Mycotoxins: Homogeneity and Stability · Aflatoxin B2 ppb 4.56 3.23-29.2% Fail Yes Aflatoxin B1 ppb...

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Mycotoxins: Homogeneity and Stability

Transcript of Mycotoxins: Homogeneity and Stability · Aflatoxin B2 ppb 4.56 3.23-29.2% Fail Yes Aflatoxin B1 ppb...

Page 1: Mycotoxins: Homogeneity and Stability · Aflatoxin B2 ppb 4.56 3.23-29.2% Fail Yes Aflatoxin B1 ppb 51.13 46.73-8.6% Caution Yes Analytical sd Low Enough? Difference less than Allowed?

Mycotoxins:

Homogeneity and Stability

Page 2: Mycotoxins: Homogeneity and Stability · Aflatoxin B2 ppb 4.56 3.23-29.2% Fail Yes Aflatoxin B1 ppb 51.13 46.73-8.6% Caution Yes Analytical sd Low Enough? Difference less than Allowed?

51.649.110

56.353.99

40.448.08

55.349.77

53.958.96

50.945.65

53.046.64

58.354.83

55.147.22

51.942.11

Rep. 2Rep. 1Sample #

Aflatoxin B1 (ppb)

Analyte Name

Homogeneity Data

Trilogy Provides: Homogeneity Data Before Round

Mean = 51.13 ppb

%RSD Between Samples = 5.4 % (A)with Analytical variance removed.

%rsd Analytical = 6.9 %

ffp σPT, Horwitz %RSD = 22 %

Allowed %RSD = 7.3 % (B)

When we apply 95% confidence intervals, the variance due to sampling is less than the allowed variance (A < B). PASS is recorded.

Page 3: Mycotoxins: Homogeneity and Stability · Aflatoxin B2 ppb 4.56 3.23-29.2% Fail Yes Aflatoxin B1 ppb 51.13 46.73-8.6% Caution Yes Analytical sd Low Enough? Difference less than Allowed?

Homogeneity Test: Rabbit Feed 201763

ISO 13528:2015 (E) Criteria

Testingy Proficiencσ Derived from Modified Horwitz

VarianceSample BetweenS :Where 2Samples Between =

( )2Testingy Proficienc2

Samples Between σ0.3S ×≤Simply Put:

Page 4: Mycotoxins: Homogeneity and Stability · Aflatoxin B2 ppb 4.56 3.23-29.2% Fail Yes Aflatoxin B1 ppb 51.13 46.73-8.6% Caution Yes Analytical sd Low Enough? Difference less than Allowed?

6.4%PassPass543.87542.21ppbZearalenone

4.1%PassPass97.2692.71ppbHT-2 Toxin

4.2%PassPass252.50263.20ppbT-2 Toxin

7.2%PassPass10.6612.27ppbOchratoxin

21.7%PassHigh AV0.120.13ppmFumonisin B3

13.2%PassHigh AV0.170.13ppmFumonisin B2

7.4%PassHigh AV0.860.91ppmFumonisin B1

7.1%High AVPass3.043.15ppmDON

9.9%PassHigh AV3.234.56ppbAflatoxin B2

6.9%PassPass46.7351.13ppbAflatoxin B1

Within Lab Analitical sd(15 dups.)

2nd Decision

1st Decision

Stability Data

Means (5 dups.)

Homogeneity Data

Means (10 dups.)

Units

Mycotoxin Homogeneity: Rabbit Feed 201763

Page 5: Mycotoxins: Homogeneity and Stability · Aflatoxin B2 ppb 4.56 3.23-29.2% Fail Yes Aflatoxin B1 ppb 51.13 46.73-8.6% Caution Yes Analytical sd Low Enough? Difference less than Allowed?

51.649.110

56.353.99

40.448.08

55.349.77

53.958.96

50.945.65

53.046.64

58.354.83

55.147.22

51.942.11

Rep. 2Rep. 1Sample #

Aflatoxin B1Analyte Name

Homogeneity Data

Stability Data

45.646.25

45.148.44

46.546.93

48.648.82

45.745.51

Rep. 2Rep. 1Sample #

Aflatoxin B1Analyte Name

Trilogy Provides: Stability Data at End of Round

Mean Before = 51.13

Mean After = 46.73

Is this sufficient stability?

Page 6: Mycotoxins: Homogeneity and Stability · Aflatoxin B2 ppb 4.56 3.23-29.2% Fail Yes Aflatoxin B1 ppb 51.13 46.73-8.6% Caution Yes Analytical sd Low Enough? Difference less than Allowed?

Mycotoxin Stability: Rabbit Feed 201763Stability Test: from 08/09/2017 to 10/16/2017

Testingy ProficiencAfterBefore σ0.3XX ×≤−

ISO 13528:2015 (E) Criteria

Testingy Proficiencσ Derived from Modified Horwitz

Testingy Proficiencσ0.5sd Analytical ×<

All this requires that the Analytical variance is LOW enough.

Page 7: Mycotoxins: Homogeneity and Stability · Aflatoxin B2 ppb 4.56 3.23-29.2% Fail Yes Aflatoxin B1 ppb 51.13 46.73-8.6% Caution Yes Analytical sd Low Enough? Difference less than Allowed?

YesPass0.3%543.87542.21ppbZearalenone

YesPass4.9%97.2692.71ppbHT-2 Toxin

YesPass-4.1%252.50263.20ppbT-2 Toxin

YesFail-13.2%10.6612.27ppbOchratoxin

NoPass-5.1%0.120.13ppmFumonisin B3

NoFail28.2%0.170.13ppmFumonisin B2

YesCaution-5.4%0.860.91ppmFumonisin B1

YesPass-3.6%3.043.15ppmDON

YesFail-29.2%3.234.56ppbAflatoxin B2

YesCaution-8.6%46.7351.13ppbAflatoxin B1

Analytical sd Low

Enough?

Difference less than Allowed?

% Difference

Mean After

Mean Before

Units

Mycotoxin Stability: Rabbit Feed 201763Stability Test: from 08/09/2017 to 10/16/2017

Page 8: Mycotoxins: Homogeneity and Stability · Aflatoxin B2 ppb 4.56 3.23-29.2% Fail Yes Aflatoxin B1 ppb 51.13 46.73-8.6% Caution Yes Analytical sd Low Enough? Difference less than Allowed?

Comments: Trilogy provides Homogeneity and Stability data with each

sample. We continue to evaluate. This is our first look at this input. The high Analytical Variance tends to confound the analysis. We do seem to have Acceptable Homogeneity. As we get a better handle on the true analytical variance we

should be able to better identify stability issues. Perhaps we should look into more appropriate storage

conditions. Relay these conditions to clients to implement immediately on receiving the sample.

A new kind of stability test. For Now, let’s wait and see how the next couple of samples

pan out.