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BS EN 14526:2025 Foodstuffs. Determination of saxitoxin-group toxins in shellfish. HPLC method using pre-column derivatization with peroxide or periodate oxidation >
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BS EN 14526:2025 Foodstuffs. Determination of saxitoxin-group toxins in shellfish. HPLC method using pre-column derivatization with peroxide or periodate oxidation, 2026
- undefined
- European foreword
- Introduction
- 1 Scope
- Table 1 — Lowest validated levels
- 2 Normative references
- 3 Terms and definitions
- 4 Principle
- Table 2 — Reaction products after oxidation with periodate and peroxide
- Figure 1 — Reaction products after derivatization with peroxide and periodate (peaks for quantification are marked with arrows)
- 5 Reagents
- Table 3 — Example of suitable compositions and concentrations for each PSP toxin in four stock solution mixtures
- 6 Apparatus
- 7 Procedure [Go to Page]
- Table 4 — Options of fractionation conditions [Go to Page]
- 8 HPLC determination
- Table 5 — Recommended mobile phase gradient at a flow of 2 ml/min
- Figure 2 — Schematic overview of procedure
- 9 Calibration curve
- 10 Identification
- 11 Calculation [Go to Page]
- Table 6 — Calculation to be applied for the different toxin compositions [Go to Page]
- Figure 3 — Chromatograms explaining the calculation of GTX1,4 in the presence of GTX2,3 and dcGTX2,3 [Go to Page]
- Figure 4 — Chromatograms explaining the calculation of NEO in the presence of dcSTX [Go to Page]
- Figure 5 — Chromatograms explaining the calculation of NEO in the presence of dcSTX, dcNEO and STX [Go to Page]
- Figure 6 — Chromatograms explaining the calculation of dcNEO in the presence of dcSTX [Go to Page]
- Table 7 — Toxicity equivalent factors (TEFs) of the PSP Toxins
- 12 Quality controls [Go to Page]
- Table 8 — Method performance criteria for series of analysis [Go to Page]
- 13 Verification
- Table 9 — Method performance criteria for verification
- 14 Test report
- Annex A (informative) Precision data
- A.1 Interlaboratory study organized by the Health Canada (2001)
- Table A.1 — Characteristics of samples
- A.2 Performance test for the total toxicity organized by the Community Reference Laboratory of Marine Biotoxins (CRLMB) 7F 2006
- Table A.2 — Characteristics of samples from performance test
- A.3 Determination of PSP toxins in shellfish including GTX6 after hydrolysis organized by the Community Reference Laboratory of Marine Biotoxins (CRLMB)8 2007
- Table A.3 — Characteristics of samples
- A.4 Extension of the validation including dcGTX2,3 and dcNEO provided by the Community Reference Laboratory of Marine Biotoxins (CRLMB)8 2008
- Table A.4 —Characteristics of samples
- Table A.5 — Precision data for STX after SPE C18 clean-up obtained by the interlaboratory study A.1
- Table A.6 — Precision data for STX after SPE-COOH clean-up obtained by the interlaboratory study A.1
- Table A.7 — Precision data for NEO after SPE C18 clean-up obtained by the interlaboratory study A.1
- Table A.8 — Precision data for NEO after SPE-COOH clean-up obtained by the interlaboratory study A.1
- Table A.9 — Precision data for dcSTX after SPE C18 clean-up obtained by the interlaboratory study A.1
- Table A.10 — Precision data for dcSTX after SPE-COOH clean-up obtained by the interlaboratory study A.1
- Table A.11 — Precision data for GTX1,4 (together) after SPE C18 clean-up obtained by the interlaboratory study A.1
- Table A.12 — Precision data for GTX1,4 (together) after SPE-COOH clean-up obtained by the interlaboratory study A.1
- Table A.13 — Precision data for GTX2,3 (together) after SPE C18 clean-up obtained by the interlaboratory study A.1
- Table A.14 — Precision data for GTX2,3 (together) after SPE-COOH clean-up obtained by the interlaboratory study A.1
- Table A.15 — Precision data for GTX5 after SPE C18 clean-up obtained by the interlaboratory study A.1
- Table A.16 — Precision data for GTX5 after SPE-COOH clean-up obtained by the interlaboratory study A.1
- Table A.17 — Precision data for C1,2 (together) after SPE C18 clean-up obtained by the interlaboratory study A.1
- Table A.18 — Precision data for C1,2 (together) after SPE-COOH clean-up obtained by the interlaboratory study A.1
- Table A.19 — Precision data for C3,4 (together) after SPE-COOH clean-up obtained by the interlaboratory study A.1
- Table A.20 — Precision data for the blind duplicates after SPE C18 clean-up obtained by the interlaboratory study A.1
- Table A.21 — Precision data for the blind duplicates after SPE-COOH clean-up obtained by the interlaboratory study A.1
- Table A.22 — Precision data for total toxicity obtained by performance test A.2
- Table A.23 — Precision data for total toxicity for the blind duplicates obtained by performance test A.2
- Table A.24 — Precision data for dcGTX2,3 obtained by interlaboratory study A.3 and A.4
- Table A.25 — Precision data for C1,2 obtained by the interlaboratory study A.3 and A.4
- Table A.26 — Precision data for dcSTX obtained by the interlaboratory study A.3 and A.4
- Table A.27 — Precision data for GTX5 obtained by the interlaboratory study A.3 and A.4
- Table A.28 — Precision data for dcNEO obtained by the interlaboratory study A.4
- Table A.29 — Precision data for GTX6 obtained by the interlaboratory study A.3 and A.4
- Table A.30 — Precision data for total toxicity obtained by the interlaboratory study A.3 and A.4
- Table A.31 — Precision data for the blind duplicates obtained by the interlaboratory study A.4
- Annex B (informative) Chromatograms
- Figure B.1 — Chromatogram Mix 1 (GTX1,4 and NEO) after periodate oxidation – 1 μM (see Table 3)
- Figure B.2 — Chromatogram Mix 2 (dcGTX2,3, C1,2, dcSTX, GTX2,3, GTX5 and STX) after periodate oxidation – 1 μM (see Table 3)
- Figure B.3 — Chromatogram Mix 3 (dcNEO) after periodate oxidation – 1 µM (see Table 3)
- Figure B.4 — Chromatogram Mix 4 (C3,4 and GTX6) after periodate oxidation – 1 μM (see Table 3)
- Figure B.5 — Chromatogram All toxins (GTX1,4, NEO, dcGTX2,3, C1,2, dcSTX, GTX2,3, GTX5, STX, dcNEO, C3,4 and GTX6) after periodate oxidation – 0,25 μM
- Figure B.6 — Chromatogram Mix 2 (dcGTX2,3, C1,2, dcSTX, GTX2,3, GTX5 and STX) after peroxide oxidation – 1 μM (see Table 3)
- Annex C (normative) Alternative calculation methods
- C.1 General
- C.2 Calculation of GTX1,4 in the presence of GTX2,3 and dcGTX2,3
- C.2.1 General
- C.2.2 Method 5
- C.2.3 Method 6
- C.2.4 Method 7
- C.2.5 Method 8
- C.2.6 Method 9
- C.3 Calculation of NEO in the presence of dcSTX
- C.3.1 General
- C.3.2 Method 10 [4], [5]
- C.3.3 Method 11
- C.3.4 Method 12 [4], [5]
- C.4 Calculation of NEO in the presence of dcSTX, dcNEO and STX
- C.4.1 General
- C.4.2 Method 13
- C.5 Calculation of dcNEO in the presence of dcSTX
- C.5.1 General
- C.5.2 Method 14
- Bibliography [Go to Page]