Using Solid Phase Extraction for Multi-Cartridge Extractions

and Extract Clean-up Procedures

Objective

•  Utilize the FMS 625/8270 Turbo Trace SPE system’s ability to perform automated multi-cartridge extractions for complex procedures

•  For single cartridge extractions, utilize the second cartridge loop to automate SPE formatted clean-up procedures in-line with SPE extractions.

Advantages

•  Reduced evaporation steps •  Reduced manual transfers of extract •  Simplified turn key procedures •  Greater reproducibility

FMS, Inc. 625/8270 Turbo Trace SPE

Touch Screen Control

SD Card for storing and Transferring Methods

Sample Size 2ml to Unlimited

Automatic Bottle Rinse

FMS, Inc. 625/8270 Turbo Trace SPE

Primary Cartridge

Secondary Cartridge

Automatic Liquid Level Sensor

Real Time Graphical Display of Extraction Steps

Positive Pressure Solvent/Sample Pump

FMS, Inc. SuperVap w/direct to GC vial

Extraction Configurations •  PCBs

–  DVB Cartridge –  NaSO4/Acidified Silica Gel clean-

up •  Organochlorine Pesticides

–  DVB Cartridge –  NaSO4/Florisil clean-up

•  Other –  Any organic inline with NaSO4

•  EPA 8270D –  Mixed CAX/DVB cartridge –  Coconut Charcoal cartridge

•  Organophosphorus/nitrogen pesticides –  C18 Cartridge –  Coconut Charcoal Cartridge

•  PAHs –  C18 Cartridge –  NaSO4/Silica Gel clean-up

Flow Diagram

Procedures •  Traditional Cartridge

Conditioning for Extraction –  Wet with Organic Solvent (MeCl,

EtAC, Hexane, etc) –  Dry –  Wet with MeOH –  Wet with H2O

§  Load Sample §  Dry Cartridge §  Elute Sample

•  Pre-wet clean-up Cartridge –  Wet with Organic Solvent

(Hexane, Hexane/Ether, DCM/Hexane, etc)

EPA 8270D •  Mixed bed Cartridge re-conditioned with

MeOH. •  Both cartridges conditioned with a 1%

NH3OH solution •  Cartridges independently dried with N2

for 1 minute each •  Mixed bed Cartridge eluted with

additional 30 mls DCM and collected as Fraction #2

•  Coconut charcoal eluted with 30 mls DCM and added to Fraction #2

•  Cartridges independently purged of residual solvent via N2 stream.

•  Cartridges wet with DCM & N2 Dried •  Cartridges conditioned with MeOH •  Cartridges conditioned with H2O •  Samples (ph=2) passed across both

cartridges at ~15mmHG •  Mixed bed cartridge partially dried with

N2 at 10 PSI •  Sample bottles sprayed with 20mls

DCM & loaded across mixed bed cartridge and collected as Fraction #1

•  Cartridge eluted with additional 10 mls DCM

•  Cartridges purged with N2 passing all DCM to collection vials.

Phosphorus/Nitrogen Pesticides

•  Cartridge eluted with additional 10 mls DCM

•  Cartridges purged with N2 passing all DCM to collection vials.

•  Coconut charcoal eluted with 20 mls DCM and added to Fraction

•  Cartridges independently purged of residual solvent via N2 stream.

•  Cartridges wet with DCM & N2 Dried •  Cartridges conditioned with MeOH •  Cartridges conditioned with H2O •  Samples (ph=2) passed across both

cartridges at ~15mmHG •  C18 cartridge partially dried with N2 at

10 PSI •  Sample bottles sprayed with 20mls

DCM & loaded across C18 cartridge and collected

PAHs •  Cartridge eluted with additional 5 mls

DCM •  Clean-up cartridge eluted with 15mls

DCM •  Fraction line purged with N2 passing all

DCM to collection vials.

•  Wet Clean-up cartridge with DCM •  Wet C18 cartridge with DCM and dry •  C18 Cartridge conditioned with MeOH •  C18 Cartridge conditioned with H2O •  Samples (ph=2) passed across both

cartridges at ~15mmHG •  C18 cartridge partially dried with N2 at

10 PSI •  Sample bottles sprayed with 20mls

DCM & loaded across C18 cartridge in-line with clean-up cartridge.

TeCDD, PCBs & PBDEs •  Cartridge eluted with additional 15mls

Hexane •  Clean-up cartridge eluted with 20mls

Hexane •  Fraction line purged with N2 passing all

Hexane to collection vials.

•  Wet Clean-up cartridge with Hexane •  Wet DVB cartridge with Hexane and dry •  DVB Cartridge conditioned with MeOH •  DVB Cartridge conditioned with H2O •  Samples (ph=2) passed across both

cartridges at ~15mmHG •  DVB cartridge dried with N2 at 10 PSI •  Sample bottles sprayed with 20mls

Hexane & loaded across DVB cartridge in-line with clean-up cartridge.

Organochlorine Pesticides •  Cartridge eluted with additional 15mls

Hexane •  Clean-up cartridge eluted with 20mls

Ether/Hexane •  Fraction line purged with N2 passing all

solvent to collection vials.

•  Wet Clean-up cartridge with Hexane •  Wet DVB cartridge with Hexane and dry •  DVB Cartridge conditioned with MeOH •  DVB Cartridge conditioned with H2O •  Samples (ph=2) passed across both

cartridges at ~15mmHG •  DVB cartridge partially dried with N2 at

10 PSI •  Sample bottles sprayed with 20mls

Hexane & loaded across DVB cartridge in-line with clean-up cartridge.

Analytical Platforms

•  Agilent 7890 w/µECD •  Thermo Trace GC, DSQ •  Thermo Trace GC w/PTV, Quantum TSQ

AB 8070 Results

OPP Results

PAH-Low Results

Analytes spiked at .05 µg/ml

PCDD/DFs Results

PBDE Results

OCP Results

Conclusions

•  Utilization of automation for multi-cartridge procedures streamlines multi-step extraction processes into a single process.

•  Eliminates extra evaporation steps, thus additional solvent consumption and reclamation.

•  Allows laboratory staff to perform other duties rather than attend manual SPE manifolds.

Acknowledgements

Questions?