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Page 1 of 24
Food Chem. Report 27211
Participants can log in to Fapas® SecureWeb at any time to obtain their laboratory number for
this proficiency test.
Laboratory numbers are displayed in SecureWeb next to the download link for this report.
REPORT INTEGRITY
Fapas® reports are distributed as digitally signed Adobe® PDF files. When these files are
opened with Adobe® Reader v9 or later, a blue ribbon and information bar indicates that the
certificate has been validated. This confirms that the author of the report is Fapas® and that
the document has not been altered since it was signed [1, 2].
The integrity of hard copies of Fapas® reports cannot be assured in this way, i.e. printed
copies are not controlled. A watermark stating this appears on every page when a Fapas®
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report is printed.
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End users of Fapas® reports should ensure that either the PDF file they are viewing displays
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a valid Fapas® digital signature or that the content of their hard copy exactly matches the
content of a PDF file that displays a valid Fapas® digital signature.
QUALITY SYSTEMS PR
EN
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0009
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Fera hereby excludes all liability for any claim, loss, demands or damages of any kind
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whatsoever (whether such claims, loss, demands or damages were foreseeable, known or
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otherwise) arising out of or in connection with the preparation of any technical or scientific
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report, including without limitation, indirect or consequential loss or damage; loss of actual or
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anticipated profits (including loss of profits on contracts); loss of revenue; loss of business;
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loss of opportunity; loss of anticipated savings; loss of goodwill; loss of reputation; loss or
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damage to or corruption of data; loss of use of money or otherwise, and whether or not
advised of the possibility of such claim, loss demand or damages and whether arising in tort
(including negligence), contract or otherwise. This statement does not affect your statutory
rights.
Nothing in this disclaimer excludes or limits Fera liability for: (a) death or personal injury
caused by Fera negligence (or that of its employees, agents or directors); or (b) the tort of
deceit; [or (c) any breach of the obligations implied by Sale of Goods Act 1979 or Supply of
Goods and Services Act 1982 (including those relating to the title, fitness for purpose and
satisfactory quality of goods);] or (d) any liability which may not be limited or excluded by law
(e) fraud or fraudulent misrepresentation.
The parties agree that any matters are governed by English law and irrevocably submit to the
non-exclusive jurisdiction of the English courts.
© Copyright Fera Science Ltd (Fera) 2018. All rights reserved.
Page 2 of 24
Food Chem. Report 27211
SUMMARY
1. The test materials for Fapas® – Food Chemistry proficiency test 27211 were dispatched in
November 2017. Each participant received a canned fish test material to be analysed for
histamine.
2. An assigned value (xa) was determined for histamine and in conjunction with the standard
deviation for proficiency (σp) was used to calculate a z-score for each result.
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Histamine 223 60 85 71
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Page 3 of 24
Food Chem. Report 27211
CONTENTS
1. INTRODUCTION 5
1.1. Proficiency Testing 5
2. TEST MATERIAL 5
2.1. Preparation 5
2.2. Screening and Homogeneity 5
2.3. Dispatch 5
3. RESULTS 5
4. STATISTICAL EVALUATION OF RESULTS 6
4.1. Calculation of the Assigned Value, xa 6
4.2. Standard Deviation for Proficiency, σp 6
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4.3. Individual z-Scores 6
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5. INTERPRETATION OF SCORES 7
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6. REFERENCES 7
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TABLES
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Table 1: Results and z-Scores 8
Table 2: Participants’ Comments 11
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FIGURES
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APPENDICES
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Food Chem. Report 27211
1. INTRODUCTION
2. TEST MATERIAL
2.1. Preparation
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Preparation of the samples for this proficiency test was sub-contracted to a laboratory meeting
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the quality requirements of the scheme’s accreditation [3].
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The test material was prepared from pilchards in tomato sauce.
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Histamine was spiked into the test material.
Samples were stored at an ambient temperature until dispatch.
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2.2. Homogeneity
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To test for homogeneity, randomly selected test materials were analysed in duplicate. Testing
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These data showed sufficient homogeneity and were not included in the subsequent
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2.3. Dispatch
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The start date was 02 November 2017. Test materials were sent to 97 participants.
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3. RESULTS
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Food Chem. Report 27211
The assigned value, xa, for histamine was derived from the consensus of the results submitted
by participants.
The following results were excluded from the calculation of the assigned value:
i) non numerical results i.e. qualitative or semi-quantitative results,
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ii) results reported as approximately 10, 100 or 1000 × greater or smaller than the
majority of submitted results (as these were considered to be reporting errors),
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iii) results uncorrected for recovery unless stating N/A.
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For histamine, this procedure was straightforward and the robust mean was chosen as the
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assigned value.
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The standard deviation for proficiency, σp, was set at a value that reflects best practice for the
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analyses in question.
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For histamine, σp was derived from the appropriate form of the Horwitz equation [8].
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The values for σp used to calculate z-scores from the reported results of this test are given in
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Table 3.
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( x − xa )
z=
σp
where x = the participant’s reported result,
xa = the assigned value
and σp = the standard deviation for proficiency.
Participants’ z-scores for histamine are given in Table 1 and shown as a histogram in Figure 1.
It is possible for the z-scores published in this report to differ slightly from the z-score that
can be calculated using the formula given above. These differences arise from the necessary
rounding of the actual assigned values and standard deviations for proficiency prior to their
publication in Table 3.
The number and percentage of z-scores in the range -2 ≤ z ≤ 2 for histamine are given in
Table 4.
Page 6 of 24
Food Chem. Report 27211
5. INTERPRETATION OF SCORES
In normal circumstances, over time, about 95% of z-scores will lie in the range -2 ≤ z ≤ 2.
Occasional scores in the range 2 <|z| <3 are to be expected, at a rate of 1 in 20. Whether or
not such scores are of importance can only be decided by considering them in the context of
the other scores obtained by that laboratory.
Scores where |z| >3 are to be expected at a rate of about 1 in 300. Given this rarity, such
z-scores very strongly indicate that the result is not fit-for-purpose and almost certainly
requires investigation.
The consideration of a set or sequence of z-scores over time provides more useful information
than a single z-score. Examples of suitable methods of comparison are provided in the IUPAC
International Harmonised Protocol for the Proficiency Testing of Analytical Chemistry
Laboratories [7].
6. REFERENCES
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1 Adobe Approved Trust List,
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https://helpx.adobe.com/acrobat/kb/approved-trust-list2.html#Whatisit
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accessed 01/06/2017.
2 GlobalSign PDF Signing Tool, https://www.globalsign.com/en/pdf-signing/
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accessed 01/06/2017
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testing.
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4 Fapas®, 2017, Protocol for Proficiency Testing Schemes, Version 6, April 2017,
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5 Fapas®, 2017, Protocol for Proficiency Testing Schemes, Version 5, April 2017,
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7 Thompson, M., Ellison, S.L.R. and Wood, R., 2006, The International Harmonised
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Protocol for the Proficiency Testing of Analytical Chemistry Laboratories, Pure Appl.
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8 Thompson, M., 2000, Recent trends in inter-laboratory precision at ppb and sub-ppb
concentrations in relation to fitness for purpose criteria in proficiency testing, Analyst,
125, 385-386.
Page 7 of 24
Food Chem. Report 27211
Histamine
assigned value: 223 mg/kg
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006 232 Not determined 12 0.6
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007 67.3 na -9.9
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008 247 100 10 1.5
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009 176 100 5 -3.0
010 191.71 99.5 0.5 -2.0
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011 205.2 na 2.6 -1.1
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Food Chem. Report 27211
Histamine
assigned value: 223 mg/kg
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037 191.94 102.55 -2.0
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038 205 NA 1 -1.1
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039 230 NA 1 0.4
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040 211.99 90.9 5 -0.7
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041 225.4 not applied 0.1
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mg/kg
043 206 na -1.1
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Page 9 of 24
Food Chem. Report 27211
Histamine
assigned value: 223 mg/kg
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067 256.06 101.9 <1 2.1
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068 171.21 100.00 <10 -3.3
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069 182.28 95 2 -2.6
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070 15.25 90% -13.1
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071 245.92 101 20 1.4
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Page 10 of 24
Food Chem. Report 27211
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Table 3: Assigned Values and Standard Deviations for Proficiency
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analyte data points, assigned value, uncertainty, standard deviation for
n xₐ u proficiency, σp
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mg/kg
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Histamine 60 85 71
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Page 11 of 24
Food Chem. Report 27211
255 mg/kg
223 mg/kg
191 mg/kg
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28
64
86
48
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46
30
75
50
67
80
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Laboratory Number
4
EN 66
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14
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60
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-10.0
8.0
6.0
4.0
2.0
0.0
-2.0
-4.0
-6.0
-8.0
z-score
Food Chem. Report 27211
HPLC Methods
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Reference laboratory number
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2001 082 085
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Agilent LCMSMS Method 018
AOAC Official Methods 066
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AOAC Official Methods 1984 14 003
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Page 13 of 24
Food Chem. Report 27211
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perchloric acid 004 013 018 028 030 042 049 058 059 060
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071 080 081
phosphate buffer 020 076
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water 018 020 023 049 054
hydrochloric acid 003
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MeOH:Water=75:25 053
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Tricloroacetico 085
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N
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blend / homogenise with solvent 003 013 018 019 029 040 059 067
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Food Chem. Report 27211
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Sample Clean-up Technique laboratory number
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carbon based column 067
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extraction 058
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filter 005 013 016 019 021 047 071 082 085
solid phase extraction (SPE) 012 029 040 056 076
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(column/cartridge)
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Dowex 027
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Food Chem. Report 27211
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Methanol 067
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Methanol:Ammonia water=95:5 040
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phosphate bufor 029
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EN
HPLC Injection Volume (µl) laboratory number
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≥10 - <25 003 004 018 019 020 023 028 029 030 040
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042 047 049 053 054 056 059 060 080 081
082 085
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≥25 - <50
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058 076
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C18 003 004 013 018 019 020 021 023 028 029
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030 040 042 053 058 059 067 071 076 080
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Food Chem. Report 27211
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methanol 018 021 023 029 053 058 060 082 085
phosphate 016 049 067
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sodium hydroxide 047
water 003 004 018 019 020 028 056 058 060 080
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081 082 085
60:40 1.2%Methylamine and 22.5% 076
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Page 17 of 24
Food Chem. Report 27211
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OPA & mercaptoethanol 049
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o-Phthaldialdehyde 021
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Source of Standards
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laboratory number
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Acros 018 029 053 082
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Merck 003
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Sigma/Aldrich 005 012 016 019 021 023 028 030 042 049
056 058 059 060 067 071 076 080 085
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Supelco 013
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Wako 047
TCI 040
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Diode Array Detector 003 013 029 060 071 080 081 082
fluorescence 016 021 023 040 047 049 053 056 076
MS 005 018 046 005 018 046
PAD 058
UV 004 019 028 030 042 059 067 085
Conductivity 012
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Food Chem. Report 27211
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330 049 053
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340 016 023 056
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345 076
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350 047
365 021
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390 040
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254 085
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418 021
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420 023
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425 056
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445 076
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480 040
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Food Chem. Report 27211
ELISA Methods
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ELISA Test Kit Name laboratory number
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Ridascreen Histamin 066
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Veratox for Histamine 038 064 065
histasure 011
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R1601 066
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7FCE3600 011
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E-3600 083
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FC E-3600 025
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Page 20 of 24
Food Chem. Report 27211
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ELISA Standards Used as Supplied (ready laboratory number
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to use) or Dilutions Required?
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as supplied 011 025 038 064 065 066
diluted 083
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Page 21 of 24
Food Chem. Report 27211
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Other Methods
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Is the Method Used Accredited? laboratory number
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yes 009 031 034 051 061 068
no 037 038 039 043 045 047 050 063
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AFNOR 042
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Procedure 35.1.32
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CAPITULO 35.1.32
AOAC Official Methods 2012 19th Edition 037 068
AOAC Official Methods 2015 20 17 061
J. Food Science 1976 14 1282-1284 050
J. Food Science 1976 41 1282-1284 063
Methode Lerke & Bell(1978) 1978 Assurance 043
de la qualite en industrie Halieutique 99
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Food Chem. Report 27211
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Page 23 of 24
Food Chem. Report 27211
1. Fapas® SECUREWEB
Access to the secure area of our website is only available to participants in our proficiency
tests. Please contact us if you require a UserID and Password. Fapas® SecureWeb allows
participants to:
• Obtain their laboratory numbers for the proficiency tests in which they have
participated.
• View the results they submitted in past and current proficiency tests.
• Submit their results and methods for current tests.
• Review future tests they have ordered.
• Order proficiency tests, reference materials and quality control materials.
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• Freely download copies of reports (PDF file), of proficiency tests in which they have
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participated.
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• View charts of their z-scores obtained in previous Fapas® – Food Chemistry
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proficiency tests. EN
2. PROTOCOL
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The Protocols [4, 5] set out how Fapas® – Food Chemistry is organised. Copies can be
downloaded from our website.
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3. CONTACT DETAILS
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This report was prepared and authorised on behalf of Fapas® by Dominic Anderson (Round
Coordinator). Participants with any comments or concerns about this proficiency test should
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contact:
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Fapas®
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