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Histamine Testing
Histamine Testing
Histamine Testing
32
paper and wash again with H2O. Prepare resin fresh weekly and
store under H2O. Place glass wool plug in base of tube, B(a), and
slurry in enough resin to form 8 cm bed. Maintain H2O level above
top of resin bed at all times. Do not regenerate resin in packed
column; rather, use batch regeneration in beaker when necessary.
Wash column with ca 10 mL H2O before applying each extract.
Codex-AdoptedAOAC Method*
A. Principle
B. Apparatus
Rinse all plastic and glass containers with HCl (1 + 3) and H2O
before use.
(a) Chromatographic tube.200 7 id mm polypropylene tube
fitted with small plastic stopcocks and ca 45 cm Teflon tubing.
Control flow rate at >3 mL/min by adjusting height of column relative
to tubing outlet. Alternatively, use 2-way valve in place of tubing.
(b) Photofluorometer.With medium pressure Hg lamp with
excitation at 350 nm and measuring emission at 444 nm.
(c) Repipets.1 and 5 mL.
C. Reagents
Table 977.13A. Interlaboratory study results for determination of histamine in tuna by fluorometric method (based on
collaborative study results of the original method)
Test sample
Histamine,
mg/100 g
Avg. histamine
found, mg/100 g
sr
RSDr, %
sR
RSDR,
%
HorRat
1.4
0.643
46.9
1.009
73.6
26
25.8
0.950
3.7
1.383
5.4
0.54
30
31.6
2.053
6.5
3.473
11.0
0.97
20
19.8
0.941
4.7
1.729
8.7
0.65
120
125.6
6.432
5.1
8.807
7.0
0.94
200
198.8
4.801
2.4
10.6555
5.4
0.47
a
Blind duplicates.
b
Approximate composition.
Table 977.13B. Interlaboratory study results for determination of histamine in canned tuna and frozen mahimahi by fluorometric
a
method (generated for modified method using 75% (v/v) methanol)
Test sample
Mean, mg/g
sr, mg/g
sR, mg/g
9.896
0.884
0.915
1.710
1.710
1
2
13.0
RSDr, %
RSDR, %
HorRat
9.01
9.32
2.475
2.562
0.83
13.17
13.17
4.788
4.788
1.22
5.627
1.205
1.295
21.42
23.03
3.374
3.626
1.88
7.831
1.084
1.084
13.84
13.84
3.035
3.035
1.19
20.28
1.140
2.077
5.62
10.24
3.192
5.816
1.01
58.02
2.111
5.466
3.64
9.42
5.911
15.305
1.09
6.575
14.050
4.15
8.87
18.410
39.340
1.19
158.4
a
Based on results received from 16 laboratories.
b
r = 2.8 sr.
c
R = 2.8 sR.
E. Determination
Found,
mg/g
Recovered,
mg/g
Recovery,
%
10.00
9.85
9.65
8.95
9.50
9.65
11.55
9.20
9.30
10.25
10.10
10.00
10.70
69.00
66.00
63.30
62.20
67.00
72.40
55.00
58.10
58.40
55.10
58.10
51.80
61.40
57.80
54.10
54.10
55.60
56.10
53.00
53.00
54.30
54.30
59.00
59.00
53.30
53.30
59.00
56.00
53.45
52.35
57.35
62.75
46.05
49.15
48.90
45.60
48.45
42.15
49.85
46.25
44.90
44.90
46.30
46.80
42.75
42.75
44.20
44.20
49.00
49.00
42.60
42.60
117.65
111.67
106.58
104.39
114.36
125.12
91.82
98.01
97.51
90.93
96.61
84.05
99.40
92.22
89.53
89.53
92.32
93.32
85.24
85.24
88.14
88.14
97.71
97.71
84.95
98.89
96.41
Lab
Avg. rec., %
a
Added 50.15 mg histamine/g.
b
Data from Laboratories I, L, and M were excluded because results for the
background or the spike were outliers.
* Codex Stan 36-1981, Rev. 1-1995, Codex Standard for Quick Frozen
Finfish, Uneviscerated and Eviscerated. Codex Stan 70-1981, Rev.
1-1995, Codex Standard for Canned Tuna and Bonita. Codex Stan
94-1981, Rev. 1-1995, Codex Standard for Canned Sardines and
Sardine-Type Products. Codex Stan 119-1981, Rev. 1-1995, Codex
Standard for Canned Finfish. Codex Stan 165-1989, Rev. 1-1995,
Codex Standard for Quick Frozen Blocks of Fish Fillet, Minced Fish
Flesh, and Mixtures of Fillets and Minced Fish Flesh. Codex Stan
166-1989, Rev. 1-1995, Codex Standard for Quick Frozen Fish Sticks
(Fish Fingers), Fish Portions, and Fish FilletsBreaded or in Batter.
Codex Stan 190-1995, Codex General Standard for Quick Frozen Fish
Fillets.