Dados de validao para Mercrio em Peixe

Repeatability (r) data (one analyst / three concentration levels / three different periods of analysis):
Period 1 n
Cexp
CnomAccuracy Period
(%)
2 n
Cexp
CnomAccuracy (%)
Period 3 n
at 200ng/mL 1
212.547
200.000
106at 200 ng/mL1
135.160 200.000
68 at 200 ng/mL1
2
213.750
200.000
107
2
163.600 200.000
82
2
3
214.405
200.000
107
3
155.120 200.000
78
3
4
212.716
200.000
106
4
152.905 200.000
76
4
5
230.074
200.000
115
5
172.613 200.000
86
5
6
222.605
200.000
111
6
167.254 200.000
84
6
var 1 51.00526
mean 217.683
median 214.078

Period 1 n
at 400 ng/mL1
2
3
4
5
6

Cexp
419.647
407.150
428.905
428.116
421.074
405.005

var 1 103.8815
mean 418.32
median 420.36

Period 1 n
at600 ng/mL 1
2
3
4

Cexp
616.347
650.000
634.905
716.716

median
SD

107
4

var 2 177.23
mean 157.78
median 159.36

CnomAccuracy Period
(%)
2 n
400.000
105at 400 ng/mL1
400.000
102
2
400.000
107
3
400.000
107
4
400.000
105
5
400.000
101
6
median
SD

105
3

Cexp
327.860
323.900
326.720
351.305
352.613
362.754

var 2 276.632
mean 340.86
median 339.58

CnomAccuracy Period
(%)
2 n
600.000
103at 600 ng/mL1
600.000
108
2
600.000
106
3
600.000
119
4

Cexp
524.960
459.700
468.120
528.601

median
SD

80
7

Cexp
128.688
131.004
145.544
143.737
136.327
135.718

Cnom
200.000
200.000
200.000
200.000
200.000
200.000

var 3 45.0728
mean 136.84
median 136.02

median
SD

CnomAccuracy (%)
Period 3 n
400.000
82 at 400 ng/mL1
400.000
81
2
400.000
82
3
400.000
88
4
400.000
88
5
400.000
91
6
median
SD

85
4

Cexp
271.088
260.904
272.244
270.637
273.327
259.518

Cnom
400.000
400.000
400.000
400.000
400.000
400.000

var 3 37.0325
mean 267.95
median 270.86

median
SD

CnomAccuracy (%)
Period 3 n
600.000
87 at 600 ng/mL1
600.000
77
2
600.000
78
3
600.000
88
4

Cexp
384.888
403.604
393.544
402.537

Cnom
600.000
600.000
600.000
600.000

5
6

718.670
603.905

600.000
600.000

120
101

var 1 2475.554
mean 656.76
median 642.45

median
SD

107
8

5
6

487.913
496.454

600.000
600.000

81
83

var 2 808.916
mean 494.29
median 492.18

median
SD

82
5

5
6

399.427
406.118

600.000
600.000

var 3 62.1921
mean 398.35
median 400.98

median
SD

Repeatability data for the 200 ng/mL level

Median (all values)
159.36
Mean (all values)
170.76
SD of mean
36.38
Recovery (%)
80
SD of recovery
18
Within-day precision (g/kg)
9.54
Within-day precision (%)
6
SD2 (variance of the every-day median)
1605.204
Between-day precision (g/kg)
41.00
Between-day precision (%)
26
Repeatability (g/kg) at the 95% confidence level
26.44
Repeatability (%) at the 95% confidence level 71
Repeatability data for the 400 ng/mL level
Median (all values)
339.58
Mean (all values)
342.38
SD of mean
64.14
Recovery (%)
85
SD of recovery
16
Within-day precision (g/kg)
11.80
Within-day precision (%)
3
SD2 (variance of the every-day median)
5599.529
Between-day precision (g/kg)
75.60
Between-day precision (%)
22
Repeatability (g/kg) at the 95% confidence level
32.68
Repeatability (%) at the 95% confidence level 62
Repeatability data for the 600 ng/mL level
Median (all values)
492.18
Mean (all values)
516.47
SD of mean
114.14
Recovery (%)
82

SD within-day

SD between-day
2.77*SD within-day
2.77*SD within-day

SD within-day

SD between-day
2.77*SD within-day
2.77*SD within-day

SD of recovery
Within-day precision (g/kg)
Within-day precision (%)
SD2 (variance of the every-day median)

19
33.40
7
14867.748
Between-day precision (g/kg)
125.69
Between-day precision (%)
26
Repeatability (g/kg) at the 95% confidence level
92.52
Repeatability (%) at the 95% confidence level 71

SD within-day

SD between-day
2.77*SD within-day
2.77*SD within-day

Validation data for Danofloxacin in milk

Repeatability (r) data (one analyst / three concentration levels / three different periods of analysis):
Cexp
Cnom
Cexp
Cnom
Period 1
n
Accuracy (%) Period 2
n
Accuracy (%)
at 200ng/mL

1
2
3
4
5
6

4.950
5.070
5.410
5.430
5.890
5.520

5.000
5.000
5.000
5.000
5.000
5.000

99
101
108
109
118
110

var 1
mean
median

0.112817
5.378
5.420

median
SD

108
7

at 200ng/mL

1
2
3
4
5
6

6.160
5.290
5.970
5.880
5.220
5.110

5.000
5.000
5.000
5.000
5.000
5.000

123
106
119
118
104
102

var 2
mean
median

0.20187
5.61
5.59

median
SD

112
9

Period 3
at 200ng/mL

n
1
2
3
4
5
6

Cexp
5.580
5.970
6.290
5.290
5.860
5.020

Cnom
5.000
5.000
5.000
5.000
5.000
5.000

Accuracy (%)
112
119
126
106
117
100

var 3
mean
median

0.217097
5.67
5.72

median
SD

114
9

Repeatability data for the 5.0 g/L level

Median (all values)
Mean (all values)
SD of mean
Recovery (%)
SD of recovery
Within-day precision (g/kg)
Within-day precision (%)
2
SD (variance of the every-day median)
Between-day precision (g/kg)
Between-day precision (%)
Repeatability (g/kg) at the 95% confidence level
Repeatability (%) at the 95% confidence level

Period 1
at 400 ng/mL

n
1
2
3
4
5
6

Cexp
8.920
11.700
10.000
11.500
11.400
10.800

Cnom
10.000
10.000
10.000
10.000
10.000
10.000

var 1
mean
median

1.1592
10.72
11.10

median
SD

n
1
2
3
4
5
6

Cexp
15.900
16.900
17.100
16.400
16.900
16.400

Cnom
15.000
15.000
15.000
15.000
15.000
15.000

var 1
mean
median

0.2
16.60
16.65

median
SD

Accuracy (%) Period 2

89
at 400 ng/mL
117
100
115
114
108
111
11

n
1
2
3
4
5
6

Cexp
11.100
9.500
11.500
11.300
9.610
10.400

Cnom
10.000
10.000
10.000
10.000
10.000
10.000

Accuracy (%)
111
95
115
113
96
104

var 2
mean
median

0.754817
10.57
10.75

median
SD

108
9

n
1
2
3
4
5
6

Cexp
16.400
16.000
15.800
14.600
14.200
16.000

Cnom
15.000
15.000
15.000
15.000
15.000
15.000

Accuracy (%)
109
107
105
97
95
107

var 2
mean
median

0.78
15.50
15.90

median
SD

106
6

Period 3
at 400 ng/mL

n
1
2
3
4
5
6

Cexp
10.700
9.820
10.900
11.200
10.700
11.700

Cnom
10.000
10.000
10.000
10.000
10.000
10.000

Accuracy (%)
107
98
109
112
107
117

var 3
mean
median

0.390467
10.84
10.80

median
SD

108
6

n
1
2
3
4
5
6

Cexp
15.000
15.600
16.100
15.200
17.000
14.800

Cnom
15.000
15.000
15.000
15.000
15.000
15.000

Accuracy (%)
100
104
107
101
113
99

var 3
mean
median

0.673667
15.62
15.40

median
SD

103
5

Repeatability data for the 10.0 g/L level

Median (all values)
Mean (all values)
SD of mean
Recovery (%)
SD of recovery
Within-day precision (g/kg)
Within-day precision (%)
2
SD (variance of the every-day median)
Between-day precision (g/kg)
Between-day precision (%)
Repeatability (g/kg) at the 95% confidence level
Repeatability (%) at the 95% confidence level

Period 1
at600 ng/mL

Accuracy (%) Period 2

106
at600 ng/mL
113
114
109
113
109
111
3

Period 3
at600 ng/mL

5.48
5.55
0.42
110
8
0.42
8
0.023
0.41
8
1.17

2.77*SD within-day

21

2.77*SD within-day

10.85
10.71
0.83
109
8
0.88
8
0.036
0.82
8
2.43
21

SD within-day

SD between-day

SD within-day

SD between-day
2.77*SD within-day
2.77*SD within-day

Repeatability data for the 15.0 g/L level

Median (all values)
Mean (all values)
SD of mean
Recovery (%)
SD of recovery
Within-day precision (g/kg)
Within-day precision (%)
SD2 (variance of the every-day median)
Between-day precision (g/kg)
Between-day precision (%)
Repeatability (g/kg) at the 95% confidence level
Repeatability (%) at the 95% confidence level

16.00
15.91
0.86
107
6
0.74
5
0.396
0.92
6
2.06
16

SD within-day

SD between-day
2.77*SD within-day
2.77*SD within-day

Intermediate reproducibility (iR) data (three analysts / three concentration levels / three different periods of analysis):
Cexp
Cnom
Cexp
Cnom
Gustavo
n
Accuracy (%)
Jose
n
Accuracy (%)
Jeferson
at 500 ng/mL

1
2
3
4
5
6
var 1

Gustavo
at 1000 ng/L

Gustavo

5.000
5.000
5.000
5.000
5.000
5.000

0.197937 median A

mean
median

5.378
5.285

SD

n
1
2
3
4
5
6

Cexp
11.300
10.800
8.910
10.900
9.230
11.400

Cnom
10.000
10.000
10.000
10.000
10.000
10.000

var 1

at 1500 ng/mL

4.880
5.040
5.820
5.480
5.090
5.960

1.161147 median A

98
101
116
110
102
119

at 0.48 g/kg

1
2
3
4
5
6

5.100
4.500
4.610
4.040
5.640
5.400

5.000
5.000
5.000
5.000
5.000
5.000

n
1
2
3
4
5
6

Cexp
4.830
5.100
4.920
4.590
5.160
4.950

Cnom
5.000
5.000
5.000
5.000
5.000
5.000

Accuracy (%)
97
102
98
92
103
99

97

var 1

0.04155

median A

99

Repeatability data for the 5.0 g/L level

Median
Mean
SD of mean
Recovery (%)
SD of recovery
Within-lab precision (g/kg)
Within-lab precision (%)
Intermediate reproducibility (g/kg) at the 95% confidence level

mean
median

4.925
4.935

SD

Intermediate reproducibility (%) at the 95% confidence level

n
1
2
3
4
5
6

Cexp
9.450
10.200
11.000
9.800
11.000
10.100

Cnom
10.000
10.000
10.000
10.000
10.000
10.000

Accuracy (%)
95
102
110
98
110
101

102
90
92
81
113
108

106

var 1

mean
median

4.882
4.855

SD

12

n
1
2
3
4
5
6

Cexp
11.000
9.680
10.900
11.000
10.500
10.300

Cnom
10.000
10.000
10.000
10.000
10.000
10.000

Accuracy (%)
110
97
109
110
105
103

Accuracy (%)
Jose
113
at 1000 ng/mL
108
89
109
92
114

0.363857 median A

at 0.48 g/kg

Jeferson
at 1000 ng/mL

109

var 1

107

var 1

11

mean
median

10.56
10.70

SD

mean
median

10.26
10.15

SD

n
1
2
3
4
5
6

Cexp
16.200
14.500
16.100
15.900
14.400
16.700

Cnom
15.000
15.000
15.000
15.000
15.000
15.000

Accuracy (%)
108
97
107
106
96
111

n
1
2
3
4
5
6

Cexp
14.900
15.000
15.400
16.200
16.000
15.500

Cnom
15.000
15.000
15.000
15.000
15.000
15.000

Accuracy (%)
99
100
103
108
107
103

107

var 1

0.272

median A

103

mean
median

15.50
15.45

SD

mean
median

10.42
10.85

SD

n
1
2
3
4
5
6

Cexp
17.100
16.700
14.400
16.100
15.600
14.900

Cnom
15.000
15.000
15.000
15.000
15.000
15.000

var 1

1.08

median A

106

var 1

mean
median

15.80
15.85

SD

mean
median

Accuracy (%)
Jose
114
at 1500 ng/mL
111
96
107
104
99

0.269667 median A

0.910667 median A
15.63
16.00

SD

Jeferson
at 1500 g/L

0.398417 median A

102

Repeatability data for the 10.0 g/L level

median
mean
SD of mean
Recovery (%)
SD of recovery
Within-lab precision (g/kg)
Within-lab precision (%)
Intermediate reproducibility (g/kg) at the 95% confidence level
Intermediate reproducibility (%) at the 95% confidence level

Repeatability data for the 15.0 g/L level

median
mean
SD of mean
Recovery (%)
SD of recovery
Within-lab precision (g/kg)
Within-lab precision (%)
Intermediate reproducibility (g/kg) at the 95% confidence level
Intermediate reproducibility (%) at the 95% confidence level

5.07
5.06
0.48
101
10
0.45
9
1.24

2.77*SD within-lab

25

2.77*SD within-lab

10.65
10.42
0.74
107
7
0.78
7
2.16

2.77*SD within-lab

20

2.77*SD within-lab

15.75
15.64
0.83
105
6
0.87
6
2.41

2.77*SD within-lab

15

2.77*SD within-lab

SD within-lab

SD within-lab

SD within-lab

Validation data for Enrofloxacin in milk

Repeatability (r) data (one analyst / three concentration levels / three different periods of analysis):
Cexp
Cnom
Cexp
Cnom
Period 1
n
Accuracy (%) Period 2
n
Accuracy (%)
at 200ng/mL

1
2
3
4
5
6

4.810
5.090
4.970
5.090
5.340
4.940

5.000
5.000
5.000
5.000
5.000
5.000

96
102
99
102
107
99

var 1
mean
median

0.03256
5.040
5.030

median
SD

101
4

at 200ng/mL

1
2
3
4
5
6

5.110
5.150
5.320
5.470
5.330
5.110

5.000
5.000
5.000
5.000
5.000
5.000

102
103
106
109
107
102

var 2
mean
median

0.021777
5.25
5.24

median
SD

105
3

Period 3
at 200ng/mL

n
1
2
3
4
5
6

Cexp
4.890
5.360
4.890
5.390
5.210
4.610

Cnom
5.000
5.000
5.000
5.000
5.000
5.000

Accuracy (%)
98
107
98
108
104
92

var 3
mean
median

0.096337
5.06
5.05

median
SD

101
6

Repeatability data for the 5.0 g/L level

Median (all values)
Mean (all values)
SD of mean
Recovery (%)
SD of recovery
Within-day precision (g/kg)
Within-day precision (%)
2
SD (variance of the every-day median)
Between-day precision (g/kg)
Between-day precision (%)
Repeatability (g/kg) at the 95% confidence level
Repeatability (%) at the 95% confidence level

Period 1
at 400 ng/mL

n
1
2
3
4
5
6

Cexp
9.500
10.500
10.700
10.400
10.200
10.100

Cnom
10.000
10.000
10.000
10.000
10.000
10.000

var 1
mean
median

0.174667
10.23
10.30

median
SD

n
1
2
3
4
5
6

Cexp
15.200
15.000
15.000
15.300
15.100
14.600

Cnom
15.000
15.000
15.000
15.000
15.000
15.000

var 1
mean
median

0.058667
15.03
15.05

median
SD

Accuracy (%) Period 2

95
at 400 ng/mL
105
107
104
102
101
103
4

n
1
2
3
4
5
6

Cexp
10.300
10.200
10.200
10.200
9.660
9.400

Cnom
10.000
10.000
10.000
10.000
10.000
10.000

Accuracy (%)
103
102
102
102
97
94

var 2
mean
median

0.137067
9.99
10.20

median
SD

102
4

n
1
2
3
4
5
6

Cexp
14.300
14.700
14.400
14.600
14.600
15.200

Cnom
15.000
15.000
15.000
15.000
15.000
15.000

Accuracy (%)
95
98
96
97
97
101

var 2
mean
median

0.098667
14.63
14.60

median
SD

97
2

Period 3
at 400 ng/mL

n
1
2
3
4
5
6

Cexp
10.500
9.820
9.940
10.300
10.100
10.100

Cnom
10.000
10.000
10.000
10.000
10.000
10.000

Accuracy (%)
105
98
99
103
101
101

var 3
mean
median

0.059947
10.13
10.10

median
SD

101
2

n
1
2
3
4
5
6

Cexp
14.500
14.500
14.600
14.900
15.100
14.700

Cnom
15.000
15.000
15.000
15.000
15.000
15.000

Accuracy (%)
97
97
97
99
101
98

var 3
mean
median

0.057667
14.72
14.65

median
SD

98
2

Repeatability data for the 10.0 g/L level

Median (all values)
Mean (all values)
SD of mean
Recovery (%)
SD of recovery
Within-day precision (g/kg)
Within-day precision (%)
2
SD (variance of the every-day median)
Between-day precision (g/kg)
Between-day precision (%)
Repeatability (g/kg) at the 95% confidence level
Repeatability (%) at the 95% confidence level

Period 1
at600 ng/mL

Accuracy (%) Period 2

101
at600 ng/mL
100
100
102
101
97
100
2

Period 3
at600 ng/mL

5.11
5.12
0.23
102
5
0.22
4
0.013
0.23
5
0.62

2.77*SD within-day

13

2.77*SD within-day

10.20
10.12
0.35
102
3
0.35
3
0.010
0.34
3
0.97
9

SD within-day

SD between-day

SD within-day

SD between-day
2.77*SD within-day
2.77*SD within-day

Repeatability data for the 15.0 g/L level

Median (all values)
Mean (all values)
SD of mean
Recovery (%)
SD of recovery
Within-day precision (g/kg)
Within-day precision (%)
SD2 (variance of the every-day median)
Between-day precision (g/kg)
Between-day precision (%)
Repeatability (g/kg) at the 95% confidence level
Repeatability (%) at the 95% confidence level

14.70
14.79
0.31
98
2
0.27
2
0.061
0.35
2
0.74
7

SD within-day

SD between-day
2.77*SD within-day
2.77*SD within-day

Intermediate reproducibility (iR) data (three analysts / three concentration levels / three different periods of analysis):
Cexp
Cnom
Cexp
Cnom
Gustavo
n
Accuracy (%)
Jose
n
Accuracy (%)
Jeferson
at 200ng/mL

1
2
3
4
5
6
var 1

Gustavo
at 400 ng/mL

Gustavo

5.000
5.000
5.000
5.000
5.000
5.000

0.017667 median A

mean
median

5.287
5.270

SD

n
1
2
3
4
5
6

Cexp
11.100
10.800
10.300
10.800
10.700
10.600

Cnom
10.000
10.000
10.000
10.000
10.000
10.000

var 1

at600 ng/mL

5.350
5.160
5.240
5.510
5.160
5.300

0.069667 median A

mean
median

10.72
10.75

SD

n
1
2
3
4
5
6

Cexp
16.500
15.400
14.200
16.200
15.700
15.300

Cnom
15.000
15.000
15.000
15.000
15.000
15.000

var 1

0.651

median A

mean
median

15.55
15.55

SD

107
103
105
110
103
106

at 200ng/mL

1
2
3
4
5
6

5.050
4.980
5.120
4.860
4.670
4.640

105

var 1

mean
median

4.887
4.920

n
1
2
3
4
5
6

Cexp
10.500
10.200
10.500
9.680
10.100
9.930

Accuracy (%)
Jose
111
at 400 ng/mL
108
103
108
107
106

5.000
5.000
5.000
5.000
5.000
5.000

101
100
102
97
93
93

at 200ng/mL

n
1
2
3
4
5
6

Cexp
4.990
4.640
4.950
4.930
4.940
4.690

98

var 1

SD

mean
median

4.857
4.935

Cnom
10.000
10.000
10.000
10.000
10.000
10.000

Accuracy (%)
105
102
105
97
101
99

n
1
2
3
4
5
6

Cexp
9.280
9.890
10.400
9.640
10.300
10.200

0.039667 median A

Jeferson
at 400 ng/mL

Cnom
5.000
5.000
5.000
5.000
5.000
5.000

99

Repeatability data for the 5.0 g/L level

Median
Mean
SD of mean
Recovery (%)
SD of recovery
Within-lab precision (g/kg)
Within-lab precision (%)
Intermediate reproducibility (g/kg) at the 95% confidence level

SD

Intermediate reproducibility (%) at the 95% confidence level

Cnom
10.000
10.000
10.000
10.000
10.000
10.000

Accuracy (%)
93
99
104
96
103
102

0.022707 median A

Accuracy (%)
100
93
99
99
99
94

108

var 1

102

var 1

mean
median

10.15
10.15

SD

mean
median

9.95
10.05

SD

n
1
2
3
4
5
6

Cexp
14.900
14.400
15.600
15.300
14.400
15.400

Cnom
15.000
15.000
15.000
15.000
15.000
15.000

Accuracy (%)
99
96
104
102
96
103

n
1
2
3
4
5
6

Cexp
14.800
15.000
15.100
15.000
15.000
14.800

Cnom
15.000
15.000
15.000
15.000
15.000
15.000

Accuracy (%)
99
100
101
100
100
99

104

var 1

0.268

median A

101

var 1

0.015

median A

100

mean
median

15.00
15.10

SD

mean
median

14.95
15.00

SD

Accuracy (%)
Jose
110
at600 ng/mL
103
95
108
105
102

0.103857 median A

Jeferson
at600 ng/mL

0.187217 median A

100

Repeatability data for the 10.0 g/L level

median
mean
SD of mean
Recovery (%)
SD of recovery
Within-lab precision (g/kg)
Within-lab precision (%)
Intermediate reproducibility (g/kg) at the 95% confidence level
Intermediate reproducibility (%) at the 95% confidence level

Repeatability data for the 15.0 g/L level

median
mean
SD of mean
Recovery (%)
SD of recovery
Within-lab precision (g/kg)
Within-lab precision (%)
Intermediate reproducibility (g/kg) at the 95% confidence level
Intermediate reproducibility (%) at the 95% confidence level

4.99
5.01
0.25
100
5
0.16
3
0.45

2.77*SD within-lab

2.77*SD within-lab

10.30
10.27
0.47
103
5
0.35
3
0.96

2.77*SD within-lab

2.77*SD within-lab

15.05
15.17
0.59
100
4
0.56
4
1.55

2.77*SD within-lab

10

2.77*SD within-lab

SD within-lab

SD within-lab

SD within-lab

Danofloxacin: Calculation of CCa and CCb through the calibration curve procedure (use of intermediate reproducibility data)
C experimental
4.88
5.04
5.82
5.48
5.09
5.96
5.10
4.50
4.61
4.04
5.64
5.40
4.83
5.10
4.92
4.59
5.16
4.95
11.30
10.80
8.91
10.90
9.23
11.40
11.00
9.68
10.90
11.00
10.50
10.30
9.45
10.20
11.00
9.80
11.00
10.10
17.10
16.70
14.40
16.10
15.60
14.90
16.20
14.50
16.10
15.90
14.40
16.70
14.90
15.00
15.40
16.20
16.00
15.50

RESUMO DOS RESULTADOS

Estatstica de regresso
R mltiplo
0.98783369
R-Quadrado
0.975815399
R-quadrado ajustado 0.975350311
Erro padro
0.693114346
Observaes
54
ANOVA
gl
1
52
53

SQ
MQ
1007.956669 1007.9567
24.98118981 0.4804075
1032.937859

Coeficientes
-0.209074074
1.058277778

Erro padro
Stat t
0.249549686 -0.837805
0.023103812 45.805333

Regresso
Resduo
Total

Interseo
Varivel X 1

F
F de significao
2098.12852
1.04467E-43

valor-P
0.405974425
1.04467E-43

95% inferiores95% superiores

Inferior 95.0%
Superior 95.0%
-0.709832143 0.291684 -0.709832 0.291684
1.011916589 1.104639 1.011917 1.104639

y = 1.0583x - 0.2091
R = 0.9758

18.00
16.00

Experimental values (g/L)

C nominal
5.00
5.00
5.00
5.00
5.00
5.00
5.00
5.00
5.00
5.00
5.00
5.00
5.00
5.00
5.00
5.00
5.00
5.00
10.00
10.00
10.00
10.00
10.00
10.00
10.00
10.00
10.00
10.00
10.00
10.00
10.00
10.00
10.00
10.00
10.00
10.00
15.00
15.00
15.00
15.00
15.00
15.00
15.00
15.00
15.00
15.00
15.00
15.00
15.00
15.00
15.00
15.00
15.00
15.00

14.00
12.00
10.00
8.00

6.00
4.00
2.00
0.00
0.00

2.00

4.00

6.00

8.00

10.00

12.00

Nominal values (g/kg)

A) Calculation of limits based on 2002/657/EC:

Ccalpha =
x-concentration corresponding to the intercept + 2.33 * std error of intercept
slope
1.058277778
Intercept
-0.209074074
Intercept to consider -0.209074074 *
Std error of intercept 0.249549686
Intercept + 2.33 SE
0.372376695
CCalpha
0.549
Intercept + 3.97 SE
0.78163818
CCbeta
0.936
*Note: when the intercept is < 0, the value 0 should be considered as the real intercept
B) Calculation of limits based on the SD of the lowest fortification level values:
SD of values at the lowest fortification level (= Std error intercept)
Intercept + 2.33*SD ordinate at CCalpha
Intercept + 3.97*SD ordinate at CCbeta
CCalpha
CCbeta

0.480493007
0.910
1.698
1.058
1.803

14.00

16.00

Enrofloxacin: Calculation of CCa and CCb through the calibration curve procedure (use of intermediate reproducibility data)
C experimental
5.350
5.160
5.240
5.510
5.160
5.300
5.050
4.980
5.120
4.860
4.670
4.640
4.990
4.640
4.950
4.930
4.940
4.690
11.100
10.800
10.300
10.800
10.700
10.600
10.500
10.200
10.500
9.680
10.100
9.930
9.280
9.890
10.400
9.640
10.300
10.200
16.500
15.400
14.200
16.200
15.700
15.300
14.900
14.400
15.600
15.300
14.400
15.400
14.800
15.000
15.100
15.000
15.000
14.800

RESUMO DOS RESULTADOS

Estatstica de regresso
R mltiplo
0.994024875
R-Quadrado
0.988085452
R-quadrado ajustado 0.987856326
Erro padro
0.463993949
Observaes
54
ANOVA
gl
Regresso
Resduo
Total

Interseo
Varivel X 1

SQ
MQ
928.4209 928.4209
11.1951 0.2152904
939.616

1
52
53
Coeficientes
-0.006666667
1.015666667

Erro padro
0.167056915
0.015466465

Stat t
-0.039907
65.66896

F
F de significao
4312.412288
1.05287E-51

valor-P
0.968320447
1.05287E-51

95% inferiores 95% superiores

Inferior 95.0%
Superior 95.0%
-0.341890884 0.328558 -0.341891 0.328558
0.984630935 1.046702 0.984631 1.046702

y = 1.0157x - 0.0067
R = 0.9881

18.000
16.000

Experimental values (g/L)

C nominal
5.000
5.000
5.000
5.000
5.000
5.000
5.000
5.000
5.000
5.000
5.000
5.000
5.000
5.000
5.000
5.000
5.000
5.000
10.000
10.000
10.000
10.000
10.000
10.000
10.000
10.000
10.000
10.000
10.000
10.000
10.000
10.000
10.000
10.000
10.000
10.000
15.000
15.000
15.000
15.000
15.000
15.000
15.000
15.000
15.000
15.000
15.000
15.000
15.000
15.000
15.000
15.000
15.000
15.000

14.000
12.000
10.000
8.000

6.000
4.000
2.000
0.000
0.000

2.000

4.000

6.000

8.000

10.000

12.000

Nominal values (g/kg)

A) Calculation of limits based on 2002/657/EC:

Ccalpha =
x-concentration corresponding to the intercept + 2.33 * std error of intercept
slope
1.015666667
Intercept
-0.006666667
Intercept to consider -0.006666667 *
Std error of intercept 0.167056915
Intercept + 2.33 SE
0.382575945
CCalpha
0.383
Intercept + 3.97 SE
0.656549286
CCbeta
0.653
*Note: when the intercept is < 0, the value 0 should be considered as the real intercept
B) Calculation of limits based on the SD of the lowest fortification level values:
SD of values at the lowest fortification level (= Std error intercept)
Intercept + 2.33*SD ordinate at CCalpha
Intercept + 3.97*SD ordinate at CCbeta
CCalpha
CCbeta

0.253423617
0.584
0.999
0.581
0.991

14.000

16.000

Summary of validation data:

5
Obtained under repeatability conditions:
Recovery (%)
112
SD of recovery
10
Within-day precision (%)
9
Between-day precision (%)
8
Repeatability (%) at the 95% confidence
24
level

Norfloxacin
Fortification levels (g/L)
10

99
5
5
5
14

Obtained under intermediate reproducibility conditions:

Recovery (%)
100
103
SD of recovery
7
7
Within-lab precision (%)
7
4

Intermediate reproducibility (%) at 20

the 95% confidence
11
level
Limits calculated according to 2002/657/EC
CCa
CCb

0.53
0.90

Norfloxacin
ication levels (g/L)

Danofloxacin
Fortification levels (g/L)
15

94
8
9
8
23

110
8
8
8
21

108
6
5

101
10
9

13

25

Danofloxacin
Fortification levels (g/L)
10

F
15

109
8
8
8
21

107
6
5
6
16

102
5
4
5
13

107
7
7

105
6
6

100
5
3

20

0.55
0.94

15

Enrofloxacin
Fortification levels (g/L)
10

15

102
3
3
3
9

98
2
2
2
7

103
5
3

100
4
4

0.38
0.65

10