Improvement of efficiency by automation.

Transcription

1 Improvement of efficiency by automation

2 RIKILT

3 Mission RIKILT contributes to the safety and health of the Dutch food supply

4 Incidents: Dioxins in.. Dioxins in CPP 1998 Meltdown Tsjernobyl DES in meat April BSE Melamine in Chinese (milk) products November 1986 Chloormequat in pears 1999 Dioxins in Irish pork Dioxins in chicken May /2009 Dioxins in milk 1989 Antibiotics ongoing Nicotine in mushrooms 2009 MPA in Dutch pig meat Summer 2002

5 How did the dioxins get into the feed? Contaminated Oil Burner Bakery Waste Suspected Contamination source: Transformer Oil like Aroclor 1260 FSAI

6 National economy under threat. Nearly 20 Billion Food Industry 8.16 Billion in Exports in ,800 pig processing workers laid off by 10th Dec 10,000 Indirect Jobs Threatened Reputation Gone for Years FSAI

7 Automation of DIOXIN method Automation is needed : To increase sample throughput from per week To reduce delivery time from workings days To improve quality Better reproducibility reduction of measurement uncertainty Better recovery Etc To reduce costs

8 Method from Sample spike with 13 C labelled standards Sample extraction concentration Extract clean up add clean up standard concentration GC HRMS add Recovery standards

9 Extraction and Clean-up Soxhlet GPC Al 2 O 3 Carbon Semi automated system; combination of three columns using three different HPLC based systems In between evaporation is necessary

10 Concentration First evaporation step using the Rotavapor: From 100 ml to < 5 ml Takes 15 min

11 Concentration Second evaporation step using the Pierce heating module: 5 ml 10 µl in six steps Takes at least 45 min.

12 Cost of DIOXIN analysis; approach ( ) Serie : n =25 +QC Sample prep 3 FTE (MBO) Measurement using GC-HRMS; 2 FTE (HBO) Supervision; 0,5 FTE (scientist)

13 Cost of instrument ((price / depletion) + maintenance + C)) = xx per day Days of use

14 Cost of instrument ((2* / 5) + (10% van ) )) = 1500 per day 160

15 Cost of DIOXIN analysis samples Cost of instrument = 7.500,-- Cost of labour = ,-- Cost of chemicals = 2.500,-- Cost for sample handling = 825,-- Total cost = ,-- Per sample 1.200,--

16 Method from 2005 Sample spike with 13 C labelled standards Sample extraction concentration Clean up add clean up standard concentration GC HRMS add Recovery standards

17 Pump Main Transducer Inlet Valve Automated Extraction Transducer Nitrogen Solvents Nitrogen Valve Pressure Gauge G Calibration Valve PRESS. Relief Valve PLE cell. 5 ml loop Output valve Extract collector

18 Method from 2005 Sample spike with 13 C labelled standards Sample extraction concentration Clean up add clean up standard concentration GC HRMS add Recovery standards

19 Clean up after 2005 Still a three step procedure, however: In line by coupling a combination of four columns Acidified silica column + silica column (capacity 3 gram fat) Al2O3 column Carbon column

20 PowerPrep Purification of ASE extract Silica oxidation of fat Al 2 O 3 removal of interferences Carbon separation of a. PBDEs & MO PCBs & Ind. PCB s b. Dioxins & NO PCBs

21 1 com 2 M3 P.S. Pump Power-Prep System/Dioxin PCDDs/ PCDFs Separation Program Silica 1 com 2 M3 M2 common Step 1: Wet Silica Column 1 com 2 M4 1. Hexane 2. 2% CH2CL % CH2CL EtAc/Benz Alumina 1 com 2 M4 5. Toluene 6. Sample com 1 2 M5 POwerprep method rikilt.ppt Forward Reverse Carbon com M6 2 2 com 1 1 M7 com M6 1 1 com 2 M7 2 M8 1 com com 2 M5 1. PCDD Step Flow Volume M1 M2 M3 M4 M5 M6 M7 M collectors Waste 6 2. PCB 3. Fraction 1 4. Fraction 2 5. Fraction 3 6. Waste Legend: M2 and M8: 6 Way Valves M3 - M7: 2 Way Valves

22 Clean up after 2005 Both fractions are automatically unattended concentrated using Turbovap (recovery standard and keeper is added) Endpoint = 500 ul Concentrated fractions are analysed on two GC HRMS Fraction A 10 l using LVI (Gerstel CIS 4) Fraction B 100 l using LVI (Gerstel CIS 4)

23 Cost of DIOXIN analysis automated approach 25 samples *1 50 samples *2 Cost of instrument = 7.500, 9.000, Cost of labour = , , Cost of chemicals = 2.500, 6.500, Cost for sample handling = 825, 1.650, Total cost = , , Per sample 1.200, 700, *1 Max capacity *2 Can be increased to 100

24 Future

25 ECF Integrated System 20ml sharp pulse On-line evaporation 100ml & nitrogen Jef Focant

26 LIMS

27 What is SQL*LIMS? Laboratory Information Management System Use it to enter information about Samples, Tests (to be) performed Results. Tracking progress of samples from receipt until tests are completed.

28 WEB based system Data stored in an oracle database SQL*LIMS SQL*LIMS Client application Forms, ExcelResults, Reports SQL*LIMS WAT IS DAT?

29 Workflow from sample to result. Principal Sample receive Approving results Performing analyses Keten van monster tot resultaat.

30 Validation of the results and samples Analyst. Stores the final results in SQLLIMS: Validation 1. Specialist. Checks the final results on task level according to laboratory specifications: Validation 2. Projectmanager. Checks the final results on sample or submissions level: according to the law. Validation 3.

31 Reporting sample(s) result(s) Keten van monster tot resultaat.

32 Coupling GC-HRMS with LIMS

33 Radio activity; Coupling of Gammaster with LIMS

34 Summary / Conclusion Automation of method achieved by: Automated extraction (ASE /PLE) Automated clean-up (Power Prep) Automated concentration (Turbovap) LVI +ALEX (Gerstel) Coupling analytical instrument with LIMS

35 Summary / Conclusion Automation of method results in: Higher sample throughput (factor 4) with same number of staff Shorter delivery time Better quality Reduction of cost

36 Summary / Conclusion Coupling analytical instruments to LIMS results in: No or less mistakes Shorter reporting time Better insight in sample flow

37 Thank you for your attention Questions?