6. AOACSPIFANMethods-2018Awards
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270 S CHIMPF ET AL . : J OURNAL OF AOAC I NTERNATIONAL V OL . 101, N O . 1, 2018
Table 4. Lycopene precision data
cis -Lycopene isomers, µg/100 g RTF
Total lycopene, µg/100 g RTF
trans -Lycopene, µg/100 g RTF
RSD r
RSD r
RSD r
,
RSD R , %
,
RSD R , %
,
RSD R , %
n
%
%
%
Product description/Batch No.
NA a
Infant GOS/FOS powder/50350017W1 Infant elemental powder/00795RF Child milk powder 1/00866RF00 Adult low-fat powder/00859RF00
NA NA NA NA NA NA NA NA NA NA
NA NA NA NA NA
NA NA NA NA NA NA NA NA NA NA
NA NA NA NA NA
NA NA 6 NA NA 6 NA NA 6 NA NA 6 NA NA 6
NA NA NA NA
Infant hydrolyzed soy powder/410457651Z
Infant formula stage 1 milk powder/4044755861 SRM1849a powder/CLC10-B Infant milk powder/K16NTAV
NA
NA NA
NA
NA NA
NA
NA NA 6
NA NA
NA NA NA NA 6.01 6.53 3.29 9.82 NA NA NA NA 11.7 35.2
NA NA
NA NA NA NA 4.97 7.20 3.05 10.7 NA NA NA NA 3.75 7.75
NA NA
NA NA 6 NA NA 6 5.36 6.61 12 3.01 10.3 12 NA NA 12 NA NA 12 4.67 7.73 12 NA NA 12 3.61 4.29 12 NA NA 12
Infant milk RTF 1/38300
4.16 7.58
3.42 16.9
7.57
SRM 1869 powder/CLC16-B
24.49
Adult high-protein RTF/00730RF00
NA NA
NA NA
NA NA
Adult high-fat RTF/00729RF00
Adult high-fat RTF spiked/00729RF00
0.02
0.82
0.83
Infant soy powder/E10NWZC
NA
NA NA
NA
NA NA
NA
Infant soy powder spiked/E10NWZC
0.05
21.2 39.6
1.81
3.64 4.79
1.86
Infant partially hydrolyzed milk powder/410057652Z Infant partially hydrolyzed milk powder spiked/410057652Z
NA
NA NA
NA
NA NA
NA
0.09
10.8 26.6
3.55
6.30 5.71
3.65
6.37 5.52 12
Infant milk RTF 2/EV4H2R
NA NA
NA NA NA NA
NA NA
NA NA NA NA
NA NA
NA NA 12 NA NA 12
Child milk powder 2/4052755861
a NA = Not Applicable. No peaks detected.
( j) Guard column holder. — YMC Part No. XPGCH-Q1. (k) HPLC system. — Binary or quaternary gradient pump with degasser, autosampler capable of injecting 50 µL, thermostatted column compartment, and UV-Vis detector (Agilent 1290 Infinity II with 60 mm flow cell) or equivalent. (l) HPLC vials. — Amber with 300 µL inserts. No split septa. (m) Light shields. — Yellow with cutoff of 440 nm. (n) N-evap. — With water bath or equivalent nitrogen evaporator. (o) Ice for cooling. (p) Pipettor. — Variable volume, 250 µL. (q) Pasteur pipets. (r) Spectrophotometer.
B. Apparatus and Materials
(a) Balance, analytical. — Minimum weighing capacity of 0.00001 g. (b) Balance, top-loading. — Minimumweighing capacity of 0.01 g. (c) Beakers. — Assorted sizes. (d) Bottle-top dispenser. — Capable of dispensing 10 mL. (e ) Centrifuge. (f) Centrifuge tubes. — 50 mL glass with Teflon-coated caps. (g) Cylinders. — Graduated glass, assorted sizes. (h) Column. — C30 3 µm, 4.6 × 250 mm; YMC Carotenoid Part No. CT99S032546WT or equivalent. (i) Guard column. — C30 guard column; 3 µm, 4.6 × 10 mm; YMC Part No. CT99S03-0104GC or equivalent (optional).
Table 5. Carotenoid spike recovery data
Analyte
Product
Spike concn, µg/100 g
Recovery, %
RSD, %
Lutein
Adult high-fat RTF/00729RF00 Infant soy powder/E10NWZC
~10 ~25 ~50 ~10 ~25 ~50 ~0.8
95.3 93.9 90.3
5.42 4.36 4.89 6.87 6.48 5.17 6.94 4.18 6.19
Infant partially hydrolyzed milk/410057652Z
b -Carotene
Adult high-fat RTF/00729RF00 Infant soy powder/E10NWZC
108
89.3 93.8
Infant partially hydrolyzed milk/410057652Z
Lycopene
Adult high-fat RTF/00729RF00 Infant soy powder/E10NWZC
102
~2
97.3
Infant partially hydrolyzed milk/410057652Z
~4.5
109
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