Journal of Aquatic Food Product Technology

ISSN: 1049-8850 (Print) 1547-0636 (Online) Journal homepage: http://www.tandfonline.com/loi/wafp20

WEFTA Interlaboratory Comparison on Salt

Determination in Fishery Products
Horst Karl PhD , Gran kesson , Monique Etienne , Almudene Huidobro
PhD , Joop Luten PhD , Rogerio Mendes PhD , Magarita Tejada PhD & Jrg
Oehlenschlger PhD
To cite this article: Horst Karl PhD , Gran kesson , Monique Etienne , Almudene Huidobro
PhD , Joop Luten PhD , Rogerio Mendes PhD , Magarita Tejada PhD & Jrg Oehlenschlger PhD
(2002) WEFTA Interlaboratory Comparison on Salt Determination in Fishery Products, Journal
of Aquatic Food Product Technology, 11:3-4, 215-228, DOI: 10.1300/J030v11n03_17
To link to this article: http://dx.doi.org/10.1300/J030v11n03_17

Published online: 15 Oct 2008.

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Date: 01 October 2016, At: 03:09

WEFTA Interlaboratory Comparison

on Salt Determination in Fishery Products
Horst Karl
Gran kesson
Monique Etienne
Almudene Huidobro
Joop Luten
Rogerio Mendes
Magarita Tejada
Jrg Oehlenschlger

ABSTRACT. The FAO/WHO Codex Alimentarius Commission has

laid down a Codex standard for salted and dried salted fish which requires an official determination method of the salt content. A draft of an
analytical method has been elaborated by a Codex working group and
the WEFTA working group on analytical methods and was asked to validate this method.
Seventeen laboratories out of 10 countries participated in a WEFTA
collaborative trial on salt determination in fish and fishery products.
Horst Karl, PhD, and Jrg Oehlenschlger, PhD, Professor, are affiliated with the
Federal Research Centre for Fisheries, Institute for Fishery Technology and Fish Quality, Palmaille 9, D-22767 Hamburg, Germany.
Gran kesson is affiliated with the Swedish Institute for Food and Biotechnology
(SIK), Box 5401, S-40229 Gteorg, Sweden.
Monique Etienne is affiliated with IFREMER, Rue de Lile d`Yeu, F- 44311 Nantes
Cedex 03, France.
Almudene Huidobro, PhD, is affiliated with the Netherlands Institute for Fisheries
Research RIVO-DLO, P.O. Box 68, NL-1970 AB Ijmuiden, The Netherlands.
Joop Luten, PhD, and Magarita Tejada, PhD, are affiliated with the Instituto de Frio
(CSIC) Ciudad Universitria, 28040 Madrid, Spain.
Rogerio Mendes, PhD, is affiliated with the Instituto Portugues de Investigacao
Maritima (IPIMAR), Avenue de Brasilia, P- 1401 Lisboa, Portugal.
Journal of Aquatic Food Product Technology, Vol. 11(3/4) 2002
http://www.haworthpressinc.com/store/product.asp?sku=J030
2002 by The Haworth Press, Inc. All rights reserved.

215

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JOURNAL OF AQUATIC FOOD PRODUCT TECHNOLOGY

Four samples containing different salt contents were distributed, including two spiked samples and two typical commercial products.
All laboratories applied a common method involving the precipitation
of fish proteins by Carrez I and II followed by titrimetric determination
of the salt content according to Mohr. They also carried out salt determination by their own home methods.
The following results were obtained:
The recovery rate of the common method was nearly quantitative and
the relative standard deviation for reproducibility was between 1.96 and
2.64%, depending on the sample. Larger variations were obtained between different laboratories when applying their home methods.
In one sample a significant difference of the measured salt content
was found between the average results of the common and the home
methods. Application of ashing of the sample before salt determination
always yielded in lower salt contents compared to other determination
procedures.
The common method is judged to be suitable as a standard method for
salt determination in fish and fishery products. [Article copies available
for a fee from The Haworth Document Delivery Service: 1-800-HAWORTH.
E-mail address: <getinfo@haworthpressinc.com> Website: <http://www.
HaworthPress.com> 2002 by The Haworth Press, Inc. All rights reserved.]

KEYWORDS. Fish, salt determination, collaborative study

INTRODUCTION
The use of salt in the preservation and processing of fish has a long tradition
and is widely applied in the fish industry. The variety of salt containing products includes heavily salted fish like dried salted cod (Baccalao), marinated
fish like Bismarckhering or lightly salted fish like Matjesharing. Each
product needs different amounts of salt often in combination with other ingredients to develop its full characteristics (Luten et al., 1997). Additionally, for a
range of products minimum salt concentrations are essential in respect of
parasitological (Karl et al., 1995) and or microbiological safety (Huss et al.,
1997). Thus, both, the determination and control of salt concentrations in fishery products are important for producers and official control laboratories.
Several salt determination methods exist which are frequently used by
industry and national control laboratories. Some European countries have implemented regulations on salt concentrations in fishery products (Bundesministerium fr Gesundheit, 1997) and the FAO/WHO Codex Alimentarius
Commission has laid down a Codex standard for salted and dried salted fish

Karl et al.

217

(Codex Committee on Fish and Fishery Products, 1995), but no reference

method is recommended either in Europe for fish and fishery products or by
the Codex Alimentarius Commission. A mandatory prerequisite of a method
to be accepted by Codex Alimentarius Commission after acknowledgement by
Codex Committee for Analysis and Sampling is the evaluation and validation
of performance data by an interlaboratory comparison study.
A draft of a method has been elaborated by a Norwegian/German working
group of the Codex Committee on Fish and Fishery products in 1995 and the
Analytical Working Group of the Western European Fish Technologists Association (WEFTA) has been asked to validate this method by an interlaboratory
comparison study. The aims were to test the variability of results of different
home methods in comparison to the well described common Codex method
(Codex Committee on Fish and Fisheries Products, 1995), both applied to the
same fish samples.
SAMPLES AND PARTICIPANTS
Four samples (Table 1) were prepared for this exercise, including one
spiked cod and one spiked mackerel sample. All preparations were tested for
homogeneity. All samples were canned and heat sterilized at 121C for 15 min
and coded by a letter A-D and a two digit code. Participants received detailed
instructions how to handle the samples and on the sample weight to be used.
Each participant was asked to carry out a duplicate analysis by the common
and their home method, respectively.
Seventeen laboratories (11 WEFTA laboratories, 4 Norwegian and 1 German official laboratory and 1 industry laboratory) participated in the collaborative study. The order of participants below does not correspond to the order
in later sections of this paper.
Participating Laboratories included

Food and Environmental Agency, Torshavn (Faroe Islands)

Swedish Institute for Food and Biotechnology (SIK), Gteborg (Sweden)
Directorate of Fisheries, Dept. of Quality Control, Central Laboratory,
Bergen, Norway

Directorate of Fisheries, Dept. of Quality Control, Regional Laboratory,

lesund, Norway

Directorate of Fisheries, Dept. of Quality Control, District Laboratory,

Troms, Norway

Directorate of Fisheries, Dept. of Quality Control, District Laboratory,

Svolvaer, Norway

Norwegian Herring Oil and Meal Industry Research Institute (SSF),

Fyllingsdalen, Norway

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JOURNAL OF AQUATIC FOOD PRODUCT TECHNOLOGY

Landesveterinr- und Untersuchungsamt, Halle, Germany

Federal Research Centre of Fisheries, Institute for Biochemistry and
Technology (two laboratories), Hamburg, Germany

Norda Lysell- Union Deutsche Lebensmittelwerke, Cuxhaven, Germany

RIVO-DLO Department of Environment, Quality and Nutrition, Ijmuiden,

The Netherlands
Rijksstation voor Zeevisserij, Ostend, Belgium
Rowett Research Institute, Aberdeen, UK
Instituto del Frio (CSIC), Madrid, Spain
Instituto Portugues de Investigacao Maritima (IPIMAR), Lisbon, Portugal
IFREMER, Nantes, France
ANALYSIS

Common Method
Draft Codex Method
Principle. The salt is extracted by water from the preweighed sample. After
the precipitation of the proteins, the chloride concentration is determined by titration of an aliquot of the solution with a standardized silver nitrate solution
(Mohr method) and calculated as sodium chloride.
Preparation of Sample
Before preparing a subsample, adhering salt crystals from salted fish should
be removed by brushing from the surface of the sample without using water.
Marinated fillets should be separated from the brine and drained in a sieve for
10 min.

TABLE 1. Description of test samples sent to participants for analysis

Identification

Description of sample

Series A

Thoroughly homogenised cod fillets, spiked with 15 % (w/w) sodium chloride

Series B

Commercially marinated herring fillets, deskinned and homogenised

Series C

Thoroughly homogenised mackerel fillets, spiked with 3.5 % (w/w) sodium

chloride

Series D

Commercially salted herring, filleted, deskinned and homogenised

All samples were canned and heat sterilised at 121C, 15 min.

Karl et al.

219

The entire sample should be subjected to a systematic cutting and randomization process to assure a subsample representative of the composition of the
whole fish or fishery product.
At least 100 g of subsample should be thoroughly homogenized by using an
high speed homogenizer. Determination should be performed at least in duplicate.
Procedure
i. Five gram of homogenized subsample is weighed into a 250 ml volumetric flask and vigorously shaken with approximately 100 ml water.
ii. Five milliliter of potassium hexacyano ferrate solution, 15% w/v (aq)
(Carrez I) and 5 ml of zinc sulphate solution, 30% w/v (aq) (Carrez II)
are added, the flask is shaken again.
iii. Water is added to the graduation mark.
iv. After shaking again and allowing to stand for precipitation, the flask
content is filtered through a folded paper filter.
v. An aliquot of the clear filtrate is transferred into an Erlenmeyer flask
and two drops of phenolphtalein are added. The aliquot is neutralized
with sodium hydroxide, 0.1 N until red, and diluted with water to approximately 100 ml.
vi. After addition of approximately 1 ml potassium chromate solution,
5% w/v (aq), the diluted aliquot is titrated under constant stirring, with
silver nitrate solution, 0.1 N. Endpoint is indicated by a faint, but distinct change in color. This faint reddish-brown color should persist after brisk shaking.
vii. Blank titration of reagents used should be done.
viii. Endpoint determination can also be made by using instruments like
potentiometer or colorimeter.
Calculation of Results
Following symbols are used for calculation:
A = volume of aliquot (ml)
C = concentration of silver nitrate solution in N
V = volume of silver nitrate solution in ml used to reach endpoint
and corrected for blank value
W = sample weight (g)
The salt content in the sample is calculated by using the equation:
Salt concentration (NaCl, % w/w) = (V*C*58.45*250*100) / (A*W*1000)
Results should be reported with one figure after the decimal point.

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JOURNAL OF AQUATIC FOOD PRODUCT TECHNOLOGY

Comments
At step (i) of the procedure, 5 g can also be weighed into a 100 ml beaker
and homogenized for 30 sec with 50 ml water using a high speed homogenizer.
Optional: a few drops of antifoaming agent can be added to prevent intensive
foaming due to homogenizing.
By using the given equation all chloride determined is calculated as sodium
chloride. However, it is impossible to estimate sodium by this methology, because other chlorides of the alkali and earth elements are present, which form
the counterparts of chlorides.
The presence of natural halogens other than chloride in fish and salt is negligible.
A step in which proteins are precipitated (ii), is essential to avoid misleading results.
Home Methods
In Table 2 principle procedures of the home methods used by participants
are described:
Home methods used by the participants varied mainly in the extraction step
of chloride before determination.
Four laboratories used as a first step an ashing of the samples followed by
an extraction of the chloride by water. Five laboratories used the AOAC
method (Hollingworth and Wekell, 1990) based on the digestion of the fish tissue with hot nitric acid. Five laboratories used as clearing step the precipitation
of proteins by Carrez I and II (Ludorff and Meyer, 1973; Anonymous, 1980),
and two laboratories extracted chloride directly from the samples by hot water
TABLE 2. Salt determination methods used by participants as home methods
Principle procedure

Laboratory no.

Reference

Ashing of the sample and extraction with water,

volumetric titration or chloride meter

2, 5, 7,16

Fiskeridirektoratet
Sentrallab, 1999

Extraction of the sample with hot water,

volumetric titration or chloride meter

15, 11,

Karl, 1992

Precipition of proteins by Carrez I and II, volumetric

titration or potentiometric endpoint determination

1, 4, 8, 10, 17,

Ludorff and Meyer,

1973

Digestion by hot HNO3, volumetric determination

3, 6, 9, 11, 12, 14

Hollingworth and
Wekell, 1990

Karl et al.

221

(Karl, 1992). In most cases determination of chloride was performed titrimetrically either according to Mohr or Volhard (Alvarez, 1990). Some laboratories used instrumental endpoint determination techniques.
Statistical Methods
Statistical processing of the data was carried out according to the collaborative study guidelines of the Journal of AOAC International (Anonymous,
1995) and the International Standard ISO 5725 (International Organization for
Standardization, 1986).

RESULTS AND DISCUSSION

The salt concentrations obtained by the common method are listed in Table 3
and results obtained by the home methods are compiled in Table 4. Data
marked in bold were omitted as outliers (Grubb test) and not included in
further calculations. The results of the statistical analysis are summarized in
Table 5.
Common Method
Differences Between and Within Laboratories
The variability within and between laboratories was relatively low and
uniform for all samples analyzed. The mean repeatability relative standard
deviation (RSDr), which gives an indication of the within laboratory variability, ranged between low 0.41 and 1.32%, depending on the sample. The
difference between the minimum and maximum salt content obtained for
each series was less than 10%. The reproducibility relative standard deviation (RSDR), a good measure for the among laboratory precision, which includes also the within laboratory repeatability, ranged between 1.96 and
2.64%. The results indicate a good homogeneity of the samples and demonstrates that the different laboratories, who had participated in this collaborative trial, were able to determine salt concentrations at different levels in fat,
lean and marinated fish matrices with reproducible accuracy when using the
common method.
The reproducibility relative standard deviations RSDR were found comparable to the Horwitz equation (RSDRH = 2(1-0.5 * log c)), which is dependent
from analyte concentration (c). This equation has been derived empirically
from an examination of more than 3000 method performance studies. It has

222
8

10

11

12

13

14

15

16

17

Bold = outliers according to Grubb-test

5.21
0
0

5.55
0.1
0.07

3.70
0.3
0.17
4.68

0.06
0.83

7.00

3.80
0
0

5.40
0
0

3.75
0.1
0.07

5.40
0.2
0.14

0.02
0.55

3.79

0.03
0.58

5.51

3.75
0.1
0.07

5.35
0.1
0.07

3.77
0.2
0.01

5.49
0
0

3.75
0.1
0.07

5.55
0.1
0.07

3.98
0.14
0.1

5.70
0.08
0.06

3.80
0
0

5.60
0
0

4.40
0
0

5.80
0
0

3.65
0.16
0.11

5.61
0.11
0.08

3.85
0.1
0.07

5.55
0.1
0.07

Salted herring
17.19 17.45 17.39 15.46 16.65 17.03 17.10 16.50 17.06 17
16.96 17.55 17.64 16.95 17.50 17.44 17.35
0.1
0.01
0.1
0.1
0
0.1
0.06
0.1
0
0.1
0
0.25
0.1
0.14
0.06
0.07
0.01
0.1
0.21
0.06
0.07
0
0.21
0.07
0.05
0.07
0
0.07
0
0.18
0.07
0.35
0.34
1.21

Series D
A. mean
Difference
SD
CV (%)

Mackerel, spiked with 3.5 % (w/w) salt

3.78
3.90
3.86
3.74
3.85
0
0
0.05
0.1
0.01
0
0
0.04
0.07
0.26

Series C
A. mean
Difference
SD
CV (%)

Marinated herring
5.41
5.60
5.57
0
0.01
0.04
0
0.01
0.7

Series B
A. mean
Difference
SD
CV (%)

Cod mince, spiked with 15 % (w/w) salt

15.29 15.45 15.32 15.34 15.10 15.40 15.00 14.70 15.02 15
14.75 15.65 15.44 15.11 15.90 15.48 15.40
0.1
0.03
0.04
0
0
0.2
0.1
0.12
0.1
0.04
0.2
0
0.09
0
0.13
0.07
0.02
0.03
0
0.14
0
0.14
0.14
0.07
0.08
0.07
0.02
0.14
0
0.06
0
0.85
0.92
0.90

Series A
A. mean
Difference
SD
CV (%)

Laboratory

TABLE 3. Arithmetric means, differences between duplicates, standard deviations (SD), and coefficient of variation
(CV) of salt determination in various samples (NaCl %), using the common method, lab 1, 6 and 9 performed triplicate
determinations

223

10

11

12

13

14

15

16

17

Bold = outliers according to Grubb-test

4.95
0.04
0.03

4.40
0.2
0.14

6.80
0.1
0.07

3.50
0
0

4.70
0
0

3.65
0.1
0.07

5.25
0.1
0.07

0.04
1.3

3.36

0.03
0.55

4.57

3.70
0
0

5.35
0.1
0.07

3.85
0.02
0.01

5.30
0.01
0.01

3.60
0
0

5.30
0.01
0.01

3.97
0.12
0.08

5.70
0.04
0.03

3.60
0
0

5.20
0
0

5.50
0
0

6.70
0.2
0.14

3.59
0.03
0.02

4.68
0.11
0.08

3.90
0
0

5.55
0.1
0.07

Salted herring
17.14 16.80 17.21 15.48 15.60 18.30 16.75 16.45 16.51 16.75 16.76 16.30 16.95 16.40 19.15 16.45 17.45
0
0.1
0.01
0.6
0.6
0.1
0.1
0.1
0.06
0
0.15
0
0.3
0.03
0.1
0.05
0
0.07
0.01
0.42
0.42
0.07
0.07
0.1
0.07
0.05
0
0.11
0
0.21
0.03
0.07
0.61
0.29

Series D
A. mean
Difference
SD
CV (%)

Mackerel, spiked with 3.5 % (w/w) salt

3.83
3.50
3.76
4.12
3.20
4.10
0
0.03
0.15
0
0
0.01
0
0.02
0.11
0
0
0.18

Series C
A. mean
Difference
SD
CV (%)

Marinated herring
5.45
4.70
5.52
0
0.03
0
0
0.02
0

Series B
A. mean
Difference
SD
CV (%)

Cod mince spiked with 15 % (w/w) salt

15.28 14.50 15.20 15.67 14.25 19.00 14.90 14.50 14.61 15.05 15.08 14.90 15.35 14.65 16.80 14.70 15.40
0
0.01
0
0.1
0
0
0.1
0.02
0
0.04
0.1
0
0.11
0
0.2
0.09
0
0.01
0
0.07
0.14
0
0
0.02
0.07
0.01
0
0.03
0.07
0
0.08
0
0.12
0.59

Series A
A. mean
Difference
SD
CV (%)

Laboratory

TABLE 4. Arithmetric means, differences between duplicates, standard deviations (SD), and coefficient of variation
(CV) of salt determination in various samples (NaCl %), using various home methods, lab 1 and 9 performed triplicate
determinations

224

0.31
2.03
0.318
2.09
2.65
0.89

17
15.25
15.32
14.70
15.90
0.07
0.46
0.2

1.71

0.61
4.05
0.611
4.06

16
15.06
14.96
14.25
16.80
0.03
0.20
0.08
0.14
2.54
0.146
2.64
3.09
0.41

16
5.52
5.55
5.21
5.80
0.04
0.72
0.11
0.08
2.11
0.094
2.47
3.27
0.26

16
3.80
3.79
3.65
3.98
0.05
1.32
0.14

0.73

0.26
7.03
0.261
7.05

16
3.70
3.68
3.20
4.12
0.02
0.54
0.06

Series C (mackerel)
spiked with 3.5% (w/w) salt
common
home
method
method
NaCl % (w/w) NaCl % (w/w)

0.33
1.92
0.337
1.96
2.61
0.94

16
17.17
17.15
16.50
17.64
0.07
0.41
0.20

2.48

0.88
5.22
0.89
5.26

17
16.85
16.76
15.48
19.15
0.1
0.59
0.28

Series D
salted herring
home
common
method
method
NaCl % (w/w) NaCl % (w/w)

Vd (%)= relative standard deviation (between laboratory coeff. of variation)

RSDr = repeatability relative standard deviation
RSDR = reproducibility relative standard deviation
R = reproducibility value

1.88

0.67
12.64
0.671
12.66

17
5.30
5.30
4.40
6.80
0.04
0.75
0.11

Series B
marinated herring
common
home
method
method
NaCl % (w/w) NaCl % (w/w)

N = number of valid means, outlying laboratories are removed by Grubbs test

sL = among-laboratories variability
sr = repeatability standard deviation (random error),
sR = reproducibility standard deviation,
r = repeatability value
RSDRH = 2(1-0.5 * logc) Horwitz equation

SL
Vd (%)
SR
RSDR
RSDRH
R

Valid N
A. mean:
Median:
Min
Max
Sr
RSDr
R

Series A (cod)
spiked with 15% (w/w) salt
common
home
method
method
NaCl % (w/w) NaCl % (w/w)

TABLE 5. Statistical validation of collaborative study on salt determination

Karl et al.

225

been proposed that reproducibility relative standard deviation values found

within a range of 0.5-2 times the Horwitz RSDRH may be considered as an acceptable precision of method performance between laboratories (IUPAC,
1990). Lower reproducibility relative standard deviations than half of the
Horwitz RSDRH (given in Table 5) were never calculated from the data obtained by the common method.
The medians of the different series A-D are closely scattering around the
mean salt concentrations.
Recovery of Salt Added to Fish
Series A (cod mince) and C (mackerel mince) were spiked with high and
low levels of salt, respectively. In both cases, the salt content of the raw material has to be taken into account, when calculating recovery rates. The salt content of the raw mackerel was determined by the Hamburg laboratory to be
0.34% sodium chloride. The salt content of raw cod muscle, used for the calculation of the recovery rate, was taken from literature data. According to various
nutrition tables (Souci et al., 1994; Holland et al., 1993), salt levels in raw cod
vary between 0.13-0.26%.
The average recovery rates with the common method were nearly quantitative, 98.6% (mackerel) and 100 to 100.8% (cod) (see Table 6) and the between
laboratory variance (Vd%) was small: 2.11 and 2.03%, respectively.
Home Methods
Generally, average salt concentrations of the samples received by the application of different home methods were slightly lower (Table 5) compared to
the common method and the between laboratory variation was larger, but only
in case of series B a significant difference was found between results of the
common and the home method (t-test, p < 0.05).
The reproducibility relative standard deviation (RSDR) was at least twice as
high, ranging from 4-12.7%.
The average recovery rates for the spiked samples were also slightly lower:
94.6 % (mackerel) and 98.7-99.5% (cod), respectively (Table 6).
To get more detailed informations on the variance within the different home
methods, the laboratories were classified according to the principal of their
method, and data were recalculated within each category (Table 2). The comparison included the ashing method, the AOAC digestion method, the precipitation by Carrez reagents (Carrez method) and the common method. The
results are compiled in Figure 1.

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JOURNAL OF AQUATIC FOOD PRODUCT TECHNOLOGY

TABLE 6. Recovery rates of salt (NaCl) in spiked samples
Mackerel
0.34

NaCl raw (%)

Spiking level

3.5 % (w/w)
Common method

NaCl found (%)

Recovery rate (%)

Cod
0.13-0.262

0.0111

3.80
98.6

15.0 % (w/w)

Home method

Common method

3.70
94.6

Home method

15.26

15.06

100-100.8

98.7-99.5

1 n = 5 determinations
2 according to literature

The salt levels reported by the four laboratories which used the ashing procedure as home method, were generally lower compared to all other values received. Also the concentrations determined by this method in the spiked
samples were each well below the spiking levels. Obviously some losses of the
chloride have occurred during ashing.
All other procedures gave nearly the same values compared to the common
method. Therefore the above stated differences between home and common
method are probably related to a systematic error of the ashing procedure.

CONCLUSIONS
From the results presented it can be concluded that the majority of laboratories who had participated in this trial were able to analyze the salt content of the
samples with high accuracy when using the common method. The results between laboratories varied only slightly, as indicated by a small reproducibility
relative standard deviation ranging between 1.9 and 2.6%. The recovery rates
found for the spiked samples were nearly quantitative.
The handling of the common method is relatively simple and does not need
advanced laboratory equipment like the ashing procedure or the AOAC method,
where a muffle furnance or a fume cupboard are necessary.
Therefore, the tested common method, which in principle has been already
applied in German and other European fish control and research laboratories
for a long time, seems to be suitable as a standard method for salt determination in fish and fishery products.
The results further indicate, that ashing of a sample before salt determination can result in a loss of chloride and should only be used with care, whereas
the AOAC method also gave acceptable results.

227

NaCl % (w/w)

NaCl % (w/w)

Ashing method
Carrez method
AOAC method
Common method
Series C

Series A

4.1
4.0
Spiking level +
3.9 natural content
3.8
3.7
3.6
3.5
3.4
3.3
3.2
Ashing method
Carrez method
AOAC method
Common method

14.2

14.4

14.6

14.8

15.0

15.6
15.4 Spiking level +
natural content
15.2

15.8

15.6

16.0

16.4

16.8

17.2

17.6

18.0

4.2

4.6

5.0

5.4

5.8

6.2

6.6

Std. Dev.
Std. Err.
Mean
Ashing method
Carrez method
AOAC method
Common method

Series D

Ashing method
Carrez method
AOAC method
Common method

Series B

FIGURE 1. Comparison of different determination methods

NaCl % (w/w)
NaCl % (w/w)

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JOURNAL OF AQUATIC FOOD PRODUCT TECHNOLOGY

REFERENCES
Alvarez, R. 1990. Standard solutions and certified reference materials, standard solution of silver nitrate No. 941.18. In: Official Methods of Analysis, 15th edn.,
AOAC, Arlington, p. 644.
Anonymous. 1980. Bestimmung des Kochsalzgehaltes in Fleisch und Fleischerzeugnissen,
L06.00 5 Amtliche Sammlung von Untersuchungsverfahren nach 35 LMBG.
Anonymous. 1995. AOAC guidelines for collaborative study procedures to validate
characteristics of a method of analysis. J. Assoc. Off. Anal. Chem. Int. 78
(5):143A-160A.
Bundesministerium fr Gesundheit. 1997. Verordnung ber die hygienischen Anforderungen an Fischereierzeugnisse und lebende Muscheln (Fischhygiene-VerordnungFischHV) i.d.F. vom 6. Nov. 1997. Bundesgesetzbl. I, 2665.
Codex Committee on Fish and Fishery Products. 1995. Revised standard for salted fish
and dried salted fish of the gadidae family of fishes. Codex Stan 167, 1989, Rev
1-1995.
Codex Committee on Fish and Fishery Products. 1995. Method for the determination
of salt content. Draft elaborated by a Norwegian/German working group, Bergen.
Fiskeridirektoratet Sentrallaoratoriet. 1999. Sodium chloride in fish and fish products,
Method No. 49.
Holland, B., Brown, J., and Buss, D.H. 1993. Fish and Fish Products. The third supplement to McCance & Widdowsons The Composition of Foods (5th Edition), The
Royal Society of Chemistry.
Hollingworth, T. and Wekell, M. 1990. Fish and Other Marine Products, Salt in Seafood No. 937.09. In: Official Methods of Analysis, 15th edn., AOAC, Arlington,
p. 870.
Huss, H.H., Dalgaard, P., and Gram, L. 1997. Microbiology of fish and fish products.
In: Luten, J.B., Brresen, T., and Oehlenschlger, J. Seafood from producer to consumer, integrated approach to quality, Elsevier, Amsterdam, pp. 413- 430.
International Organization for Standardization. 1986. Precision of test methodsDetermination of repeatability and reproducibility for a standard test method by inter-laboratory tests, ISO 5725.
IUPAC. 1990. Analytical, applied and clinical chemistry divisions; Interdivisional
working party for harmonization of quality assurance schemes for analytical laboratories: Harmonized protocol for the adoption of standardized analytical methods
and for the presentation of their performance characteristics. Pure Appl. Chem.
62:149-162.
Karl, H., Roepstorff, A., Huss, H.H., and Bloemsma, B. 1995. Survival of Anisakis larvae in marinated herring fillets. Int. J. Fd. Sci.Technol. 29: 661-670.
Karl, H. 1992. Vergleich verschiedener Methoden zur Essigsure- und Kochsalzbestimmung in Marinaden. Infn Fischw. 39(3):137-143.
Ludorff, W. and Meyer, V. 1973. Fische und Fischerzeugnisse, Verlag Paul Parey,
Berlin, Hamburg, pp. 222-223.
Luten, B.J., Borresen, T., and Oehlenschlger, J. 1997. Seafood from producer to consumer, integrated approach to quality. Processing, Packaging and Distribution: Effects of ripening. Elsevier, Amsterdam, pp. 283-351.
Souci, S.W., Fachmann, W., and Kraut, H. 1994. Food Composition and Nutrition Tables. 5th edition. CRC Press, London, Tokyo.