AOAC Final Action Methods in 2017

P ACQUETTE & T HOMPSON : J OURNAL OF AOAC I NTERNATIONAL V OL . 101, N O . 2, 2018 559

Table 6. ( continued )

RSD r (AES versus MS)

RSD R (AES versus MS)

mg/100 g a

SMPR: <10%

MS versus AES SMPR: <5%

ICP-MS mean 0.0600 0.0658 0.0465

ICP-AES mean

ICP-MS RSD r

ICP-MS RSD R

ICP-AES RSD r

ICP-AES RSD R

Sample

Difference, %

Difference

Difference

12.3 b

Infant Powder Milk Infant Powder Soy Infant RTF Control Placebo, Infant RTF

0.061 0.068 0.046

– 1.6 – 3.5

0.9 1.0 1.2 0.9 1.0 4.7 9.2 b 6.3 b 1.4 36 b 2.2 1.7 2.4 3.2 2.5 2.0 0.8 1.1 1.4 39 b 1.2 1.3 1.6 1.1 0.9 1.0 2.0 0.5 1.1 1.2 3.4 1.7 33 b 1.2 1.5 2.9 2.5

2.7

1.8 4.2 1.2

4.6 5.2 3.7

7.7 2.9 5.5

5.2 b

8.1 9.1

1.8

2.3

32.9 b

15.6 b

70.5 b 11.3 b

0.0025 0.0036

– 37

24

55

5.2 b 4.1 21 b 8.4 b 6.2 b

4.3

4.4 5.5 7.5 29 b 4.2 99 b 5.9 7.2 4.4 4.4 3.1 5.1 4.2 3.5 4.6 4.3 3.7 58 b 5.7 4.7 4.3 3.8 4.3 2.6 5.3 4.8 2.6 4.9 24 b 3.7 50 b 4.3 4.1

7.0

Toddler Powder

0.0278 0.0052

0.029 0.007

– 3.4 – 30 – 40 – 35 – 4.0

78 b 71 b 48 b 21 b

Whole-Milk Liquid

3

73 64 19 17

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Whole-Milk Powder

0.0040 0.0060

16

Whey Powder

0.0345 0.1172 0.0042 c

0.049 0.122 0.023 0.054

2.1 4.8

Whey Protein Concentrate

b

b

Butter

7.6 b

56 b

Cheese

0.0498

– 8.1 – 8.3

4.7 5.1

50

Mean (above SMPR limit)

7.6

26.4

19.3

Zinc

Adult Low-Fat Powder

0.719

0.748

– 4.0

2.0 1.3 3.3 2.6 3.1 3.5 3.5 3.6 2.6 4.2 2.4 2.5

– 0.1 – 0.4

9.4 5.9 6.2 8.0 9.0

5.1 1.4 3.1 2.9 4.9 1.7 1.8 6.2 2.2 4.9 1.2 2.9 5.4 1.5 3.8 5.1 2.7 3.4 11

Adult High-Fat RTF

2.60

2.57 0.46 2.22

1.1

Placebo, High-Fat Adult High-Protein Placebo, High-Protein Placebo, Child Milk Child Milk Powder Child Elemental Powder Infant Elemental Powder

0.453

– 0.9 – 0.5

1.0

2.21

– 0.6

0.298 0.159 0.728 0.546 0.732 0.540 0.559 0.603 0.560 0.828 0.717 0.327 0.388 0.356 0.182 c 0.0058 c 0.0895 c

0.289 0.161 0.740 0.554 0.750 0.007 0.552 0.580 0.608 0.551 0.852 0.706 0.094 0.335 0.375 0.357 0.127 0.788 0.066

3.0

0.6 1.5 2.7 2.5 1.2 2.9 1.2 1.0 3.9 3.5 0.7 1.3 2.1 2.5 1.8 2.7 1.0 – 8

14.9 b

– 1.5 – 1.7 – 1.4 – 2.5 – 2.2 – 3.7 – 0.8 – 12

6.3 6.1

10.0

30.6 b

53.5 b

Placebo, Elemental

– 4.5

Infant, Partly Hydrolyzed Milk Infant, Partly Hydrolyzed Soy

8.0 9.5 5.6 6.6 9.7 4.1 9.0 9.9 5.3 8.2 67 b 11 b

Infant FOS/GOS powder

5.0 b

Infant Powder Milk Infant Powder Soy Infant RTF Control Placebo, Infant RTF

1.6

– 2.9

4.3 1.7

1.6

3.3 b

– 5.3 – 2.3

Toddler Powder

2.7 3.6 3.0 6.1 2.6

Whole-Milk Liquid

3.4

Whole-Milk Powder

– 0.3

Whey Powder

36

44

7.3

Whey Protein Concentrate

0.871

10.0

0.0844 c

b

b

Butter

Cheese

2.46

2.40

2.5

2.4 3.0

1.2 1.5

4.8 7.9

0.6 3.8

Mean (above SMPR limit)

– 0.1

a RTF, butter, cheese, whey protein concentrate, whey powder, and whole milk analyzed as-is; 25 g infant and adult powders and whole-milk powder reconstituted in 200 g water prior to analysis — see the METHOD section. b Results that failed SMPR criteria. c Mean results that have levels that are below the SMPR analytical range.

Conclusions

elements were adjusted upward about 2-fold, which does not at all limit the utility of the method. This method is also suitable for the analysis of dairy ingredients and milk products, such as butter, cheese and whole milk. The determination of minor/trace elements, such as Mo, Se, Cu, Mn, Fe, and Zn, in the dairy products is within scope and works very well with this method, even though the ISO/IDF working groups were originally only looking for a method to

A collaborative study has been successfully completed for Method 2015.06 , meeting all requirements of the SPIFAN SMPRs for trace and ultratrace elements in the same method. The exception was that at the SMPR lower limits for Cu, Mn, and Fe, the desired repeatability and reproducibility could not be met, and so the recommended lower limits for these