BS EN 16204:2012 pdf download

BS EN 16204:2012 pdf download.Foodstuffs —Determination of lipophilic algal toxins (okadaic acid group toxins,yessotoxins,azaspiracids, pectenotoxins) inshellfish and shellfish products by LC-MS/MS.
The lowest standard should be at or equal to the LOO.
Samples more highly concentrated than the highest calibration level can also be diluted with blank shellfish extract to obtain the Calibration renge
The ratio between intercept and slope is calculated and used as a quality parameter. The absolute value of thi5 ratio corresponds lo the concentration plotted on the x-axis nd shall not be greater than half the quantification limit. Additionally, the correlation coefficient (r2) should be equal to or greater than 0.985
7.6 Determination of algal toxins in sample test solutions
lnect aliquots of the sample test solution (6.2), (6,3) into the HPLC system in an appropriate sequence.
7.7 Quality control measures for sequences
All samples subject to quantitative determination of lipophilic algal toxins shall be analyzed at least by duplicate injection. The repeatability limit of the duplicate injection shall be smaller than 2,8 x r, where. r stands for the repeatability standard deviation of the extract,
To check the quality of chemical analysis. it has proven necessary to run simultaneously at least one QM sample per sequence. This sample should contain a known concentration of lipophilic algal toxins such as a sample with assigned value used in an inter-laboratory trial, a certified reference material (e.g. NRC Mus-b), a laboratory reference material, or a blank extractIblank homogenate spiked with standards. When tolerance or warning limits are defined, the different repeatabilty standard deviations of extracts and homogenates shall be taken into account
The matrix effects expected within a sequence shall be corrected as described in 8.3.
For the determination of lipopliic algal toxins the adoption of a defined sequence has been proven suitable, The following operations layout is recommended:
a) For sequences including more than 20 samples or exceeding a run time 0112 h:
1) calibration standards;
2) matrix correction standard:
3) QM sample:
4) samples (n > 20. first injection):
5) calibration standards;
6) matrIx correction standard:
7) QMsaniple;
B) samples (n > 20. second iiect1on);
9) optionally: one calibration standard
b) For sequences including less than 20 samples or a run time below 12 h:
1) samples (n C 20, first injection);
A.1 Details on the inter-laboratory study
The data given in Table Al to Table A.12 were ob(ained ii an international inter-laboratory study (see [8J.
(16)) organized by the Working Group Phycotoxins of the Federal Office for Consumer Protection and Food
Safety (Bundesamt fw Verbraucher5ctiutz und Lebensmittelsicherhett — BVL) according to the German Food
and Feed Code, Section 64 (Lebensmitlel- und Futtermittelgesetzbuch-LFGB, § 64) in accordance with
ISO 5725-2, -4 and 4 with 16 participating laboratories from different European countries (including 7 NRLs).
This validation study was carried Out In three independent sub-studies. Precision data for okadaic acid. DTX2, DTX-1 (including their esters). AZA-1 AZA-2. AZA-3, ‘(TX, 45-OH-YTX and PTX-2 were determined in naturally contaminated blue mussels (homogenate of cooked and raw mussels), spiked extracts of oysters (homogenate of raw shellfish) and spiked extracts of clams (homogenate of raw shellfish). Test samples 1 to 8 were analyzed by 13 laboratorIes by means of duplicate Injection (analogous to the repeatability standard deviation (SD) of an extract) In three separate sequences (intermediate conditions). Test samples 9 to 12 were analyzed by eight laboratorIes withm one single sequence by means of duplicate infection (analogous to the repeatability standard deviation (SD) of an extract). Test samples 13 to 16 were analysed by 15 laboratories within one single sequence by means of duplicate inlection (analogous to the repeatability standard deviation (SD) of an extract). The results of the statistical evaluation of the investigated toxins are given In Table Al to Table A.12. The corrected HORRAT values were calculated according to 1171.
The different analytical conditions, ie. acidic and basic mode phases, have been used by the different participants and had no influence on the laboratory results.
Sample 2 is a blank blue mussel homogenate which was found by al laboratories as an uncontaminated material.