AOAC Final Action Methods in 2018
Table 2015.09B. Trans vitamin K 1 SLV data–accuracy
Spike level
100%
50%
No. of replicates (duplicates on multiple days)
Native level, µg/100 g RTF Recovery, % RSD, %
Sample type
Recovery, % RSD, %
Child formula powder Infant elemental powder
6 6 6 6 6 6 6 6 6 6 6 6
2.66 7.57 1.11 a 3.26 7.69 8.99 2.92 6.09 6.26 9.01 9.10 10.7
98.2 93.2 104 96.4 96.6 97.9 98.0 97.6 97.9 100 96.7 98.2
5.9 7.6 2.9 2.0 3.6 1.0 2.5 1.0 1.7 1.3 2.7 1.2
96.2 94.0 95.5 95.1 91.9 96.1 95.2 102 102 104 106 93.8
7.1 2.6 1.8 1.8 3.0 2.6 2.6 2.3 0.3 0.4 0.7 4.0
SRM 1849a
Adult nutritional powder milk protein based
Infant formula powder partially hydrolyzed milk based Infant formula powder partially hydrolyzed soy based
Adult nutritional powder low fat Infant formula powder milk based Infant formula powder soy based Infant formula RTF milk based Adult nutritional RTF high protein Adult nutritional RTF high fat a Results reported as mg/kg powder.
(q) Vortex mixers . (r) Yellow lights or yellow shields with cutoff of at least 440 nm . C. Reagents (a) Acetic acid .—Glacial, ACS. (b) Helium or nitrogen .—Zero grade or equivalent (only needed if using helium or nitrogen sparge).
(c) Hexane .—HPLC grade. (d) Iso-octane (2,2,4-trimethylpentane) .—HPLC grade. (e) Isopropanol (isopropyl alcohol) .—HPLC grade. (f) Methanol .—HPLC grade. (g) Phytonadione/phylloquinone (vitamin K 1 ) .—U.S. Pharmacopeia Reference, Official Lot or equivalent primary reference standard. Store per label instructions.
Table 2015.09C. MLT trans vitamin K 1 data Sample ID
K16NTAV E10NWZC 410057652Z 410457651Z 00729RF00 00730RF00 4052755861 4044755861 00847RF00 00820RF00
Total No. of labs
8
8
8
8
8
8
8
8
8
8
Total No. of replicates
16
16
15
16
16
16
16
16
16
15
Overall mean of all data (grand mean), µg/100 g
6.16
6.19
7.74
8.24
9.28
7.00
3.61
7.24
1.37
2.85
Repeatability SD
0.132
0.135
0.231
0.188
0.208
0.501
0.111
0.205
0.028
0.138
Reproducibility SD
0.314
0.301
0.300
0.372
0.781
1.13
0.213
0.334
0.089
0.170
Repeatability RSD, % 2.15
2.18
2.98
2.28
2.24
7.16
3.08
2.83
2.03
4.81
Reproducibility RSD, %
5.11
4.86
3.87
4.52
8.42
16.1
5.88
4.61
6.50
5.94
HorRat
0.210
0.200
0.165
0.194
0.368
0.676
0.220
0.194
0.151
0.154
Sample ID
EV4H2R EV4H2Q CLC10-B a
00866RF00 00859RF00 00795RF00 50350017W1 00796RF00 00821RF00
Total No. of labs
8
8
8
8
8
8
8
8
8
Total No. of replicates
16
16
15
16
16
16
16
15
16
Overall mean of all data (grand mean), µg/100 g
6.78
1.86
1077 a
4.46
2.91
8.67
3.96
1.41
2.85
Repeatability SD
0.241
0.119
15.0
0.105
0.029
0.276
0.087
0.064
0.050
Reproducibility SD
0.361
0.198
39.5
0.195
0.095
0.834
0.177
0.114
0.159
Repeatability RSD, % 3.56
6.37
1.39
2.35
0.99
3.19
2.20
4.55
1.76
Reproducibility RSD, %
5.33
10.6
3.66
4.36
3.25
9.62
4.46
8.07
5.58
HorRat
0.222
0.365
0.231
0.121
0.084
0.294
0.121
0.188
0.144
a Results in μ g/kg powder.
© 2019 AOAC INTERNATIONAL
Made with FlippingBook HTML5