DICLOFENAC Validation according to requirements

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Presentation transcript:

DICLOFENAC Validation according to 17025 requirements EQS: 0.1 µg/L in surface water 0.01 µg/L in other (coastal) waters Validation according to 17025 requirements SPE-LC-MS/MS method Sample volume: 1L Limit of detection (0.1 ng/L) LOD=b+3SD, where b is the mean value of blank samples (n=15) and SD is their relative standard deviation Limit of quantification (0.2 ng/L) LOQ=b+10SD, where b is the mean value of blank samples (n=15) Linearity Evaluated by R2 and residual plots of extracted spiked calibration standards on 5 different days Working range (0.2-97.3 ng/L) Defined by the LOQ and the highest point of calibration curve Recovery (71.2%) Trueness Assessed by significance test (t-test) on 15 replicate quality control samples (QCs) at low (2.91 ng/L) and high (87.3 ng/L) spiking level) Repeatability and Intermediate Precision Assessed by one-way ANOVA on fifteen replicate quality control samples (QCs) at at low (2.91 ng/L) and high (87.3 ng/L) spiking level) Extract stability Evaluated after one week storage at 4°C in the dark. The acceptance criteria established requires the concentration fall within 2 SD Sample stability Evaluated in water samples stored at 4°C for 38, 83 and 96 days. Uncertainty budget

E2 and EE2 Validation according to 17025 requirements Parameters E2 AA-EQS 400 pg/L 35 pg/L LOQ (at 1/3 EQS) Yes No Recovery >75% Sample volume: 1 L Parameter Same approach than used for diclofenac method validation Limit of detection Limit of quantification Linearity Working range Recovery Trueness Repeatability and Intermediate Precision Extract stability Sample stability Uncertainty budget Validation report for E2 in 1 L water sample foreseen within 2014 EE2 E2

Sample volume: 10 L Mariani Box 1 2 3 4 5 6 Parameters E2 EE2 AA-EQS Battery 12 V Flow-meter/Counter Pump (Flow rate: 0.1-0.2 L/min) Holder-SPE: adsorbent Water Sampling line Waste Mariani Box Isochronous stability experiment (0-10 weeks) 1 2 3 4 5 6 30 cm Parameter Ad hoc validation scheme considering the complexity of 10 L sample volume manipulation Limit of detection Limit of quantification Linearity Working range Recovery Trueness Repeatability and Intermediate Precision Extract stability Sample stability Uncertainty budget Validation report for E2 and EE2 in 10 L water sample foreseen within end of March 2015 In details, my presentation will touch the following topics: After the presentation of JRC role and mission, I will briefly cite the regulations addressed for our role execution before entering into details of the watch list pilot exercise currently on-going, the presentation of the soft-shell concept, of the European Innovation partnership on water and of the Information Platform for chemical monitoring. Parameters E2 EE2 AA-EQS 400 pg/L 35 pg/L LOQ (at 1/3 EQS) Yes Recovery >75% 20 May 2019