A L O S Project Workshop IV .


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A L O S Project Workshop IV. S OLID- P HASE E XTRACTION. ALOS: ROSKILDE-MEETING November 2005. Outline. Principles of solid phase extraction Features and benefits Silica products and polymers Practice Applications. ALOS: ROSKILDE-MEETING November 2005. Principles
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A L O S Project Workshop IV S OLID-P HASE E XTRACTION

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ALOS: ROSKILDE-MEETING November 2005 Outline Principles of strong stage extraction Features and advantages Silica items and polymers Practice Applications

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ALOS: ROSKILDE-MEETING November 2005 Principles Why do test arrangement? Expel impedances from test More exact results Concentrating analytes to enhance location Protecting gear to lessened expenses

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ALOS: ROSKILDE-MEETING November 2005 Principles of SPE is an extraction procedure whereby a watery specimen is sifted through a thin bed of sorbent particles, the analytes of intrigue are expelled from the fluid grid, and concentrated onto the sorbent. Once thought, the analytes are expelled by an eluting dissolvable.

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ALOS: ROSKILDE-MEETING November 2005 Comparison of LLE versus SPE Disk LLE Uses 200 - 500 ml solvent Shaking/constant process Forms emulsions Little selectivity Takes 1 - 2 hours/sample SPE circle Uses 2 - 20 ml dissolvable Filtration handle No emulsions shaped Wide selectivity (adsorbent) Takes 10 - 20 min. /test

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ALOS: ROSKILDE-MEETING November 2005 Problems with the LLE Procedure Tedious and tedious Shaking and division time Evaporation time Expensive-work and materials Time calculate Solvent cost and presentation Solvent transfer Poor results Forming of emulsions Irreproducible extractions Low recuperations

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ALOS: ROSKILDE-MEETING November 2005 What are the Benefits of SPE? SPE utilizes less dissolvable than LLE SPE is speedier (no less than 5 times) High limit Total SPE expenses are extensively not exactly LLE High selectivity: wide decision of reinforced stages and solvents Automation much less demanding

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ALOS: ROSKILDE-MEETING November 2005 SPE Column

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ALOS: ROSKILDE-MEETING November 2005 SPE Column frill

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ALOS: ROSKILDE-MEETING November 2005 SPE-Experimental Set-up

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ALOS: ROSKILDE-MEETING November 2005 Silicagel-Phases Reversed Phase C 18 Adsorption Si-OH Normal Phase NH 2 CN C-OH(OH)

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ALOS: ROSKILDE-MEETING November 2005 Phases Anion Exchange N + NH 2 Cation Exchange C 6 H 5 - SO 3 H COOH SO 3 H Biochromatography WP PEI (NH 2 ) WP Butyl (C 4 ) WP CBX (COO) Sephadex G-25

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ALOS: ROSKILDE-MEETING November 2005 Interactions Non polar: van der Waals ~ 20 KJ/mole Polar: Dipole/Dipole ~ 40 KJ/mole Hydrogen bond ~ 40 KJ/mole Electrostatic: Ionic ~ 600 KJ/mole!

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ALOS: ROSKILDE-MEETING November 2005 Reversed Phase Principle

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ALOS: ROSKILDE-MEETING November 2005 Mixed Mode Principle

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ALOS: ROSKILDE-MEETING November 2005 Polymer-Phase Principle R (- CH-CH 2 ) n - N-CH 3 C=O CH 3 R

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ALOS: ROSKILDE-MEETING November 2005 Polymer-Phase Principle R (- CH-CH 2 ) n - N-CH 3 C=O CH 3 R SO 3 H or CH 2 N + R 3 SO 3 H or CH 2 N + R 3

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ALOS: ROSKILDE-MEETING November 2005 Practice

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ALOS: ROSKILDE-MEETING November 2005 4 Steps in SPE

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ALOS: ROSKILDE-MEETING November 2005 Conditioning of silica-based sorbents Add a natural dissolvable to flush and enact the alkyl-chains (C 18 , C 8 and so forth.)! Try not to give the segment a chance to run dry amid molding!

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of regular colors in drinks Sample Preparation: 1 mL blackberry-juice is disintegrated in 2 mL of refined water. Segment Conditioning: A 3 mL C18 (Baker: 7020-03) SPE cartridge is molded with 1 mL methanol took after by one section volume of refined water. Test Addition/Wash: The arranged specimen is suctioned through the section. A 5 mL refined water wash is used to evacuate sugars, sugar shading and natural acids. Elution: The dye(s) [anthocyanines, flavonoids, tannins or potentially alkaloids)] is (are) eluted with a column volume of methanol. Now and again propanol-2 will be more effective. Examination: For point by point investigation an assimilation range can be taken from the eluate. - TLC-analyses should be possible.

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of characteristic colors in refreshments: test stack

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of regular colors in drinks: test stack

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of common colors in drinks: washing step

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of normal colors in drinks: elution step

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of normal + manufactured colors in refreshments:

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of characteristic + engineered colors in drinks: test stack

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of normal + manufactured colors in drinks: elution step

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of regular + engineered colors in drinks

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ALOS: ROSKILDE-MEETING November 2005 Application Database Environmental Water, Soil Pharmaceutical/clinical Serum, plasma, pee, blood Food/encourage Juice, grain, drain Biological/biotech Water, plasma, pee

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ALOS: ROSKILDE-MEETING November 2005 Environmental - PAH \'s from water and soil - PCB\'s from oil- - Pesticides from water/soil- - and so forth. Nourishment/Feed/Beverages - Aflatoxine from corn dinner - Caffeine from di-charged eating regimen cola - Vitamin E from juice - and so on. Pharmaceutical/Clinical/Biological - Benzodiazipines from serum - Anabolic Steroids/Urine - Aflatoxine from liver - and so forth

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ALOS: ROSKILDE-MEETING November 2005 Thank you for your consideration

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of characteristic colors in refreshments Sample Preparation: 1 mL blackberry-juice is broken up in 2 mL of refined water. Section Conditioning: A 3 mL C18 (Baker: 7020-03) SPE cartridge is adapted with 1 mL methanol took after by one segment volume of refined water. Test Addition/Wash: The arranged example is suctioned through the segment. A 5 mL refined water wash is used to expel sugars, sugar shading and natural acids. Elution: The dye(s) [anthocyanines, flavonoids, tannins as well as alkaloids)] is (are) eluted with a column volume of methanol. Now and then propanol-2 will be more effective. Investigation: For itemized examination an assimilation range can be taken from the eluate. - TLC-trials should be possible.

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of normal colors in refreshments: test stack

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of characteristic colors in drinks: test stack

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of regular colors in refreshments: washing step

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of common colors in refreshments: elution step

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of common + engineered colors in drinks:

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of characteristic + manufactured colors in drinks: test stack

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of regular + engineered colors in drinks: elution step

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ALOS: ROSKILDE-MEETING November 2005 Experiment 1: Rapid Extraction of characteristic + engineered colors in refreshments

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ALOS: ROSKILDE-MEETING November 2005 Experiment 2: Rapid Extraction of iron-particles from water tests or waste water Sample Preparation: Dissolve 100 mg Fe(NO 3 ) 3 or FeCl 3 in 10 mL of refined water or utilize a measure of approximately 100mL waste water, which contains press (III) particles. Segment Conditioning: A 3 mL sulfonic corrosive (Baker: 7090-03) SPE segment is molded with 2 mL methanol followed by one section volume of refined water. Test Addition/Wash: 2 mL of the specimen is suctioned through the segment. The section is washed with 2 mL of refined water. Elution: Fe 3+ - particles are eluted in 1-2 mL hydrochlorid corrosive (c=0,1 M). The eluate is shaded yellow . Examination: For definite investigation - add NH 4 SCN to the eluate. The shading changes to dark red.

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ALOS: ROSKILDE-MEETING November 2005 Experiment 2: Rapid Extraction of iron-particles from water tests or waste water

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ALOS: ROSKILDE-MEETING November 2005 Experiment 2: Rapid Extraction of iron-particles from water tests or waste water

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ALOS: ROSKILDE-MEETING November 2005 Experiment 2: Rapid Extraction of iron-particles from water tests or waste water

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ALOS: ROSKILDE-MEETING November 2005 Experiment 2: Rapid Extraction of iron-particles from water tests or waste water

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ALOS: ROSKILDE-MEETING November 2005 Experiment 3: Rapid Extraction of sugars (glucose) Sample Preparation: Dissolve 100 mg glucose in 10 mL water. Segment Conditioning: A 3 mL Amino (Baker: 7088-03) SPE segment is adapted with 2 mL ethanol. Test Addition/Wash: 2 mL of the readied test is suctioned through the section. Elution: Sugar is eluted with 2 mL water. Investigation: For nitty gritty examination - utilize few drops of Fehling-arrangements. For itemized examination - an ingestion range can be taken from the eluate. -TLC-trials should be possible.

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ALOS: ROSKILDE-MEETING November 2005 Experiment 4: Rapid Extraction of ß-carotine from Multivitamine-juice or carot-juice Sample Preparation: 5 mL of Multivitamine-juice or carot-juice is separated or centrifuged. Section Conditioning: A 3 mL C18 (Baker

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