Laboratory Performance Assessment. Spring Report. Test Material A

Transcription

1 Laboratory Performance Assessment Spring 2015 QS Fachgesellschaft Obst-Gemüse-Kartoffeln GmbH Report Test Material A Pesticide Residues in Red Pepper Purée June 2015

2 Index of contents Page 1. Scope of proficiency testing (PT) 3 2. Test items and homogeneity Summary of results of homogeneity testing 4 3. Requested testing parameters 5 4. Criteria of assessment and test items 5 5. Demonstration of the results 5 6. Remarks and comments 6 7. Results, tables and graphics 7.1 Summary 7.2 Rating of performance 7.3 Results of Acetamiprid 7.4 Results of Bupirimate 7.5 Results of Cyprodinil 7.6 Results of Flutriafol 7.7 Results of Pirimicarb-desmethyl 7.8 Results of Propamocarb 7.9 Results of Triadimenol page 2 of 23

3 1. Scope of proficiency testing (PT) This proficiency testing was run by QS Fachgesellschaft Obst-Gemüse-Kartoffeln GmbH. This proficiency testing represents an ability test. It is used to be an external quality assurance and shows on each testing field the performance/ability of the laboratory. This report refers to the performance assessment of laboratories which analysed test material A. Each laboratory received a sample of red pepper puree with seven spiked pesticides. 30 participants reported results and were evaluated. The evaluation and reporting was subcontracted to DRRR GmbH. 2. Test items and homogeneity QS required three different materials in terms of spiked pesticides. Thus, the three test materials partly differed in the type of spiked pesticides as well as in the levels of spiked pesticides. Test material A was distributed to thirty (30) participants. The test material for this Performance Assessment was prepared by the GLP department of LUFA Speyer. The homogeneity tests were performed by the LAVES Oldenburg, Germany. The material was distributed into labelled bottles with at least 100 g in each. The bottles were stored at - 20 C in the dark until distribution. The following pesticides were spiked to give the approximate final concentrations: 50 μg/kg Acetamiprid, 70 μg/kg Bupirimate, 280 μg/kg Cyprodinil, 80 μg/kg Flutriafol, 80 μg/kg Pirimicarb-desmethyl, 240 μg/kg Propamocarb and 90 μg/kg Triadimenol. page 3 of 23

4 2.1 Summary of results of homogeneity testing The homogeneity test was carried out at all requested parameters to get information about the principal suitability of the material for this proficiency testing. If the standard deviation (s material) of the material homogeneity is smaller than 30 % of a test statistic the samples are classified as homogenous. The test statistic is usually calculated of all previous proficiency testings with this material type determining the relative mean standard deviation as well as Uex of the relative mean standard deviation of all previous proficiency testings with this material type. The relative values are referred to absolute values related to the actual value of the material and are added to obtain the test statistic. When this rule could not be followed it will be proved if the higher variance is usual for this material type. The test statistic for the evaluation of the homogeneity test of test material A was calculated with the results from this proficiency testing round (), because no previous proficiency testing data is available for the requested parameter matrix combination. The homogeneity test was carried out at 10 representative random samples in double determination acc. to ISO (Intern. Harmonised Protocol). The homogeneity tests are subcontracted by: LAVES Oldenburg, Germany In the following table the evaluation of the homogeneity test is shown: parameter spiked level [µg/kg] mean (homogeneity test) [µg/kg] recovery (homogeneity test) [%] standard deviation of the material homogeneity (s material ) [µg/kg] test statistic [µg/kg] evaluation of the homogeneity test (s material < 30 % test statistic) Acetamiprid homogenous Bupirimate homogenous Cyprodinil homogenous Flutriafol homogenous Pirimicarbdesmethyl homogenous Propamocarb homogenous Triadimenol homogenous page 4 of 23

5 3. Requested testing parameters The participants were requested to report which pesticides the red pepper puree had been analysed for. The results had to be reported without consideration of the recovery. The participants were asked to report also recovery rates for the quantified pesticides. The limit of quantification (LoQ) had to be specified for all sought and found pesticides. The laboratories were requested to identify and quantify the following seven pesticides. Acetamiprid Bupirimate Cyprodinil Flutriafol Pirimicarb-desmethyl Propamocarb Triadimenol. 4. Criteria of assessment and test items The test materials for the 2015 Spring Laboratory Performance Assessment of QS Fachgesellschaft Obst-Gemüse-Kartoffeln GmbH were prepared by the GLP department of LUFA Speyer to provide individual test material tailored to QS needs. The performance assessment considers the following test criteria: No false negative results are reported (thus identification of all seven pesticides) No false positive results are reported Correct quantification of at least 5 pesticides related to the 70 % 120 % recovery criteria. Analytical results between 70 % and 120% of the spiked levels have been considered satisfying. 5. Demonstration of the results Each laboratory was given a number (laboratory code). A summarized evaluation of the laboratory performance is shown in table 1 to 3 according to the test criteria. The results of all participants analysing Test Material A are presented in tables 4 to 11. Each table follows a diagram with the individual results in ascending order. The diagrams include the spiked level and the accepted range of the respective pesticide. page 5 of 23

6 6. Remarks and comments The performance of laboratory 30 is rated as failed, because the results were not submitted within the deadline. 7. Results, tables and graphics 7.1 Summary Table 1: Summarized laboratory rating in test material A QS criteria number of participants percent of participants passed failed 7 23 total Table 2: Number of satisfactory participants in test material A QS criteria number of satisfactory participants number of participants satisfactory % all analyts identified all analyts identified and reported in acceptable results no false positive results page 6 of 23

7 7.2 Rating of performance Table 3: Rating laboratory code criterion 1 all analytes identified criterion 2 number of acceptable results criterion 3 number of false positive results rating 1 yes 7 0 passed 2 no 6 0 failed 3 yes 7 0 passed 4 no 4 0 failed 5 yes 3 0 failed 6 yes 5 0 passed 7 yes 7 0 passed 8 yes 7 0 passed 9 yes 7 0 passed 10 no 2 0 failed 11 yes 7 0 passed 12 yes 7 0 passed 13 yes 5 0 passed 14 no 6 0 failed 15 yes 7 0 passed 16 yes 7 0 passed 17 yes 6 0 passed 18 yes 7 0 passed 19 yes 6 0 passed 20 yes 7 0 passed 21 yes 7 0 passed 22 yes 7 0 passed 23 yes 7 0 passed 24 yes 7 0 passed 25 no 6 0 failed 26 yes 7 0 passed 27 yes 7 0 passed 28 yes 5 0 passed 29 yes 7 0 passed 30 yes 5 0 failed page 7 of 23

8 Table 4: Number of satisfactory results in test material A analyte number of satisfactory results total number of correct identification satisfactory (%) Acetamiprid Bupirimate Cyprodinil Flutriafol Pirimicarb-desmethyl Propamocarb Triadimenol page 8 of 23

9 7.3 Results of Acetamiprid Table 5: Results for Acetamiprid in test material A Acetamiprid - spiked level: 50 µg/kg laboratory code result (µg/kg) recovery (%) LoQ (µg/kg) accepted range (µg/kg): yes yes yes yes no 6 56, yes yes yes yes 10 25, no yes yes no ,3 10 yes yes yes yes yes yes yes yes yes 23 55, yes yes 25 no yes yes no yes yes page 9 of 23

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11 7.4 Results of Bupirimate Table 6: Results for Bupirimate in test material A Bupirimate - spiked level: 70 µg/kg laboratory code result (µg/kg) recovery (%) LoQ (µg/kg) accepted range (µg/kg): yes yes yes yes yes 6 82, yes yes yes yes 10 64, yes yes yes no ,2 10 yes ,9 10 yes yes yes yes yes yes yes yes 23 60, yes yes yes yes yes ,7 10 yes yes yes page 11 of 23

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13 7.5 Results of Cyprodinil Table 7: Results for Cyprodinil in test material A Cyprodinil - spiked level: 280 µg/kg laboratory code result (µg/kg) recovery (%) LoQ (µg/kg) accepted range (µg/kg): yes yes yes yes yes yes yes yes yes , yes yes yes yes ,5 10 yes ,1 10 yes yes yes yes yes yes yes yes , yes yes yes yes yes ,6 10 yes yes yes page 13 of 23

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15 7.6 Results of Flutriafol Table 8: Results for Flutriafol in test material A Flutriafol - spiked level: 80 µg/kg laboratory code result (µg/kg) recovery (%) LoQ (µg/kg) accepted range (µg/kg): yes yes yes no no 6 97, no yes yes yes 10 no yes yes yes ,9 10 yes yes yes yes yes yes yes yes yes 23 83, yes yes yes yes yes yes yes yes page 15 of 23

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17 7.7 Results of Pirimicarb-desmethyl Table 9: Results for Primicarb-desmethyl in test material A Pirimicarb-desmethyl - spiked level: 80 µg/kg laboratory code result (µg/kg) recovery (%) LoQ (µg/kg) accepted range (µg/kg): yes yes yes 4 no yes 6 96, yes yes yes yes 10 no yes yes yes 14 no ,9 10 yes yes yes yes no yes yes yes 23 68, yes yes yes yes yes ,9 10 yes yes yes page 17 of 23

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19 7.8 Results of Propamocarb Table 10: Results for Propamocarb in test material A Propamocarb - spiked level: 240 µg/kg laboratory code result (µg/kg) recovery (%) LoQ (µg/kg) accepted range (µg/kg): yes 2 no yes yes no no yes yes yes 10 no ,7 10 yes yes yes ,6 10 yes ,4 10 yes yes no yes yes yes yes yes , yes yes yes yes yes ,4 10 yes yes no page 19 of 23

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21 7.9 Results of Triadimenol Table 11: Results for Triadimenol in test material A Triadimenol - spiked level: 90 µg/kg laboratory code result (µg/kg) recovery (%) LoQ (µg/kg) accepted range (µg/kg): yes yes yes no no yes yes yes yes 10 no yes yes yes ,1 10 yes yes yes yes yes yes yes yes yes 23 81, yes yes yes yes yes ,2 10 no yes no page 21 of 23

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23 QS Fachgesellschaft Obst-Gemüse-Kartoffeln GmbH GF: Dr. H.-J. Nienhoff Schedestraße Bonn Tel Fax page 23 of 23