AOAC SPIFAN Nutrients ERP (December 7, 2022)

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

LOQ meets the requirement of AOAC SMPR 2014.013 of 0,5 mg/100g. A summary of the data can be found in table 9. Experimental data of the LOD and LOQ can be found in appendix B.

Tabel 9. LOD and LOQ

Blank Mean (mg/100 g)

0,09 0,02 0,06 0,20 0,15 0,29

Standard deviation Spiked method blank

S LOD S LOQ

LOD (mg/100g) LOQ (mg/100g)

E. Precision

The precision of the method is determined as described by AOAC SLV guidelines and represents the repeatability of the method. All samples were analyzed in duplicate over six different days with two different analysts and two different LC-MS systems. The determined repeatability of each sample can be found in table 10. The RSD of the repeatability in the analyzed samples was between 0,7-4,6% and meets the requirements set in AOAC SMPR 2014.013. The experimental data of the repeatability experiment can be found in appendix C1.

Table 10. Repeatability

SMPR requirement RSD r

Meets SMPR requirement RSD r

Mean Result (RTF basis) (mg/100 g)

Sample Name

S r

RSD r (%) n

NIST RM 8260 NIST RM 8261

4,45 3,55

0,03 0,68 0,05 1,52 0,05 1,13 0,05 1,31 0,21 4,55 0,44 3,26 0,11 1,72

12 12 12 12 12 12 12

≤7% ≤7% ≤7% ≤7% ≤7% ≤5% ≤5%

Yes Yes Yes Yes Yes Yes Yes

NIST RGTM 10175 4,38

NIST SRM 1869 NIST SRM 1849b

3,82 4,54

SPIFAN DOMY545 13,66

Liquid IFT

6,20

The repeatability was also determined from spiked samples to obtain the precision at higher concentrations. Spiked samples were analyzed on three different days in triplicate (See paragraph F). The RSD of the repeatability at spiked levels is between 0,7-1,7% and meets the SMPR 2014.013 requirements as presented in table 11. The experimental data of the repeatability assessment of the spiking experiments can be found in appendix C3.