Dietary Fibre and Inulin in cereal food

Transcrição

May 2016
DLA 26/2015 - Dietary Fibre and Inulin
DLA
Dienstleistung
Lebensmittel
Analytik GbR
Evaluation Report
proficiency test
DLA 26/2015
Dietary Fibre and Inulin in
cereal food
Dienstleistung Lebensmittel Analytik GbR
Waldemar-Bonsels-Weg 170
22926 Ahrensburg, Germany
[email protected]
www.dla-lvu.de
Coordinator of this PT:
Dr. Matthias Besler
Reprint, also in part, only with written permission from DLA-Ahrensburg
Page 1 of 31
May 2016
Inhalt / Content
1. Introduction.........................................................3
2. Realisation..........................................................3
2.1 Test material...................................................3
2.1.1 Homogeneity....................................................4
2.2 Test.............................................................4
2.3 Submission of results............................................4
3. Evaluation...........................................................5
3.1 Assigned value...................................................5
3.2 Standard deviation...............................................5
3.3 Outliers.........................................................5
3.4 Target standard deviation........................................5
3.4.1 General model (Horwitz)........................................6
3.4.2 Value by precision experiment..................................6
3.4.3 Value by perception............................................7
3.5 z-Score..........................................................7
3.6 z'-Score.........................................................7
3.7 Quotient ........................................................8
3.8 Standard uncertainty.............................................8
4. Results..............................................................9
4.1 Total Dietary Fibre in g/100g...................................10
4.2 Soluble Fibre in g/100g.........................................12
4.3 Unsoluble Fibre in g/100g.......................................14
4.4 Total Dietary Fibre after Inulinase-Reaction....................16
4.5 Soluble Total Dietary Fibre after Inulinase-Reaction ...........18
4.6 Unsoluble Total Dietary Fibre after Inulinase-Reaction..........18
4.7 Inulin in g/100g................................................19
5. Documentation.......................................................21
5.1 Primary data....................................................21
5.2 Homogeneity.....................................................25
5.3 Analytical Methods..............................................27
6. Index of participant laboratories...................................30
7. Index of references.................................................31
Page 2 of 31
May 2016
1. Introduction
The participation in proficiency testing schemes is an essential element
of the quality-management-system of every laboratory testing food and
feed, cosmetics and food contact materials. The implementation of
proficiency tests enables the participating laboratories to prove their
own analytical competence under realistic conditions. At the same time
they receive valuable data regarding the validity of the particular
testing method.
The purpose of DLA is to offer proficiency tests for selected parameters
in concentrations with practical relevance.
Realisation and evaluation of the present proficiency test follows the
technical requirements of DIN EN ISO/IEC 17043 (2010) and DIN ISO
13528:2009 (6).
2. Realisation
2.1
Test material
The test material is a common in commerce breakfast cereal product with
addition of a customized semi-finished product rich in inulin from
European suppliers. The materials were crushed, mixed and homogenized.
Afterwards the samples were packaged lightproof in portions to
approximately 20 g. The portions were numbered chronologically.
The composition of the samples is given in table 1. The fat content of
the samples is < 10%.
Table 1: Composition of DLA samples
Ingredients
Amount
Breakfast Cereals
Ingredients: Cereal whole meals (oat, wheat, barley,
rye), sugar, honey, glucose syrup, salt, calcium carbonate, calcium phosphate, colourant: carotenes, flavour, antioxidants: ascorbyl palmitate, alpha-tocopherol, niacin, vitamin B6, vitamin B2, vitamin B1,
folic acid, vitamin D, vitamin B12, iron.
80
g/100g
20
g/100g
Nutrients per 100 g: fat 3,5 g, carbohydrates 74 g
thereof sugar 29 g, fibre 7 g, protein 9 g
Cereal semi-finished product with 25% inulin
Page 3 of 31
May 2016
2.1.1 Homogeneity
Homogeneity of the test material was checked by 5fold determination of
fructose by HPLC-RI. With a repeatability standard deviation of 7,8 % the
homogeneity of the test material was considered acceptable. The precision
data of similar methods for determination of mono- and disaccharides were
for the relative repeatability standard deviation 0,46 – 2,9 % and for
the relative reproducibility standard deviation 2,5 – 7,0 % for milk product containing foods (18). The results are given in the documentation.
The calculation of the repeatability standard deviation of the participants was also used as an indicator of homogeneity. For total dietary fibre and inulin it was 9,2% and 6,7% respectively. The relative repeatability standard deviations of the official German ASU §64 methods for bread
were 2,49 % (total dietary fibre), 5,14 % (unsoluble fibre) and 14,6 %
(soluble fibre) (15). The relative repeatability standard deviations of
the official German ASU §64 methods for inulin were 1,86 % (instant
meal), 4,92 % (infant food) and 2,35 % (chocolate) (17).
The repeatability standard deviations of the participants' results for
total dietary fibre and inulin are given in the documentation.
Additionally in the documentation the portion numbers are graphically assigned to the results of total dietary fibre and inulin. There is no
trend recognizable in the results which could suggest inhomogeneity.
2.2 Test
Two portions of test material were sent to every participating laboratory
in the 16th week of 2015. The testing method was optional. The tests
should be finished at 29th may 2015.
2.3 Submission of results
The participants submitted their results in provided standard forms by
email.
The final concentration of each parameter of the numbered samples was
used for each statistical evaluation.
Queried and documented were single results, recovery and the testing
methods used.
All participants submitted their results in time.
Page 4 of 31
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3. Evaluation
3.1 Assigned value
Because the analysed material was no certified reference material the
robust mean of the submitted results was used as assigned value X (6).
The distribution of submitted results showed no hint for bimodal
distribution or other reasons for a higher variability.
The statistical evaluation is performed when there are at least 7 results
for a parameter.
Single results giving values outside the measuring range of the
participating laboratory were considered for statistical evaluation (e.g.
results given as > 25 mg/kg and < 2,5 mg/kg, respectively) when a result
indicating „>“ is above and a result indicating „<“ is below the target
range.
3.2 Standard deviation
For comparison to the target standard deviation a robust standard deviation (Sx) was calculated (6).
3.3 Outliers
Statistical outliers were determined by Mandel´s-H-Statistic for 95%
significance niveau (5). Detected outliers were stated for information
only, when z-score was < -2 or > 2.
3.4 Target standard deviation
The target standard deviation of
according to the following methods.
the
assigned
value
is
determined
In general the Horwitz target standard deviation is suitable for the
statistical
evaluation
of
interlaboratory
tests
where
different
analytical methods are applied. The standard deviation from precision
experiments are derived from proficiency tests where a specific
analytical method is mandatory. For information the z-scores from both
models were given in the result tables, if available.
For the valuation of total dietary fibre and inulin the target standard
deviation according to a precision experiment was applied (3.4.2, offical German ASU §64 methods: 15, 17). Additionally the standard uncertainty was considered by valuating with z'-score (see 3.6).
For all other parameters there were less than 7 quantitative results,
thus no statistical valuation was done.
Page 5 of 31
May 2016
3.4.1 General model (Horwitz)
The relative target standard deviation in % of the assigned value is
derived from following equation (Horwitz)
σ
(%)
= 2(1-0,5logX)
From the result the target standard deviation is calculated
σ
= X *
σ
(%)
/ 100.
3.4.2 Value by precision experiment
Using the reproducibility standard deviation σR and the repeatability
standard deviation σr of a precision experiment the between-laboratories
standard deviation can be calculated σL :
 L = 2R− 2r  .
And then, using the number of replicate measurements n, each participant
is to perform, the target standard deviation for proficiency assessment
is calculated :
=
  2L  2r /n .
The target standard deviations given in table 2 were calculated from the
precision data of the respective methods.
Tabelle 2: Relative target standard deviations (RSD) from precision
experiments (15, 17)
RSD σ
Parameter
Matrix
Total dietary fibre
Rye-wheat bread
4,6 %
Unsoluble fibre
Rye-wheat bread
7,2 %
ASU §64 L 17.03-1 (15)
Soluble fibre
Rye-wheat bread
16,6 %
ASU §64 L 17.03-1 (15)
Inulin
Instant meal
Infant food
Chocolate
1
3,2 %
7,0 %
3,5 %
Method / Literature
1
1
ASU §64 L 17.03-1 (15)
ASU §64 L 00.00-94
(17)
used in evaluation (s. chapter 4)
Page 6 of 31
May 2016
3.4.3 Value by perception
The target standard deviation for proficiency assessment can be set at a
value that corresponds to the level of performance that the coordinator
would wish laboratories to be able to achieve (6).
For the present evaluation of results the target standard deviation according to the related ASU §64 methods was applied for total dietary fibre and inulin (3.4.2).
Additionally the standard uncertainty was considered for fructose and
lactose by valuating with z'-score (see 3.6).
3.5 z-Score
To assess the results of the participants the z-score is used. It
indicates about which multiple of the target standard deviation ( σ )
the result (x) of the participant is deviating from the assigned value
(X) (6).
Participants’ z-scores were derived as:
z = (x – X) /
σ
;
the requirements for the analytical performance are generally considered
as fulfilled if
-2 ≤ z ≤ 2 .
3.6 z'-Score
The z'-score can be used for the valuation of the results of the
participants, in cases the standard uncertainty has to be considered (s.
3.8). The z'-score represents the relation of the deviation of the result
(x) of the participant from the respective assigned value (X) to the
square root of quadrat sum of the target standard deviation ( σ̂ ) and
the standard uncertainty (Ux) (6).
Participants’ z'-scores are derived as:
In the following we define the denominator
deviation σ '.
as the target standard
The requirements for the analytical performance are generally considered
as fulfilled if
-2 ≤ z' ≤ 2 .
The z'-Score was used for the analytes total dietary fibre and inulin
(see also 3.7 and 3.8).
Page 7 of 31
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3.7 Quotient
x
S / 
Following the Horrat-value the results of a proficiency-test (PT) can be
considered convincing, if the quotient of robust standard deviation and
target standard deviation does not exceed the value of 2.
A value > 2 means an insufficient precision, i.e. the analytical method
is too variable, or the variation between the test participants is higher
than estimated. Thus the comparability of the results is not given (11).
In the present proficiency tests the quotients Sx/ σ̂ were
In the present proficiency test the quotient Sx/ σ̂ for total dietary
fibre (3,0) and inulin (2,7) was clearly above 2,0. Therefore evaluation
was done according to 3.6 by z'-Scores. The resulting quotients S x/ σ̂ '
were 2,0 and 1,9 then.
3.8 Standard uncertainty
u X that depends on the
The assigned value X has a standard uncertainty
analytical method, differences between the analytical methods used, the
test material, the number of participant laboratories and perhaps on
u X for this PT is calculated
other factors. The standard uncertainty
as follows (6).
x
u X =1,25∗S /  p
u X ≤ 0,3∗
If
 the standard uncertainty of the assigned value needs
not to be included in the interpretation of the results of the PT (6).
Values exceeding 0,3 imply, that the target standard deviation could be
too low with respect to the standard uncertainty of the assigned value.
In the present proficiency tests the quotients Ux/ σ̂ were 1,1 and 1,0 for
total dietary fibre and inulin respectively. At the same time the
quotients Sx/ σ̂ were > 2,0. Therefore the target range was extended
according 3.6 z'-score considering the standard uncertainty.
Page 8 of 31
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4. Results
All following tables are anonymized. With the delivering of the
evaluation-report the participants are informed about their individual
evaluation-number.
In the first table the characteristics are listed:
Statistic Data
Number of results
Number of outliers
Mean
Median
Robust mean (X)
Robust standard deviation (Sx)
Target range:
Target standard deviation σ̂ or σ̂ '
Target standard deviation for information
lower limit of target range (X - 2 σ̂ ) or (X - 2 σ ') *
upper limit of target range (X + 2 σ ) or (X + 2 σ ') *
Quotient Sx/ σ '
Standard uncertainty uX
 '
Quotient u X / 
Number of results in the target range
* Target range is calculated with z-score or z'-score
In the second table the
laboratories are listed:
Auswertenummer
Evaluation
number
Parame te r
[Einheit / Unit]
individual
results
Abweichung
z-Score
[Einheit / Unit]
σ̂
of
the
participating
z-Score
(Info)
Deviation
[Einheit / Unit]
Page 9 of 31
Hinweis
Remark
May 2016
4.1 Total Dietary Fibre in g/100g
Vergleichsuntersuchung
/
Proficiency Test
Statistic Data
Number of results
Number of outliers
Mean
Median
Robust Mean (X)
Robust standard deviation (S x)
Target range:
Target standard deviation σ̂ '
Target standard deviation ASU
(for Information)
lower limit of target range
upper limit of target range
Quotient Sx/ σ̂ '
Standard uncertainty ux
11
1
6,23
6,00
6,06
0,840
0,423
0,280
5,22
6,91
2,0
0,32
Quotient ux / σ̂ '
Results in the target range
Percent in the target range
0,75
8
73
Ergebnisse / Results
12
Gesamtballaststoffe /
Total dietary
fibre [g/100g]
10
8
obere Grenze
upper limit
6
4
rob. Mittelwert
robust mean
2
untere Grenze
lower limit
0
1
2
3
4
5
6
7
8
9
10
11
12
13
Auswertenummer / evaluation number
Abb. 1: Ergebnisse Gesamtballaststoffe
Fig. 1: Results total dietary fibre
Page 10 of 31
May 2016
Ergebnisse der teilnehmenden Institute:
Results of Participants:
Auswerte- Gesamtballaststoffe / Abweichung
[mg/kg]
nummer
Total dietary fibre
[g/100g]
Deviation
Evaluation
[mg/kg]
number
1
6,3
0,24
2
5,53
-0,53
3
6,51
0,45
z'-Score
σ̂
z-Score
(Info)
0,6
-1,3
1,1
0,8
-1,9
1,6
Remark
4
9,49
3,43
8,1
12,2
5
6
7
8
9
10
4,47
6,0
6,3
7,05
5,48
-1,59
-0,11
0,24
0,99
-0,58
-3,8
-0,3
0,6
2,3
-1,4
-5,7
-0,4
0,8
3,5
-2,1
5,44
6
-0,62
-0,06
-1,5
-0,1
-2,2
-0,2
11
12
13
Hinweis
Ausreisser /
Outlier
* Mean calculated by DLA.
z'-Score
>
4
3
2
1
0
-1
-2
-3
-4
6
11
10
2
7
12
1
8
3
9
4
Abb. 2:
Fig. 2:
Z'-Scores Gesamtballaststoffe
Z'-Scores total dietary fibre
Page 11 of 31
*
May 2016
4.2 Soluble Fibre in g/100g
/
Proficiency Test
Statistic Data
Number of results
Number of outliers
Mean
Median
Robust Mean (X)
Target range:
Target standard deviation σ̂
(for Information)
Quotient Sx/ σ̂
Standard uncertainty u x
3
0
3,35
2,24
2,57
0,694
*
Quotient ux / σ̂
* Due to the low number of results (<7) no statistical evaluation was done.
6
5
Lösliche
Ballaststoffe
/ Soluble
dietary fibre
[g/100g]
4
3
2
rob.
Mittelwert
robust mean
1
0
1
2
3
4
5
6
7
8
9
10
11
12
13
Abb. 3: Ergebnisse Lösliche Ballaststoffe
Fig. 3: Results soluble dietary fibre
Page 12 of 31
May 2016
Auswertenummer
Evaluation
number
1
2
3
4
5
6
7
8
9
10
11
12
13
Lösliche
Ballaststoffe /
Soluble dietary fiber
[g/100g]
Abweichung
5,6
3,03
2,24
-0,33
2,2
-0,37
Hinweis
[mg/kg]
Deviation
Remark
[mg/kg]
Page 13 of 31
May 2016
4.3 Unsoluble Fibre in g/100g
/
Proficiency Test
Statistic Data
Number of results
Number of outliers
Mean
Median
Robust Mean (X)
Target range:
(for Information)
Quotient Sx/ σ̂
3
0
3,31
3,80
3,31
1,06
*
Quotient ux / σ̂
6
5
Unlösliche
Ballaststoffe
/ Unsoluble
dietary fibre
[g/100g]
4
3
2
rob.
Mittelwert
robust mean
1
0
1
2
3
4
5
6
7
8
9
10
11
12
13
Abb. 4: Ergebnisse unlösliche Ballaststoffe
Fig. 4: Results unsoluble dietary fibre
Page 14 of 31
May 2016
Auswertenummer
Evaluation
number
1
2
3
4
5
6
7
8
9
10
11
12
13
Unlösliche
Ballaststoffe /
Unsoluble dietary
fiber [g/100g]
Abweichung
3,89
0,58
2,23
-1,08
3,8
0,49
Hinweis
[mg/kg]
Deviation
Remark
[mg/kg]
Page 15 of 31
May 2016
4.4 Total Dietary Fibre after Inulinase-Reaction
in g/100g
/
Proficiency Test
Statistic Data
Number of results
Number of outliers
Mean
Median
Robust Mean (X)
Target range:
(for Information)
Quotient Sx/ σ̂
3
0
5,11
5,25
5,11
1,65
*
Quotient ux / σ̂
10
9
8
7
6
5
4
3
2
1
0
Gesamtballaststoffe
nach Inulinase-Reaktion / Total
dietary fiber
with inulinase reaction
[g/100g]
1
2
3
4
5
6
7
8
9
10
11
12
13
Abb. 5: Ergebnisse Gesamtballaststoffe nach Inulinase-Reaktion
Fig. 5: Results total dietary fibre with inulinase reaction
Page 16 of 31
May 2016
Auswertenummer
Evaluation
number
1
2
3
4
5
6
7
8
9
10
Gesamtballaststoffe nach
Inulinase-Reaktion / Total
dietary fiber with inulinase
reaction [g/100g]
Abweichung
3,59
-1,52
6,49
1,38
11
12
13
5,25
0,14
Hinweis
[mg/kg]
Deviation
Remark
[mg/kg]
Page 17 of 31
May 2016
4.5 Soluble Total Dietary Fibre after Inulinase-Reaction
in g/100g
/
Proficiency Test
The was only one result submitted (participant 6: 1,56 g/100g).
Further details are given in the documentation.
4.6 Unsoluble Total Dietary Fibre after InulinaseReaction in g/100g
/
Proficiency Test
The was only one result submitted (participant 6: 2,03 g/100g).
Further details are given in the documentation.
Page 18 of 31
May 2016
4.7 Inulin in g/100g
/
Proficiency Test
Statistic Data
Number of results
Number of outliers
Mean
Median
Robust Mean (X)
Target range:
Target standard deviation σ̂ '
(for Information)
Quotient Sx/ σ̂ '
11
1
3,74
3,51
3,68
0,69
0,366
0,258
2,95
4,41
1,9
0,26
Quotient ux / σ̂ '
0,71
8
73
Results of participants 2 and 7 were not considered.
7
Inulin
[g/100g]
obere
Grenze
upper limit
rob. Mittelwert robust
mean
untere
Grenze
lower limit
6
5
4
3
2
1
0
1
2
3
4
5
6
7
8
9
10
11
12
13
Abb. 6: Ergebnisse Inulin
Fig. 6: Results Inulin
Page 19 of 31
May 2016
Auswertenummer
Evaluation
number
1
Inulin
[g/100g]
4,1
2
Abweichung
z'-Score
[mg/kg]
σ̂
z-Score
(Info)
0,42
1,1
1,6
< 0,1
-
-
-
3
4
5
6
3,5
5,35
4,62
2,78
-0,18
1,67
0,94
-0,9
-0,5
4,6
2,6
-2,5
-0,7
6,5
3,6
-3,5
7
-
-
-
-
8
9
10
11
12
13
14
15
3,73
3,47
3,80
2,98
3,3
3,51
0,05
-0,21
0,12
-0,7
-0,38
-0,17
0,1
-0,6
0,3
-1,9
-1,0
-0,5
0,2
-0,8
0,5
-2,7
-1,5
-0,7
Deviation
Hinweis
Remark
[mg/kg]
Ergebnis ausgeschlossen
/Result excluded
Ausreisser / Outlier
No mean calculated!
Sample 1: 4,4 g/100g
sample 2: 0,6 g/100g
z'-Score
5
4
3
2
1
0
-1
-2
-3
-4
-5
6
11
12
9
3
13
8
10
1
5
4
Abb. 7:
Fig. 7:
Z'-Scores Inulin
Z'-Scores Inulin
Page 20 of 31
May 2016
5. Documentation
5.1 Primary data
Parameter
Analyte
Teilnehmer
Participant
Einheit
Unit
Proben-Nr. A
Sample No. A
Proben-Nr. B
Sample No. B
Ergebnis (Mittel)
Result (Mean)
Ergebnis A
Result A
Ergebnis B
Result B
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
31
22
35
27
7 ; 39
43
17
51
49
2
5
15
54
62
87
76
56
7; 39
72
92
66
64
28
44
90
83
6,3
5,53
6,51
9,49
6,4
5,49
6,50
9,26
6,1
5,56
6,52
9,71
Gesamtballaststoffe /
total dietary
fibre
1
2
3
4
5
6
7
8
9
10
11
12
13
4,47
6,3
7,05
5,48
5,44
6
2,26
6,6
5,9
7,30
5,475
5,44
6
2,69
5,3
6,7
6,80
5,485
1
2
3
4
5
6
7
8
9
10
11
12
13
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
31
22
35
27
7 ; 39
43
17
51
49
2
5
15
54
62
87
76
56
7; 39
72
92
66
64
28
44
90
83
5,6
5,45
5,75
2,24
2,13
2,35
N/A
N/A
N/A
2,2
2,2
2,2
Lösliche
Ballaststoffe /
soluble dietary
fibre
5,9
Nachdruck, auch auszugsweise, nur mit schriftlicher Genehmigung von DLA-Ahrensburg
Seite 21 von 31
May 2016
Parameter
Analyte
Teilnehmer
Participant
Einheit
Unit
Proben-Nr. A
Sample No. A
Proben-Nr. B
Sample No. B
Unlösliche
Ballaststoffe /
unsoluble
dietary fibre
1
2
3
4
5
6
7
8
9
10
11
12
13
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
31
22
35
27
7 ; 39
43
17
51
49
2
5
15
54
62
87
76
56
7; 39
72
92
66
64
28
44
90
83
1
2
3
4
5
6
7
8
9
10
11
12
13
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
31
22
35
27
7 ; 39
43
17
51
49
2
5
15
54
62
87
76
56
7; 39
72
92
66
64
28
44
90
83
Gesamtballaststoffe nach
InulinaseReaktion / total
dietary fibre
with Inulinase
reaction
Ergebnis (Mittel)
Result (Mean)
Ergebnis A
Result A
Ergebnis B
Result B
3,89
3,81
3,96
2,23
2,13
2,34
N/A
N/A
N/A
3,8
3,8
3,7
N/A
6,49
N/A
6,48
N/A
6,50
5,25
5,25
3,59
Seite 22 von 31
May 2016
Parameter
Analyte
Teilnehmer
Participant
Einheit
Unit
Proben-Nr. A
Sample No. A
Proben-Nr. B
Sample No. B
Lösliche
Ballaststoffe
nach InulinaseReaktion /
soluble dietary
fibre with
Inulinase
reaction
1
2
3
4
5
6
7
8
9
10
11
12
13
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
31
22
35
27
7 ; 39
43
17
51
49
2
5
15
54
62
87
76
56
7; 39
72
92
66
64
28
44
90
83
Unlösliche
Ballaststoffe
nach InulinaseReaktion /
unsoluble
dietary fibre
with Inulinase
reaction
1
2
3
4
5
6
7
8
9
10
11
12
13
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
31
22
35
27
7 ; 39
43
17
51
49
2
5
15
54
62
87
76
56
7; 39
72
92
66
64
28
44
90
83
Ergebnis (Mittel)
Result (Mean)
Ergebnis A
Result A
Ergebnis B
Result B
1,56
1,84
1,27
N/A
N/A
N/A
2,03
2,04
2,03
N/A
N/A
N/A
Seite 23 von 31
May 2016
Parameter
Analyte
Teilnehmer
Participant
Einheit
Unit
Proben-Nr. A
Sample No. A
Proben-Nr. B
Sample No. B
Ergebnis (Mittel)
Result (Mean)
Ergebnis A
Result A
Ergebnis B
Result B
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
g/100g
31
22
35
27
7 ; 39
43
17
51
49
2
5
15
54
62
87
76
56
7; 39
72
92
66
64
28
44
90
83
4,1
< 0,1
3,5
5,35
4,62
2,78
Inulin
1
2
3
4
5
6
7
8
9
10
11
12
13
4,1
< 0,1
3,5
5,4
4,62
3,14
4,4
3,74
3,57
3,82
3,04
3,3
3,38
4,0
< 0,1
3,5
5,3
4,62
2,41
0,6
3,72
3,37
3,79
2,91
3,3
3,64
3,73
3,47
3,80
2,98
3,3
3,51
Seite 24 von 31
May 2016
5.2 Homogeneity
5.2.1 Homogeneity test before the PT
Homogeneity test for fructose by HPLC-RI:
Independant samples
1
2
3
4
5
g/100g
Mean
3,08
0,239
Repeatability Standard Deviation
3,2
3,2
2,7
3,3
3,0
7,8%
5.2.2 Comparison of sample number / test results
Homgenität / homogeneity
Gesamtballaststoffe / Total dietary fibre
100
90
80
70
60
50
40
30
20
10
0
DLA-Nr. / No.
Ergebnis *10
Page 25 of 31
May 2016
Homgenität / homogeneity
Inulin
100
90
80
70
60
50
40
30
20
10
0
DLA-Nr. / No.
Ergebnis *10
Page 26 of 31
May 2016
5.3 Analytical Methods
Details by the participants
Parameter
Analyte
Teilnehmer Methodenbeschreibung Frittendurchmesser
Participant
Method description
1
AOAC 991.43
2
3
4
5
ASU L 00.00-18
internal method
AOAC 2009.01
6
ASU § 64 LFGB L 00.0018
7
Ballaststoffe /
dietary fibre
8
AOAC 985.29
9
§64 LFGB L.00.00-18
11
ASU § 64 LFGB, L 00.0018, 1997-01, correction
2002-12
§64 LFGB L 00.00-18
12
AOAC 991.43
10
Frit diameter
Porendurchmesser
Angaben zu Amylase
Angaben zu Protease
Pore diameter
Notes to Amylase
Notes to Protease
2
Megazyme Kit AOAC
991.43
Megazyme Kit AOAC
991.43
Angaben zu
Amyloglucosidase
Notes to
Amyloglucosidase
Megazyme Kit AOAC
991.43
sigma tdf kit
TDF-100A kit sigma
sigma tdf kit
TDF-100A kit sigma
sigma tdf kit
TDF-100A kit sigma
from Testkit Merck
1.12979.0001
Dietary fibre kit
Megazyme
Megazyme
Sigma A 3306; Lot
SLBJ0135V
Bioquant Total dietary
fibre
Merck 1.12979.001
from Testkit Merck
1.12979.0001
Megazyme
Sigma P 3910; Lot
SLBL7614V
fibre
Merck 1.12979.001
from Testkit Merck
1.12979.0001
Dietary fibre kit
Megazyme
Megazyme
Sigma A 9913; Lot
091M8701V
fibre
Merck 1.12979.001
protease, 350 tyrosine
units/ml (Megazyme)
amyloglucosidase, 3300
units/ml (Megazyme)
4,5 cm
30 mm
40-100 µm
40 mm
40-90 µm
3 cm
2
N/A
Filtering paper MN
640W
N/A
30 mm
2
3.3 cm
40-100 μm
α-amylase, 3000 units/ml
(Megazyme)
Ballaststoffkit Megazyme
13
Seite 27 von 31
May 2016
Teilnehmer
Angaben zur Inulinase
Methode ohne
Inulinase ist
akkreditiert
Participant
Notes to Inulinase
Method is accredited
without Inulinase
Parameter
Analyte
Ballaststoffe /
dietary fibre
1
no
2
yes
3
4
5
6
7
8
9
10
11
12
13
yes
yes
N/A
Fluka 57620; Lot BCBF4971V
not applicable
yes
yes
Yes
yes
yes
yes
no
Methode mit
Inulinase ist
akkreditiert
Method ist
accredited with
Inulinase
no
N/A
yes
no
yes
not applicable
Seite 28 von 31
May 2016
Parameter
Analyte
Teilnehmer
Methodenbeschreibung
UV-Testkit Hersteller
HPLC Säule
Detektor
Participant
Method description
UV-Testkit
manufacturer
HPLC column
Detector
1
AOAC 997.08
/
2
3
AOAC 997 08/99
4
Inulin
5
6
7
8
In-house method
Fructan HK method
Testkit Thermo Fisher
AOAC 999.03
9
§64 LFGB L.00.00-94
10
11
ASU § 64 LFGB, L 00.00-94,
2006-09
HPLC
AOAC 997.08
(HPLC RI)
PA100 dionex
PAD
Methode ist
akkreditiert
Method is
accredited
no
no
x
GC FID
no
Megazym
Megazyme
NH2-RP
RI
n/a
n/a
n/a
yes
yes/no
no
No
r-biopharm 10716260;
Lot 10759000 May
2016
yes
r-biopharm
10716260035
yes
12
AOAC 999.03
not applicable
13
LAV 21.0051.01
r-Biopharm
Angaben zur Inulinase
Notes to Inulinase
no
x
Dionex CarboPac
PA1
Angaben zur
Amyloglucosidase
Notes to
Amyloglucosidase
RI
yes
PAD
no
sigma
remark : result=
fructans
ja
Seite 29 von 31
Sigma-Aldrich 57620
exo- and endo-inulinase
(Megazyme)
May 2016
6. Index of participant laboratories in alphabetical order
Teilnehmer / Participant
Ort / Town
Land / Country
Germany
Germany
Germany
Germany
Germany
Germany
BELGIUM
Germany
Germany
ITALY
NETHERLANDS
ENGLAND
BELGIUM
[Die Adressdaten der Teilnehmer wurden für die allgemeine Veröffentlichung des Auswerte-Berichts nicht angegeben.]
[The address data of the participants were deleted for publication of the evaluation report.]
Seite 30 von 31
May 2016
7. Index of references
1. DIN EN ISO/IEC 17043:2010; Konformitätsbewertung – Allgemeine
Anforderungen an Eignungsprüfungen / Conformity assessment – General
requirements for proficiency testing
2. Verordnung / Regulation 882/2004/EU; Verordnung über amtliche Kontrollen /
Regulation on official controls
3. DIN EN ISO/IEC 17025:2005; Allgemeine Anforderungen an die Kompetenz von
Prüf- und Kalibrierlaboratorien / General requirements for the competence
of testing and calibration laboratories
4. Richtlinie / Directive 1993/99/EU; über zusätzliche Maßnahmen im Bereich
der amtlichen Lebensmittelüberwachung / on additional measures concerning
the official control of foodstuffs
5. ASU §64 LFGB : Planung und statistische Auswertung von Ringversuchen zur
Methodenvalidierung
6. DIN ISO 13528:2009; Statistische Verfahren für Eignungsprüfungen durch
Ringversuche / Statistical methods for use in proficiency testing by
interlaboratory comparisons
7. The International Harmonised Protocol for the Proficiency Testing of
Ananlytical Laboratories ; J.AOAC Int., 76(4), 926 – 940 (1993)
8. The International Harmonised Protocol for the Proficiency Testing of
Ananlytical Chemistry Laboratories ; Pure Appl Chem, 78, 145 – 196 (2006)
9. Evaluation of analytical methods used for regulation of food and drugs;W.
Horwitz; Analytical Chemistry, 54, 67-76 (1982)
10.A Horwitz-like funktion describes precision in proficiency test; M.
Thompson, P.J. Lowthian; Analyst, 120, 271-272 (1995)
11.Protocol for the design, conduct and interpretation of method performance
studies; W. Horwitz; Pure & Applied Chemistry, 67, 331-343 (1995)
12.Recent trends in inter-laboratory precision at ppb and sub-ppb
concentrations in relation to fitness for purpose criteria in proficiency
testing; M. Thompson; Analyst, 125, 385-386 (2000)
13.ASU §64 LFGB: L 00.00-18: Bestimmung der Ballaststoffe in Lebensmitteln
14.ASU §64 LFGB: L 16.08-1: Bestimmung der Ballaststoffe in Getreidekleie
15.ASU §64 LFGB: L 17.03-1: Bestimmung der Ballaststoffe in Mischbrot
16.ASU §64 LFGB: L 48.01-25: Bestimmung der Ballaststoffe in Säuglings- und
Kindernahrung auf Milchbasis
17.ASU §64 LFGB: L 00.00-94: Bestimmung von Inulin in Lebensmitteln
18.Chávez-Servín et al. (2004) Analysis of mono- and disaccharides in milkbased formulae by high-performance liquid chromatography with refractive
index detection. J Chromatogr A. 1043(2):211-5
Page 31 of 31

Dietary Fibre and Inulin in cereal food

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