High sample throughput in a modern dioxin laboratory using dual acquisition

Transcription

1 High sample throughput in a modern dioxin laboratory using dual acquisition Wim Traag *1 and Jeroen Markesteijn *2 *1 DSP-Systems, Erichemseweg 7, 4117GG Erichem The Netherlands *2 Nofalab, Jan van Galenstraat 41, 3115JG Schiedam, The Netherlands Information:

2 Nofalab is founded in 2004

3 Core business of Nofalab Edible oils and fats Nuts/sub-tropical fruits spices and grains Food and Feed safety Bio fuels Micro-biology 3

4 New laboratory opened April 2014 and extended in 2015

5 Lab manager Jeroen Markesteijn at the Thermo Scientific DFS high resolution mass spectrometer

6 Two DFS high resolution mass spectrometers both equipped with dual acquisition

7 Dioxin analysis at Nofalab How it all started (2008) Before 2008 approximately samples per year were outsourced In 2008 the first generation of an automated system for clean-up and a DFS were purchased, accreditation was obtained Number of samples increased yearly; food and feed

8 Analysis GC-HRMS The Golden Standard Automated extraction >P and >T Automated clean-up Separation of: MO-PCBs + NDL PCBs (fraction A) Dioxins + NO-PCBs (fraction B) GC/HRMS

9 Dioxin analysis at Nofalab Total number of samples per year around % fat/oil type direct dilution no extraction needed 20% cereal based (animal feed), minerals, meat, fish(meal),eggs etc; extraction is required e.g. PLE, Schmedes etc. Average weekly number of samples 160 Turn around time: 5 % of samples within 8 hrs 40 % of samples within 24 hrs 50 % of samples within 2-3 days 5 % of samples within 2 weeks For 2015/16 increase of 15% is expected and focus on 8 hrs TaT

10 How do they manage Average weekly number of samples 160 On top at least 15 QA samples + 15 Procedure blanks Often 10 samples reanalysis Total number of samples is fractions On top at least 10 dioxins standards + 10 DL and NDL- PCB standards Total number of injections is meter nonpolar column run-time for each fraction 60 minutes In case of two single GC-HRMS instruments 210 hrs required per instrument Lack of > 42 hrs per week Solution combination of ultimate clean-up and dual acquisition

11 How do they manage? The new of purification system The Fully-Automated Sample Preparation System for dioxins and PCBs analysis has three features High Performance Clean-up User-friendly Column Design Unique way of flow switching Main advantages Low solvent consumption Hexane 90 ml Toluene 4 ml Run-time 90 minutes No cross contamination Columns easy to connect and no leakage High quality chromatograms

12 Background --- Features of New System High performance clean-up 4 columns Silver nitrate Si column Sulfuric acid Si column Carbon column Alumina column Heated Purification and elution Enhances dioxins elution speed Accelerate a chemical reaction User-friendly column design Unique way of flow switching without valves

13 Background --- Features of New System High performance clean-up User-friendly column design Clap! Easy connection Disposable parts Clap! No cross contamination No washing is required Clap!

14 Background --- Features of New System High performance clean-up 1 90 ml of hexane for eluting dioxins and PCBs: i. Trapping dioxins and NO-PCBs on carbon ii. Trapping MO and NDL-PCBs on alumina 2 Open the pinch valve 3 Elution PCBs with 1.5 ml of toluene GC vial 4 Close the pinch valve and open the other pinch valve 5 Elution Dioxins with 1,5 ml of toluene GC vial

15 First results Recovery in real samples Congener Avg Recovery (%) Stdev n= C 12 -TCDF 84,9 10, C 12 -PeCDF 87,6 12, C 12 -PeCDF 93,4 15, C 12 -HxCDF 82,8 10, C 12 -HxCDF 87,6 11, C 12 -HxCDF 83,3 12, C 12 -HxCDF 84,3 14, C 12 -HpCDF 82,6 12, C 12 -HpCDF 85,5 15,2 OCDF-13C 12 82,8 11,2 Sample type: PFAD Fish oil Mix of fatty acid Bergafat* Minerals Compound feed *Pretreatment with acidified silica is needed C 12 -TCDD 87,6 11, C 12 -PeCDD 90,7 13, C 12 -HxCDD 90,3 11, C 12 -HxCDD 77,5 11, C 12 -HxCDD 88,4 12, C 12 -HpCDD 83,6 13,3 OCDD- 13 C 12 87,1 16,3 PCB C12 79,2 12,6 PCB C12 79,4 14,2 PCB C12 90,5 14,2 PCB C12 90,1 15,6 PCB C12 92,9 14,0 PCB C12 89,8 11,0 PCB C12 87,5 10,7 PCB C12 85,5 8,7 PCB C12 84,4 11,4 PCB C12 84,6 13,1 PCB C12 79,6 15,9 PCB C12 82,7 14,4 PCB C 12 77,3 15,9 PCB C 12 80,2 11,6 PCB C 12 80,7 11,2 PCB C 12 79,6 12,9 PCB C 12 73,4 13,2 PCB C 12 76,9 14,0

16 First results PeCDD trace peak of interest is 1,2,3,7,8 *1 sample tocopherol Result after classical clean-up Result after clean-up using the new system *1 TEF = 1,0

17 How do they manage GC-HRMS Dual Acquisition GC 1 GC 2

18 How do they manage GC-HRMS Dual Acquisition GC 1 GC 1 GC 2

19 How do they manage GC-HRMS Dual Acquisition GC 1 GC 2

20 How do they manage GC-HRMS Dual Acquisition GC 2 GC 1

21 GC 2 Dual acquisition = 1.8 improvement of efficiency Every 66 minutes two samples GC 1

22 SP SYSTEMS Information : info@xxx.xxx or +31 xx-xxxxx

23 How did they start with GC-HRMS Dual Acquisition DFS1 Sequence file Fraction A MO and NDL PCBs GC 1 Sequence file fraction B NO-PCBs and PCDD/Fs GC 2 St PCB 1 St PCB 2 St PCB 3 St PCB 4 St PCB 5 St PCB 6 Solvent QA 1 fraction A Proc Blank Sample 1 Sample 2 ξ Sample 20 St PCB 3 QA 2 fraction A Proc Blank Sample 21 Sample 22 ξ Sample 40 ξ Sample 80 GC 1 GC 2 Total required time per instrument: =(((420/2)*66)/60)/2= 115 hrs St Dioxin 1 St Dioxin 2 St Dioxin 3 St Dioxin 4 St Dioxin 5 St Dioxin 6 Solvent QA 1 fracrion B Proc Blank Sample 1 Sample 2 ξ Sample 20 St Dioxin 3 QA 1 fracrion B Proc Blank Sample 21 Sample 22 ξ Sample 40 ξ sample 80

24 How did they start with GC-HRMS Dual Acquisition DFS 2 Sequence file Fraction A MO and NDL PCBs GC 1 St PCB 1 St PCB 2 St PCB 3 St PCB 4 St PCB 5 St PCB 6 Solvent QA 1 fraction A Proc Blank Sample 81 Sample 82 ξ Sample 100 St PCB 3 QA 2 fraction A Proc Blank ξ Sample 160 GC 1 GC 2 Total required time per instrument: =(((420/2)*66)/60)/2= 115 hrs Sequence file fraction B NO-PCBs and PCDD/Fs GC 2 St Dioxin 1 St Dioxin 2 St Dioxin 3 St Dioxin 4 St Dioxin 5 St Dioxin 6 Solvent QA 1 fracrion B Proc Blank Sample 1 Sample 2 ξ Sample 100 St Dioxin 3 QA 1 fracrion B Proc Blank ξ Sample 160

25 How do they manage nowadays GC-HRMS Dual Acquisition Sequence file fraction B NO-PCBs and PCDD/Fs GC 1 St Dioxin 1 St Dioxin 3 St Dioxin 5 Solvent QA 1 fracrion B Sample 1 Sample 4 ξ Sample 20 St Dioxin 3 Proc Blank ξ sample 200 DFS 1 Used for fraction B GC 1 GC 2 DFS 2 Used for fraction A Sequence file Fraction B NO-PCBs and PCDD/Fs GC 2 St Dioxin 2 St Dioxin 4 St Dioxin 6 Solvent Proc Blank Sample 2 Sample 3 ξ Sample 19 St Dioxin 5 QA 2 fraction B ξ Sample 199 MO and NDL PCBs GC 1 GC 1 GC 2 MO and NDL PCBs GC 2

26 Maintenance How do they manage GC-HRMS Dual Acquisition Every Monday liner and septum are replaced Every fortnight column and ion volume are replaced Once a year source is cleaned Once a year preventive maintenance by Thermo Average downtime less than 5%

27 Concluding remarks Combination of high performance clean-up and GC-HRMS with dual data acquisition is the ultimate solution Mid 2015 capacity will be increased to samples per year by: 10 channel automated clean-up system Third DFS instrument with dual acquisition or two triple quads will be purchased Same number of staff LVI under discussion In 2015 time will be invested for expanding the scope with new matrices (e.g. environment) and new analytes (e.g. flame retardants)

28 Thank you for your attention Questions?