.01
610.01
610.01
610.08
610.01
610.01
610.99
620.11
620.02
620.09
620.01
620.01
Analyte
AB2 (ppb)
AB2 (ppb)
AG1 (ppb)
AG1 (ppb)
AG1 (ppb)
AG1 (ppb)
AG1 (ppb)
AG1 (ppb)
AG1 (ppb)
AG2 (ppb)
AG2 (ppb)
AG2 (ppb)
AG2 (ppb)
AG2 (ppb)
AG2 (ppb)
AG2 (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Deoxynivalenol (ppb)
Total Fumonisin (ppb)
Total Fumonisin (ppb)
Total Fumonisin (ppb)
Total Fumonisin (ppb)
Total Fumonisin (ppb)
Method
LC-MS/MS
LC-MS/MS
LC-MS/MS
LC post-col photochem der. -Fl
LC-MS/MS
LC-MS/MS
LC-MS/MS
LC-MS/MS
Vicam Aflatest, LC-Fl
LC post-col photochem der. -Fl
LC-MS/MS
LC-MS/MS
LC-MS/MS
LC-MS/MS
LC-MS/MS
Vicam Aflatest, LC-Fl
Neogen Veratox for DON
r-Biopharm Ridascreen DON
GC-MS
Neogen Veratox for DON
Neogen Veratox for DON
LC
LC-MS/MS
LC-MS/MS
LC-MS/MS
LC-MS/MS
LC-MS/MS
Neogen Veratox for DON
Neogen Veratox for DON
LC-MS/MS
Neogen Veratox for DON
Neogen Veratox for DON
Neogen Veratox for DON
Neogen Veratox for DON
r-Biopharm Ridascreen FAST DON
Neogen Veratox for DON
Neogen Veratox for DON
Miscellaneous technique
Vicam FumoniTest
Neogen Veratox for Fumonisin 5/1
r-Biopharm Ridascreen Fast Fumo
Neogen Veratox for Fumonisin
Neogen Veratox for Fumonisin
Result 1
2.9
Result 2
2.6
0.8
1
1.6
2.1
2.314
2.5
270
984
1,271
1,147
1,688
1,858
2,100
2,300
2,300
2,100
2,400
2,500
2,400
2,400
1,812
2,200
2,478
3,010
1.3
2.43
3
3
1,600
Page 2 of 4
1.7
2.1
2.451
2.4
280
984
1,199
1,751
1,661
1,591
2,030
2,000
2,100
2,370
2,200
2,100
2,350
2,400
3,160
2,900
2,756
2,290
1.3
2.5
3
3.1
1,900
Detect ?
D1 D2
Y
Y
N
N
Y
Y
N
N
N
N
N
N
N
N
N
N
N
N
N
N
N
N
N
N
N
N
N
N
N
N
N
N
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Probability
LOD
1
1
0.5
1
1
1.1
0.6
0.44
0.5
1
0.3
1
1.6
0.6
100%
98.54%
100%
2.57%
90.30%
2.57%
2.57%
0.47%
74.19%
Z Score
1.96
NoZ
1.30
NoZ
NoZ
NoZ
NoZ
NoZ
NoZ
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
-6.99
-6.99
-6.99
-6.99
-6.09
-3.74
-2.91
-2.20
-1.46
-1.29
-0.16
0.12
0.28
0.40
0.61
0.61
0.86
0.95
1.23
1.44
1.66
1.77
-7.14
-7.14
-7.14
-7.14
-2.00
of Detection
Robust
Value
1.922
1.922
0.7
0.7
0.7
0.7
0.7
0.7
0.7
ND (0.5)
ND (0.5)
ND (0.5)
ND (0.5)
ND (0.5)
ND (0.5)
ND (0.5)
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,114
2,428
2,428
2,428
2,428
2,428
Horwitz
0.423
0.423
0.154
0.154
0.154
0.154
0.154
0.154
0.154
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
302.2
339.9
339.9
339.9
339.9
339.9
Lab #
0957
0042
2052
0033
2033
0959
0964
0035
0227
2052
2033
2060
0001
0964
0553
0001
2052
2060
0553
0964
2033
2052
2060
0553
0660
0958
0959
0957
2050
0964
2060
2033
0003
0001
0227
0918
0553
2023
0964
0553
2033
0918
0001
Code
620.01
620.01
620.23
620.01
620.23
620.01
620.01
620.09
620.01
621.23
621.23
621.23
621.23
621.21
621.23
622.23
622.23
622.23
622.23
622.21
622.23
623.23
623.23
623.23
630.01
630.01
630.01
630.01
630.01
630.01
630.23
630.23
630.01
630.23
630.01
630.23
630.23
630.20
630.21
640.23
640.23
640.23
640.23
Analyte
Total Fumonisin (ppb)
Total Fumonisin (ppb)
Total Fumonisin (ppb)
Total Fumonisin (ppb)
Total Fumonisin (ppb)
Total Fumonisin (ppb)
Total Fumonisin (ppb)
Total Fumonisin (ppb)
Total Fumonisin (ppb)
FB1 (ppb)
FB1 (ppb)
FB1 (ppb)
FB1 (ppb)
FB1 (ppb)
FB1 (ppb)
FB2 (ppb)
FB2 (ppb)
FB2 (ppb)
FB2 (ppb)
FB2 (ppb)
FB2 (ppb)
FB3 (ppb)
FB3 (ppb)
FB3 (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
Ochratoxin A (ppb)
T-2 (ppb)
T-2 (ppb)
T-2 (ppb)
T-2 (ppb)
Method
Result 1
Neogen Veratox for Fumonisin
1,900
Neogen Veratox for Fumonisin
2,400
LC-MS/MS
2,296
Neogen Veratox for Fumonisin
2,200
LC-MS/MS
2,630
Neogen Veratox for Fumonisin
3,300
Neogen Veratox for Fumonisin
2,925
r-Biopharm Ridascreen Fast Fumo 2,938
Neogen Veratox for Fumonisin
3,000
LC-MS/MS
1,679
LC-MS/MS
1,720
LC-MS/MS
1,758
LC-MS/MS
1,770
LC-Fl, OPA der.
2,494
LC-MS/MS
2,139
LC-MS/MS
382
LC-MS/MS
419.9
LC-MS/MS
515.8
LC-MS/MS
509.9
LC-Fl, OPA der.
650.9
LC-MS/MS
780
LC-MS/MS
197.4
LC-MS/MS
298.5
LC-MS/MS
301.8
Neogen Veratox for Ochratoxin
39.7
Neogen Veratox for Ochratoxin
41
Neogen Veratox for Ochratoxin
52.2
Neogen Veratox for Ochratoxin
95.3
Neogen Veratox for Ochratoxin
86.1
Neogen Veratox for Ochratoxin
97.8
LC-MS/MS
155.4
LC-MS/MS
180
Neogen Veratox for Ochratoxin
203
LC-MS/MS
211
Neogen Veratox for Ochratoxin
222
LC-MS/MS
228
LC-MS/MS
206.1
LC
317
LC post-col photochem der. Fl
285.5
LC-MS/MS
25.72
LC-MS/MS
118
LC-MS/MS
126
LC-MS/MS
180
Page 3 of 4
Result 2
1,600
2,050
2,154
2,450
2,440
2,200
2,690
2,833
3,000
1,605
1,650
1,692
1,768
2,466
3,307
403
376.4
479.7
723.4
793.2
680
173.2
276.9
428.6
34.1
41.8
69.3
44.9
88.8
100.2
170.7
190
203
210
209
218
241
272
333.5
29.34
107
119
171
Detect ?
D1 D2
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Y
Probability
LOD
of Detection
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
100%
Z Score
-2.00
-0.60
-0.60
-0.30
0.31
0.95
1.12
1.34
1.68
-0.81
-0.65
-0.50
-0.34
2.29
3.18
-1.71
-1.65
-0.63
0.58
1.66
1.75
-1.74
0.15
1.58
-3.67
-3.53
-2.96
-2.69
-2.18
-1.84
0.04
0.69
1.22
1.44
1.59
1.81
1.82
3.91
4.35
-3.93
-1.42
-1.13
0.44
Robust
Value
2,428
2,428
2,428
2,428
2,428
2,428
2,428
2,428
2,428
1,860
1,860
1,860
1,860
1,860
1,860
559.5
559.5
559.5
559.5
559.5
559.5
279.4
279.4
279.4
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
161.5
160.6
160.6
160.6
160.6
Horwitz
339.9
339.9
339.9
339.9
339.9
339.9
339.9
339.9
339.9
271
271
271
271
271
271
97.678
97.678
97.678
97.678
97.678
97.678
54.149
54.149
54.149
34
34
34
34
34
34
34
34
34
34
34
34
34
34
34
33.823
33.823
33.823
33.823
Detect ?
Probability
Robust
Lab #
Code
Analyte
Method
Result 1 Result 2 D1 D2
LOD
of Detection Z Score
Value
Horwitz
0202
640.05 T-2 (ppb)
r-Biopharm Ridascreen FAST T-2
238.9
235.9
Y
Y
100%
2.27
160.6
33.823
0964
640.01 T-2 (ppb)
Neogen Veratox T-2 / HT-2
8,418
8,659
Y
Y
100%
247.70
160.6
33.823
0227
640.01 T-2 (ppb)
Neogen Veratox T-2 / HT-2
40,100
40,760
Y
Y
100%
1190.59
160.6
33.823
0555
640.23 T-2 (ppb)
LC-MS/MS
N
N
1000
0.00%
NoZ
160.6
33.823
2060
640.23 T-2 (ppb)
LC-MS/MS
N
N
200
12.18%
NoZ
160.6
33.823
0957
650.01 Zearalenone (ppb)
Neogen Veratox Zearalenone
0.183
0.195
Y
Y
100%
-4.96
216
43.514
0553
650.24 Zearalenone (ppb)
LC-MS/MS
79.03
71.35
Y
Y
100%
-3.24
216
43.514
0202
650.06 Zearalenone (ppb)
r-Biopharm Ridascreen FAST Zear 103.2
104.1
Y
Y
100%
-2.58
216
43.514
0918
650.24 Zearalenone (ppb)
LC-MS/MS
118
141
Y
Y
100%
-1.99
216
43.514
2033
650.24 Zearalenone (ppb)
LC-MS/MS
147.5
148
Y
Y
100%
-1.57
216
43.514
0227
650.01 Zearalenone (ppb)
Neogen Veratox Zearalenone
168
151
Y
Y
100%
-1.30
216
43.514
2052
650.24 Zearalenone (ppb)
LC-MS/MS
205.4
135.2
Y
Y
100%
-1.05
216
43.514
0003
650.01 Zearalenone (ppb)
Neogen Veratox Zearalenone
255
213
Y
Y
100%
0.41
216
43.514
0035
650.07 Zearalenone (ppb)
r-Biopharm Ridascreen FAST Zear 295.8
176.9
Y
Y
100%
0.47
216
43.514
0033
650.01 Zearalenone (ppb)
Neogen Veratox Zearalenone
254
227
Y
Y
100%
0.56
216
43.514
0027
650.01 Zearalenone (ppb)
Neogen Veratox Zearalenone
264
284
Y
Y
100%
1.33
216
43.514
0001
650.24 Zearalenone (ppb)
LC-MS/MS
285
309
Y
Y
100%
1.86
216
43.514
0660
650.01 Zearalenone (ppb)
Neogen Veratox Zearalenone
302
293.1
Y
Y
100%
1.87
216
43.514
2023
650.20 Zearalenone (ppb)
LC
358.1
292.6
Y
Y
100%
2.51
216
43.514
2060
650.24 Zearalenone (ppb)
LC-MS/MS
359.2
353.4
Y
Y
100%
3.22
216
43.514
0964
650.01 Zearalenone (ppb)
Neogen Veratox Zearalenone
383.1
391.2
Y
Y
100%
3.93
216
43.514
0958
650.01 Zearalenone (ppb)
Neogen Veratox Zearalenone
N
N
0
100.00%
NoZ
216
43.514
0555
650.24 Zearalenone (ppb)
LC-MS/MS
N
N
500
0.00%
NoZ
216
43.514
Notes: Interpreting Z Scores: Red indicates a normally distributed Z value >3 or <-3 (requires action), Orange = Z between 2 and 3 or -2 and -3 (warning) and Green = Z < 2
and >-2 (OK at 95%). If only 1 of 2 results detected Z for that is Grey and Probability of Detection is for the Non-Detect (see documentation). A Red NoZ indicates both
results Not Detected with a Probability Of Detecting a single value.
Where the Assigned Value is ND then the LOD follows as (LOD) in the Analyte units.
Page 4 of 4
Revised Mycotoxin Proposal
Recommendations
 Use Robust Consensus to Calculate Z Scores.
 Where There is Minimal Data Use Reference Lab to Calculate
Z Scores.
 Continue to Collect Reference Lab Homogeneity Data.
 Continue to Use Horwitz Relationship to Estimate σp (fit for
purpose).
 Continue to Calculate Probability of Detection for Non Detects.
 Include Analyte Report in the Data Reporting Website
Comments?
Dog Food # 201464
 Ship Date ~ 12/20/2014
 Data Due 01/10/2015
 Reports Available 01/31/2015
THANK YOU!