66 / 112
128
l,rrpo
l:.t
/\t...,:Jot-jllNAl-
ot;,,\OAC
INI-tiRNAl'toN/\l-
\,ir¡_.9(r.
No.
t.2013
Table
11.
Cooked hamburger accuracy and
precision
from
independent laboratory
F¡nal
result,
ppm
Recovery.
Yo
Repli
æte
Target
concn
ppm
Neogen
Q
Labs
sample
Dilut¡on
(QL) lD
No.
lD
No.
factor
0.0
10.0
20.0
1
2
3
4
Ã
'I
;-r
2n
3n
4n
5n
7
8
I
10
6n
7n
8n
9n
10n
11
12
IJ
14
15
1ln
12n.
13n
14n
15n
16
17
18
20
tbn
17n
18n
19n
20n
21
22
4481
1.0
3893
1.0
3517
1.0
2762
1.0
1724
1.0
i\i
'
O
JOOS
LU
3999
1.0
1663
1
.0
4440
1.0
1429
1.0
1649
i
.0
4183
1
,0
2351
1.0
3197
1.0
269
1.0
1481
I .0
2007
1.0
939
1.0
691
1.0
4137
1.0
3710
1
.0
4731
1.0
1888
1_0
3675
1.0
1670
1
.0
1370
1.0
4360
1.0
4353
1.0
3442
1.0
3435
1,0
4226
'1.0
86
1.0
'1905
1
.0
1895
1
.0
460
1.0
901
1.0
3823
1.0
4891
1.0
1711
'f
.0
4464
1_0
1423
1.0
2680
1.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
0.0
c.8
c.5
o.2
0,5
0.7
0.2
0,6
0.6
0.5
0.4
oâ
ô1
9.5
9.4
9.6
8.8
7.5
7.9
4.7
5.1
4.9
5.1
4.5
4.7
5.1
5_1
4.9
4.8
11.9
11,9
11
.8
12.3
13.5
12.7
12.0
12.4
12.3
12.4
8.1
7.3
8.3
9.4
7
.5
8.0
7.5
7.9
18.7
19.8
19.2
19.4
19.0
19.4
17
.5
18.3
20.2
19.8
23.2
20.9
21.9
23.4
21.7
20.8
21
.0
21.1
25.2
23.1
36.8
33.5
30,0
28.5
29.5
27
3
NA"
NA
NA
NA
NA
NA
NA
NA
NA
NA
li;',
li/r
NA
NA
NA
NA
NA
NA
NA
NA
186
186
190
188
150
158
94
102
98
102
90
94
102
102
98
96
'119
119
118
123
1
35
127
120
124
81
73
83
94
73
88
75
80
75
79
91
99
96.5
96.5
95
96.5
87.5
91,5
101
99
116
104_5
1
09.5
117
1
08.5
104
1
05
105.5
1?6
1
1
5.5
92
83.8
75
71.3
738
683
Table
11.
(continuedl
Final result.
ppm
Recovery
%
Replicate
Target
concn,
Q Labs
ppm
(QL)
lD
No.
Neogen
sample
Dilution
lD
No.
factor
77
74.5
80
66
82
83.8
86.8
85.5
87.8
89.8
84.3
86.3
i
/
ó
/9
3
'
NA
= Not applicable.
lnternal
Validation Studies
All
anal¡,ses
\\'cre generated
liom
one
kil
lot
unle ss
specilìed.
Spike
and Recovery (Repeatability and Recovery)
Blind-coded samplcs
uelc
prepared
liom
each
ol
eight
gluten-lree
producls spiked
at
various
levels (unspikcd.
5.0.
10.0.
and 25.0 ppnr)
as
described
in
Reference lt,Íalerictl Used
in
Standard Pt'epãrdt¡on
and
Spiking section
of
this
document.
Each
sarnple rvas
ertracted
and
iudependerrtly analt'zed
bv
three
individual
technicians
in
the sanie
laborator¡,.
using
the
same
reader. Each
technicialt
extracted and analr,zcd
a separate
sample
set.
(a)
7Þsting.-'I'he
above preparations
were
tested
f'ollorving
procedure
set
tbrth
rn Sanple
Preparation
an¿l
Extaclion,
Proc'etlural
Nofes,
Precoulions, Analysis,
and
Interprelulion
of
lles¡rlfs
sections
of
this docurneltt.
(b)
Resu/ts.-1-he
evaluation
of
sarnple
exllacts for
recoverv
indicates
an
average
ol'
I
I3.70%
recover\¡ at 5.0
ppm.
lll.60%
recover)/
at
l0
ppm.
at'ul 106.70Yo
recovery at 25 ppm
(Table
l)
across
all
m¿rlrixes.
An
overall
ll0.'l\yo
recover)'
$,as
observed
across
all
levels. The evaluation
ol'the
salne
sarnple extracts
f'or
repeatabilitv indicates
a
3.409/o
RSD
at
5.0 ppnr.
a.1.00%
RSD
at
10.0
ppm, and an 8.10% RSD at 25.0 pprn
across
all
nlatrixes.
An overall
5.20% RSD s'as observed
across
all
leve ls
and
r.natrixes
(1'able
l).
Comparìson to Existing Methods
NatLrrall¡,
incurred
samples
rvere
sourcecl
at
local
stores
and
used rvhen
fbL¡ncj
1<l
contailì
rrieasurable
gliadin
levels.
Duplicate
samples
u,ere
blind-cclded
and
anal),zed
b),thrì
candidate
Velator EI-ISA
urethod
and
OMA
2012.01. ,,\ll
sarnples anal¡.zed
in triplicate
and means ir,cle compared.
(a)
7Þsting.-l'he
above preparations \\'ere tested
fòllorving
procedures
set
l-orth
ín
Sanple Pre¡taralion
ancl ExlracÍion,
Ì'
rocedural
Note
s,
P re
cauÍ
ions,
.'Nnal)ts
is,
and
Inte
rpre
tal
ion
o.[
Rcs¡¿1/s
sections
ol
this docr¡rnent
fìrr
the
Neogen method.
(b)
llc.rrr/1.s.-Data
inclicate
0.9(r
I
con'e
l¿rtion
betrr,een
the
Veratox
ELISA
method and
the
Olr4A
nethod
2012.01
24
21n
23n
24n
25n
1774
1
.0
4664
1.0
1797
'1.0
4076
1.0
4851
2.O
21
2.0
lbb4
2.u
30.8
29.8
32.O
26.4
34_7
34.2
35.1
35,9
33.7
34.5
3¡.¡ rìt