AOAC SPIFAN Nutrients ERP (December 7, 2022)

Amino-06 (SLV) 10-2022 FOR ERP USE ONLY DO NOT DISTRIBUTE

Table 11. Repeatability of Spiking experiments

Spiking Level

Sample Name

Low 8,30 0,11 1,32 ≤5% 9,23 0,15 1,58 ≤5% 8,54 0,11 1,24 ≤5% Yes Yes

Medium

High

Mean result (mg/100 g)

55,05

104,90

S r

0,90 1,63 ≤5%

1,32 1,26 ≤5%

NIST RM 8261

RSD r

SMPR requirement RSD r

Meets SMPR requirement RSD r

Yes

Yes

Mean result (mg/100 g)

54,26

104,28

S r

0,39 0,72 ≤5%

1,24 1,19 ≤5%

NIST RGTM 10175

RSD r

SMPR requirement RSD r

Meets SMPR requirement RSD r

Yes

Yes

Mean result (mg/100 g)

54,63

106,28

S r

0,44 0,80 ≤5%

1,80 1,69 ≤5%

NIST SRM 1869

RSD r

SMPR requirement RSD r

Meets SMPR requirement RSD r

Yes

Yes

Yes

The analysis of taurine in the supplied SPIFAN kit samples was also analyzed at a different laboratory using the same method. The laboratory analyzed the samples once in duplicate. With this extra datapoints the intermediate precision (iR) was determined. Intermediate precision variables are three technicians, three different LC-MS systems, two different HILIC columns and two different laboratories. From the results of both laboratories the intermediate precision of the method was determined. The intermediate precision was calculated using one sided ANOVA. The determined RSD of the intermediate precision of the method ranged between 1,3-6,7%. The results are summarized in table 12. Experimental data can be found in appendix C4.

Table 12. Intermediate precision

Sample Name NIST RM 8260 NIST RM 8261

Mean Result (mg/100 g)

S iR

RSD iR (%)

4,56 3,57 4,38 3,84 4,63 6,24

0,29 0,09 0,06 0,09 0,31 0,19

6,3 2,4 1,3 2,4 6,7 3,0

NIST RGTM 10175 NIST SRM 1869 NIST SRM 1849b

Liquid IFT

F. Accuracy

The accuracy of the method was determined by accepted reference values and spike recovery experiments. Reference materials NIST SRM 1869 and 1849a were used to assess the accuracy of the method based on their reference values of taurine. Both reference materials were analyzed on three days in triplicate according to the AOAC SLV Guidelines. The determined accuracy of the method with NIST SRM 1849a is in good agreement with the reference value. The accuracy of the method with NIST SRM 1869 is lower than expected. Although the determined result is still within 95% uncertainty of the reference value a small bias

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