AOAC SPIFAN ERP Reviewer Forms (March 16, 2017)

FOR EXPERT REVIEW PANEL USE ONLY

NOT FOR DISTRIBUTION

which appeared to have a low bias, likely related to incomplete elution of biotin from the

immunoaffinity column, however their results were included in the data set.

14 different product types were analyzed in duplicate over two separate days. Two practice

samples were analyzed by all 12 laboratories. The 12 remaining samples were analyzed by 9

laboratories. For biotin, relative to the SMPR, all 14 samples appeared to fall into the higher mass

fraction range of > 1mcg/100g reconstituted product.

•

The values for RSDr ranged from 2.3% to 7.0%. Without excluding any data, 12 of the 14

samples met the SMPR requirement of RSDr ≤ 6%. The Study Director noted that for each

of the 2 samples which exceeded this limit, the removal of 1 laboratory’s data set would

reduce the RSDr to < 6%. No formal outlier testing was performed, and the data was

simply presented as a whole.

•

The values for RSD

ranged from 3.0% to 9.5%. Without excluding any data, all 14 samples

met the SMPR requirement of RSD

≤ 12%.

With respect to accuracy, SRM-1849a was included in the MLT sample set and was analyzed by 9

laboratories on 2 different days: 17 of the 18 values produced fell within the certified mass fraction

range for the material (199 ± 13 mcg/100g), and the grand mean was within 1.5% of the certified

mass fraction value.

With respect to biocytin, the Study Director noted that the compound was not detected by any

laboratory in any samples. Since biocytin had not been included in the original SLV, it was unclear

whether the compound was present in the sample matrices but not recovered, or simply absent in

the samples. Upon inquiry, the Study Director provided SLV data in which 2 SPIFAN matrices were

spiked on 1 day, in duplicate, at each of 2 levels, in which average recovery ranged from 90% - 99%,

appearing to satisfy the SMPR criteria.

•

System suitability:

Not stated.

Recommendation:

Add system suitability and calculations. Although the entire SPIFAN set was not spiked, acceptable for

First Action status.

3/2017: To remain faithful to the SMPR requirement for “determination of total biotin” the

quantification of biocytin should be added to the existing 2016.02. The updated language concerning

sample elution of the immunoaffinity column, calculations, and system suitability should all be added to

the method: Acceptable for Final Action status.

From:

George Joseph [mailto

Sent:

Tuesday, March 07, 2017 1:50 PM

To:

Scott Christiansen

Subject:

RE: Biotin / Biocytin