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What are food examples of hydrophilic substances?
Simple sugas, oligosaccharides, amino acids, some small proteins and peptides, some vitamins
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What are some food examples of hydrophobic substances?
fats, phospholipids, sterol, vitamins, carotenoids
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what are some examples of volatile food substances?
essential oils, LMW fatty acids, flavor compounds, pesticides
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what are some examples of food substances that are sensitive to acids and bases?
proteins, amino acids, color compounds
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What are some important considerations to include when doing sample prep?
- qualitative or quantitative
- quantity range of analyte
- size of sample material
- nature of impurities
- desired level of accuracy
- instrumentation required
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what are the primary goals of sample prep?
- remove interfering impurities
- selective enrichment of analyte
- increased [analyte]
- conversion of analyte into other forms for analysis (derivatization)
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what are the 6 steps of sample prep?
- 1. drying
- 2. grinding
- 3. solvent extraction
- 4. separation of extract from residue
- 5. cleanup
- 6. derivatization, concentration, etc.
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what is drying of the sample?
- remove water which is the main component of food matrices
- lyophilization (freeze drying), oven drying, vacuum oven drying
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what does separation of extract from residue include?
filtration, centrifugation, membrane separation (molecular sieve)
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what does sample cleanup include?
remove extracted impurities that can potentially interfere with further analysis
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what are some examples of solvent extraction?
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what is ASE/PSE/PFE?
- accelerated solvent extraction
- pressurized liquid extraction
- pressurized fluid extraction
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what is MAE?
microwave-assisted extraction
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what is UE?
ultrasonic extraction
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what is SPE?
solid-phase extraction
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what types of analytes can be lost to Soxhlet extraction?
thermally labile volatile analytes
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what is a pro of Soxhlet extraction?
minimizes the use of extraction solvent by circulation (continuous process)
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what is a con of Soxhlet extraction?
can be interference from contaminants from the extraction thimble used, so always need to do a blank extraction prior to actual
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what is accelerated solvent extraction?
- involves the use of pressurized liquids or pressurized fluids for extraction
- elevated temperatures and pressures are used in these techniques
- this allows the extraction solvents to penetrate the sample matrices, thus enhancing solvation of desired solute
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what is the most popular ASE technique?
super-critical CO2 extraction
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How is microwave-assisted extraction done?
- water in sample is heated by microwave
- the expansion of the heated water generated pressure from within the sample
- increased pressure disrupts sample matrix from the inside and allows analyte to escape and to be dissolved in extraction solvent
- requires less solvent compared to conventional extraction methods
- the solvent used may be microwave absorbing or non-microwave absorbing
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How is solid-phase extraction done?
- analytes suspended or dissolved in a liquid mixture are passed over a sorbent material, which selectively binds the solute of interest
- weakly bound impurities are washed out with a weak solvent and the desired analyte(s) are eluted with a strong solvent
- can be used as primary method or just for cleanup step
- several types of sorbent materials are available, depending on the physicochemical properties of the desired analyte (reversed phase, normal phase, ion exchange, affinity)
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how do you ensure you get just the desired analyte during a SPE process?
- condition the column
- load sample into column, some impurities leave immediately by not attaching to the solid phase
- wash the column, more weakly bound impurities leave
- selectively elute the desired sample, leaving behind the last of the impurities in the column
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how do molecular sieves work?
- membrane filtration techniques use specialized materials to achieve separation of particles or molecules based on their size
- the membrane is selectively permeable which allows preferential transport of matter through its pores
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