environmental analysis i. solid phase extraction step-by-step method development
TRANSCRIPT
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ENVIRONMENTALENVIRONMENTALANALYSISANALYSISI. Solid Phase ExtractionI. Solid Phase Extraction
ENVIRONMENTALENVIRONMENTALANALYSISANALYSISI. Solid Phase ExtractionI. Solid Phase Extraction
step-by-step
method development
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Goal of Six-Step ModeGoal of Six-Step ModeGoal of Six-Step ModeGoal of Six-Step Mode
Isolation
Purification
Trace enrichment
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Six-Step Method DevelopmentSix-Step Method DevelopmentSix-Step Method DevelopmentSix-Step Method Development
Compile known parameters
Tech Support Form
Follow step-by-step guide
Fill in method development form
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Technical Support FormTechnical Support FormTechnical Support FormTechnical Support Form
Application support request form
Name:________________________________________________________Company/Inst._______________________________________________
__Address:_______________________________________________________________________________________________________________________________________________________________________________________________________________Postal/Zipcode:_________________Phone:_________________________
ext:___________________________
Fax:_________________________________________________________
In order to provide a solution to your SPE application problem wewouldappreciate you taking the time to complete as much as possible of the twosided application request form. Our past experience in SPE consultingworkhas clearly indicated that the chances of a successful conclusion increase inline with the amount of informationsupplied!If for reasons of confidentiality you are unable to disclose the structuresofthe compounds to be extracted, a representative ofthe
Consultancy Divisionof IST would be willing to sign a suitable non-disclosure agreement inorderto progress with solving your SPE problem. Please contact yourISTDistributor for furtherinformation.
1 What is/are the compounds to be extracted?
_____________________________________________________________What are the Merck Index (12th edn.) reference numbers of the
analytes(s)(if any)?
_____________________________________________________________
Compound Structure(s)
Customer ContactInformation
Please fax or mail a photocopy of thisApplication Support Request Form toyour IST Distributor using the contactinformation on the back cover ofthecatalogue.
The Analyte(s)
13
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Pertinent DataPertinent DataPertinent DataPertinent Data
The analyte(s)
The matrix
The analytical method
Existing method(s)
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The AnalyteThe AnalyteThe AnalyteThe Analyte
Structure pKa(s) Concentration Sample volume Solubility Stability
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The MatrixThe MatrixThe MatrixThe Matrix
Type of matrix
pH and ionic strength
Interferences
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The Analytical MethodThe Analytical MethodThe Analytical MethodThe Analytical Method
Final technique
Compatible solvents
HPLC conditions
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Existing MethodExisting MethodExisting MethodExisting Method
Liquid-liquid method
Current SPE method details
Data from current method
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Method Development ExampleMethod Development ExampleMethod Development ExampleMethod Development Example
Pollution Unlimited1224 Sunnyside DriveElution, Alaska
(907) 663-3217 573(907) 663-3218
Dr. Anna Light
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The AnalyteThe AnalyteThe AnalyteThe Analyte
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The Analyte (cont.)The Analyte (cont.)The Analyte (cont.)The Analyte (cont.)
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The MatrixThe MatrixThe MatrixThe Matrix
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The Analytical MethodThe Analytical MethodThe Analytical MethodThe Analytical Method
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Other InformationOther InformationOther InformationOther Information
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Following the GuideFollowing the GuideFollowing the GuideFollowing the Guide
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The “Form”The “Form”The “Form”The “Form”Sample name _________________
Analyte of Interest ________________
Sample size ____________________
Sorbent Bed Mass _______ Cartridge volume_____
Sorbent phases to try 1) _____ 2) _____ 3) _____ 4) _____
1. Sample pretreatment ___________________________
2. Condition column with ____ mL of _________ at ___ mL/min
3. Equilibrate column with ____ mL of _________ at ___ mL/min.
4. Load sample at ______ mL per minute.
5. Remove interference with ____ mL of _________ at ___ L/min.
Drying step _____ minutes
6. Elute analyte with ____ mL of _________ at ___ mL/min.
Remember to include soak step if possible!
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Filling in the FormFilling in the FormFilling in the FormFilling in the Form
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Following the GuideFollowing the GuideFollowing the GuideFollowing the Guide
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Sample Size DeterminationSample Size DeterminationSample Size DeterminationSample Size Determination
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Filling in the FormFilling in the FormFilling in the FormFilling in the Form
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Sorbent CapacitySorbent CapacitySorbent CapacitySorbent Capacity
Hydrophobic phases: 1- 5% of Sorbent Mass
Ion Exchangers0.3 to 0.6 milli-equivalents per gram
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Following the GuideFollowing the GuideFollowing the GuideFollowing the Guide
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Select a MechanismSelect a MechanismSelect a MechanismSelect a Mechanism
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Select a MechanismSelect a MechanismSelect a MechanismSelect a Mechanism
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Select a MechanismSelect a MechanismSelect a MechanismSelect a Mechanism
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Select a MechanismSelect a MechanismSelect a MechanismSelect a Mechanism
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Following the GuideFollowing the GuideFollowing the GuideFollowing the Guide
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Selecting a SorbentSelecting a SorbentSelecting a SorbentSelecting a Sorbent
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Filling in the FormFilling in the FormFilling in the FormFilling in the Form
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Following the GuideFollowing the GuideFollowing the GuideFollowing the Guide
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A Reminder...A Reminder...A Reminder...A Reminder...
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Sample PretreatmentSample PretreatmentSample PretreatmentSample Pretreatment
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Filling in the FormFilling in the FormFilling in the FormFilling in the Form
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Following the GuideFollowing the GuideFollowing the GuideFollowing the Guide
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Conditioning and Conditioning and EquilibrationEquilibrationConditioning and Conditioning and EquilibrationEquilibration
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Conditioning and Conditioning and EquilibrationEquilibrationConditioning and Conditioning and EquilibrationEquilibration
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Filling in the FormFilling in the FormFilling in the FormFilling in the Form
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Following the GuideFollowing the GuideFollowing the GuideFollowing the Guide
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Sample Loading RateSample Loading RateSample Loading RateSample Loading Rate
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Filling in the FormFilling in the FormFilling in the FormFilling in the Form
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Following the GuideFollowing the GuideFollowing the GuideFollowing the Guide
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Removing InterferencesRemoving InterferencesRemoving InterferencesRemoving Interferences
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Removing InterferencesRemoving InterferencesRemoving InterferencesRemoving Interferences
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Filling in the FormFilling in the FormFilling in the FormFilling in the Form
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Following the GuideFollowing the GuideFollowing the GuideFollowing the Guide
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Drying TimeDrying TimeDrying TimeDrying Time
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Filling in the FormFilling in the FormFilling in the FormFilling in the Form
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Following the GuideFollowing the GuideFollowing the GuideFollowing the Guide
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Selecting an Elution SolventSelecting an Elution SolventSelecting an Elution SolventSelecting an Elution Solvent
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Elution Solvent VolumeElution Solvent VolumeElution Solvent VolumeElution Solvent Volume
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The Completed FormThe Completed FormThe Completed FormThe Completed Form
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What if Low Recovery?What if Low Recovery?What if Low Recovery?What if Low Recovery?
Losses during rinse step
Analyte breakthrough
Poor elution
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Losses During Losses During Rinse StepRinse StepLosses During Losses During Rinse StepRinse Step
Check rinse for presence of
analyte
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Analyte BreakthroughAnalyte BreakthroughAnalyte BreakthroughAnalyte Breakthrough
Stack Columns Elute Separately
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Analyte BreakthroughAnalyte BreakthroughAnalyte BreakthroughAnalyte Breakthrough
Check pH and ionic strength at
each step of extraction procedure
Select phase offering greater
interaction
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Impact of pHImpact of pHImpact of pHImpact of pH
Analyte loaded at pH=2
Analyte loaded at pH=7
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Selection of Bonded PhaseSelection of Bonded PhaseSelection of Bonded PhaseSelection of Bonded Phase
Analyte well retained on C8
Analyte poorly retained on C2
Analyte well retained on C18(EC)
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Poor ElutionPoor ElutionPoor ElutionPoor Elution
Select stronger elution solvent pH, ionic strength, % organics
Select less retentive sorbent
Include a soak step
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Solvent StrengthSolvent StrengthSolvent StrengthSolvent Strength
Elution with 20% methanol in water
Elution with 5% methanol in water
Elution with 100% methanol.
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Less Retentive SorbentLess Retentive SorbentLess Retentive SorbentLess Retentive Sorbent
Analyte completely eluted from C8
Traces of analyte remain on C18(EC)
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Soak StepSoak StepSoak StepSoak Step
The analyte is completely eluted from the column which was soaked for one minute with the elution solvent.
Some analyte remains on the column that was not soaked in the elution solvent.