6. AOACSPIFANMethods-2018Awards

225

142 C ampos G iménez & M artin : J ournal of AOAC I nternational V ol . 100, N o . 1, 2017 remaining 22 laboratories reported valid data. The full set of original data is listed in Table 1, whereas the results of the statistical evaluation are presented in Table 2. No significant differences could be observed between laboratories using HPLC (5) or UHPLC (6) conditions, when suitability conditions were respected (i.e., the separation of orotic acid and isoascorbic acid from ascorbic acid). In general, the precision results (repeatability and reproducibility) were well within the limits stated in Standard Method Performance Requirement (SMPR ® ) 2012.012 (8). Two samples showed much higher variability (RSD>25%) than the SMPR. By excluding these values from the statistical evaluation, repeatability ranged from 1.4 to 7.3% and reproducibility from 3.2 to 11.4%. HorRat values were all <2 (0.4–1.7). Part 3

Action status because the high repeatability and reproducibility values had been obtained in two samples [infant formula RTF (milk-based) and adult nutritional powder (low-fat)].

The ERP offered the method authors the opportunity to test fresh samples from the new SPIFAN kit. Additional multi- laboratory testing (MLT) on these two matrixes was therefore organized (part 3). Twelve laboratories agreed to participate in this study. Two did not receive samples due to customs restrictions. The remaining 10 laboratories reported valid data, which are presented in Table 3. After statistical analysis ( see Table 4), the results for the adult nutritional powder (low-fat) product were well within

These results were submitted to the AOAC Expert Review Panel (ERP) in January 2015. Based on the aforementioned data, the method was not recommended to move forward to Final

Table 1. Full set of original data a

Adult nutritional powder (milk protein-based)

Infant formula RTF (milk-based)

Adult nutritional powder (low-fat)

Adult nutritional RTF (high-protein)

Infant formula powder (part. hyd., soy-based) d

Child formula powder

Infant formula powder (soy-based)

Infant elemental powder

Lab No.

Adult nutritional RTF (high-fat) b SRM 1849a c

1 14.3 13.7 8.3 8.2 5.1 2.5 3.0 6.3 4.0 10.4 2.5 3.0 12.6 5.1 21.8 21.4 32.8 28.0 19.5 20.4 2 16.8 15.9 8.1 8.0 4.9 3.7 4.5 6.2 9.8 9.9 3.7 4.5 9.1 5.3 20.2 19.9 28.4 31.4 19.7 19.6 3 16.5 15.9 7.8 8.0 4.7 2.3 2.3 6.3 9.7 10.1 2.3 2.3 12.4 11.2 18.7 18.8 31.9 27.7 19.5 19.0 4 17.3 16.0 7.9 7.7 4.6 3.1 3.1 5.9 10.1 10.0 3.1 3.1 8.5 13.3 19.8 20.5 35.8 35.6 18.5 18.8 5 19.0 17.2 8.2 8.0 5.1 4.5 3.1 6.3 10.3 10.3 4.5 3.1 8.6 13.0 19.9 19.1 28.7 33.7 19.1 19.4 6 18.8 19.1 8.5 7.5 4.9 4.9 4.0 6.2 9.6 9.9 4.9 4.0 15.8 7.8 20.1 20.1 36.0 42.4 19.5 20.0 7 17.8 17.4 7.9 8.2 4.9 6.2 4.0 6.4 10.0 9.9 6.2 4.0 12.9 4.8 19.8 19.6 30.6 35.2 19.0 19.4 8 19.8 19.6 9.5 9.3 5.0 2.4 4.3 6.7 10.3 6.8 2.4 4.3 9.0 13.2 20.9 20.2 32.9 32.8 16.2 17.8 9 17.5 19.5 7.9 8.7 4.8 3.4 3.3 6.5 11.0 11.1 3.4 3.3 14.9 14.7 16.5 20.7 36.3 40.4 21.7 21.1 10 18.6 19.1 8.3 8.1 4.8 2.5 3.0 6.6 10.8 10.2 2.5 3.0 13.4 13.3 20.9 20.1 36.0 35.5 19.7 19.5 11 19.5 19.3 9.0 9.3 5.2 5.1 3.3 7.1 11.7 11.8 5.1 3.3 14.3 14.5 21.4 20.7 37.7 34.4 20.6 20.4 12 12.8 12.8 8.4 8.1 4.5 2.5 2.4 6.0 10.1 10.0 2.5 2.4 4.9 4.9 15.9 15.7 27.1 32.8 18.3 18.5 13 16.8 16.6 7.9 7.7 5.1 5.4 2.7 6.4 10.5 10.4 5.4 2.7 NA e NA 18.3 18.4 NA NA 19.2 19.7 14 15.1 16.7 7.8 7.7 4.8 3.5 1.8 6.4 9.2 9.1 3.5 1.8 14.9 15.9 16.3 16.8 32.1 33.7 17.8 18.8 15 20.4 21.4 8.3 8.5 5.3 7.2 5.1 7.4 11.7 10.2 7.2 5.1 14.8 11.9 24.0 23.2 41.1 40.6 22.3 24.0 16 19.4 18.4 8.5 8.2 5.1 2.9 4.5 6.7 10.9 11.0 2.9 4.5 13.8 5.8 20.4 20.3 36.8 32.0 20.7 20.6 17 NA NA 8.7 8.0 3.8 3.6 NA 6.1 7.8 8.4 NA NA 12.9 13.0 NA NA 37.6 36.2 15.9 16.4 18 19.1 19.5 8.5 8.4 5.3 3.0 2.9 6.0 10.7 10.5 3.0 2.9 9.3 14.0 21.9 18.9 36.9 37.5 21.4 21.2 19 17.2 18.4 6.9 7.7 4.9 4.5 3.6 6.4 10.3 10.7 4.5 3.6 12.9 3.1 20.5 18.2 34.1 31.7 20.1 19.9 20 19.1 18.2 10.1 10.0 5.8 2.2 2.3 7.3 9.3 11.4 2.2 2.3 13.0 7.2 19.4 19.4 36.6 32.7 21.0 20.8 21 16.0 17.9 7.3 NA 4.7 NQ f 2.7 6.2 9.7 9.7 NQ 2.7 11.3 12.0 17.5 17.6 25.8 29.3 18.5 18.6 22 16.4 17.2 8.1 8.0 5.1 5.5 4.2 6.2 10.6 10.6 5.5 4.2 11.0 6.2 20.6 20.5 33.8 35.1 18.3 17.9 a  All results are in mg/100 g of reconstituted powder (25 g+200 g of water) or are as-is for RTF products. b  RTF=Ready-to-feed. c  SRM=Standard Reference Material (www.nist.gov/srm). d  part. hyd.=Partially hydrolyzed.

e  NA=Not analyzed. f  NQ=Below the LOQ.