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High sample throughput in a modern dioxin laboratory using dual acquisition
Information: www.dspsystems.eu
Wim Traag*1and Jeroen Markesteijn*2
*1 DSP-Systems, Erichemseweg 7, 4117GG Erichem The Netherlands *2 Nofalab, Jan van Galenstraat 41, 3115JG Schiedam, The Netherlands
Nofalab is founded in 2004
Core business of Nofalab
3
Edible oils and fats Nuts/sub-tropical fruits spices and grains Food and Feed safety Bio fuels Micro-biology
New laboratory opened April 2014 and extended in 2015
Lab manager Jeroen Markesteijn at the Thermo Scientific™ DFS™ high resolution
mass spectrometer
Two DFS high resolution mass spectrometers both equipped with dual
acquisition
Dioxin analysis at Nofalab How it all started (2008)
Before 2008 approximately 500-1000 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
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
Dioxin analysis at Nofalab
Total number of samples per year around 8000 80% 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
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 200 400 fractions On top at least 10 dioxins standards + 10 DL and NDL- PCB standards Total number of injections is 420 60 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
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
How do they manage ? The new of purification 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
Background --- Features of New System
Clap!
Clap!
Clap!
High performance clean-up User-friendly column design
• Easy connection
• Disposable parts
• No cross contamination
• No washing is required
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
④ Close the pinch valve and open the other pinch valve
⑤ Elution Dioxins with 1,5 ml of toluene
Background --- Features of New System
GC vial
GC vial
First results Recovery in real samples
Congener Avg Recovery (%) Stdevn=80
2378-13C12-TCDF 84,9 10,2
12378-13C12-PeCDF 87,6 12,2
23478-13C12-PeCDF 93,4 15,4
123478-13C12-HxCDF 82,8 10,7
123678-13C12-HxCDF 87,6 11,9
123789-13C12-HxCDF 83,3 12,6
234678-13C12-HxCDF 84,3 14,3
1234678-13C12-HpCDF 82,6 12,8
1234789-13C12-HpCDF 85,5 15,2OCDF-13C12 82,8 11,2
2378-13C12-TCDD 87,6 11,8
12378-13C12-PeCDD 90,7 13,0
123478-13C12-HxCDD 90,3 11,6
123678-13C12-HxCDD 77,5 11,5
123789-13C12-HxCDD 88,4 12,0
1234678-13C12-HpCDD 83,6 13,3
OCDD-13C12 87,1 16,3
PCB 77-13C12 79,2 12,6PCB 81-13C12 79,4 14,2PCB 126-13C12 90,5 14,2PCB 169-13C12 90,1 15,6
PCB 105-13C12 92,9 14,0PCB 114 13C12 89,8 11,0PCB 118-13C12 87,5 10,7PCB 123-13C12 85,5 8,7PCB 156-13C12 84,4 11,4PCB 157-13C12 84,6 13,1PCB 167-13C12 79,6 15,9PCB 189-13C12 82,7 14,4
PCB 28-13C12 77,3 15,9
PCB 52-13C12 80,2 11,6
PCB 101-13C12 80,7 11,2
PCB 153-13C12 79,6 12,9
PCB 138-13C12 73,4 13,2
PCB 180-13C12 76,9 14,0
Sample type: PFAD Fish oil Mix of fatty acid Bergafat* Minerals Compound feed *Pretreatment with acidified silica is needed
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
How do they manage GC-HRMS Dual Acquisition
GC 1 GC 2
How do they manage GC-HRMS Dual Acquisition
GC 1 GC 2
GC 1
How do they manage GC-HRMS Dual Acquisition
GC 1 GC 2
How do they manage GC-HRMS Dual Acquisition
GC 2
GC 1
GC 2
GC 1
Dual acquisition = 1.8 improvement of efficiency Every 66 minutes two samples
SP SYSTEMS Information : [email protected] or +31 xx-xxxxx
How did they start with GC-HRMS Dual Acquisition DFS1
GC 1 GC 2
Total required time per instrument: =(((420/2)*66)/60)/2= 115 hrs
Sequence file Fraction AMO and NDL PCBs
GC 1
St PCB 1St PCB 2St PCB 3St PCB 4St PCB 5St PCB 6Solvent
QA 1 fraction AProc BlankSample 1Sample 2
ξSample 20St PCB 3
QA 2 fraction AProc BlankSample 21Sample 22
ξSample 40
ξSample 80
Sequence file fraction BNO-PCBs and PCDD/Fs
GC 2
St Dioxin 1St Dioxin 2St Dioxin 3St Dioxin 4St Dioxin 5St Dioxin 6
SolventQA 1 fracrion B
Proc BlankSample 1Sample 2
ξSample 20St Dioxin 3
QA 1 fracrion BProc BlankSample 21Sample 22
ξSample 40
ξsample 80
How did they start with GC-HRMS Dual Acquisition DFS 2
GC 1 GC 2
Total required time per instrument: =(((420/2)*66)/60)/2= 115 hrs
Sequence file Fraction AMO and NDL PCBs
GC 1
St PCB 1St PCB 2St PCB 3St PCB 4St PCB 5St PCB 6Solvent
QA 1 fraction AProc BlankSample 81Sample 82
ξSample 100
St PCB 3QA 2 fraction A
Proc Blankξ
Sample 160
Sequence file fraction BNO-PCBs and PCDD/Fs
GC 2
St Dioxin 1St Dioxin 2St Dioxin 3St Dioxin 4St Dioxin 5St Dioxin 6
SolventQA 1 fracrion B
Proc BlankSample 1Sample 2
ξSample 100St Dioxin 3
QA 1 fracrion BProc Blank
ξSample 160
How do they manage nowadays GC-HRMS Dual Acquisition
GC 1 GC 2
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
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
MO and NDL PCBs GC 1
MO and NDL PCBs GC 2
How do they manage GC-HRMS Dual Acquisition
Maintenance • 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%
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 12.000 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)
