CONCEPCION, Elaine F.

Chem 28 HW 2 #4

A. Continuous vs. semi-continuous vs. discontinuous solvent extraction

Continuous solvent extraction

- Solvent from a boiling flask continuously flows over the sample held in a ceramic thimble
- Fat content is measured by weight loss of sample or by weight of fat removed
- Gives faster, more efficient extraction than semi-continuous
- Though they may cause channeling that results in incomplete extraction
- Ex: Goldfish (standard method), Wiley, Underwriters

Semi-continuous

- Solvent builds up in the extraction chamber for 5-10 min and completely surrounds the sample, then siphons back to the boiling flask
- Fat content is measured by weight loss of the sample or by weight of fat removed
- Provides a soaking effect of the sample; does not cause channeling
- Though this requires more time than continuous
- Ex: Soxhlet (standard method)

Discontinuous

- Fat is extracted with a mixture of ethyl ether and petroleum ether in a Mojonnier flask, and the extracted fat is dried to a constant
weight and expressed as percent fat by weight
- Does not require removal of moisture from the sample
- Can be applied to both liquid and solid samples (applied primarily to dairy foods, but is applicable to other foods)
- Mejonnier (standard method)

Reference: Nielsen, S. S. Food Analysis, 5th ed.; Springer: USA, 2017; pp 303-313.

B. Matrix
 Cheese Milk (liquid) Milk (powder) Feeds Cereal
Method/s used;  Acid & alkaline hydrolysis  Extraction Same methods used Extraction of  Acid hydrolysis for
Principle for extraction of fat and with ethers for liquid milk crude fat with extraction of total
fatty acids; from known diethyl ether lipids;
 Addition of pyrogallic weight of by Randall  Extraction of
acid to minimize milk; modification hydrolyzed fat
oxidative degradation of  Ether extract of Soxhlet components into ethyl
fatty acids during is decanted method/ and petroleum ethers,
analysis; into pre- submersion then evaporated;
 Addition of triglyceride to weighed dry method  Saponification and
internal standard; weighing dish, methylation of
 Extraction of fat into then ether is extract;
ether, then methylation evaporated;  Determination of fatty
to fatty acid methyl  Drying of acid methyl esters by
esters (FAMEs); extracted fat capillary gas
 Quantitative to constant chromatography
measurement of FAMEs weight
using capillary gas
chromatography against
C11:0 std.
Fat expression  Total fat = sum of % fat by weight % fat by weight % crude fat,  Total fat = sum of
individual fatty acids ether individual fatty acids
expressed as triglyceride extraction expressed as
equivalents % crude fat, triglyceride
 Saturated & hexanes equivalents;
monounsaturated fats = extraction  Saturated,
sum of respective fatty unsaturated, &
acids monounsaturated fats
 Monounsaturated fat = sum of individual
includes only cis form fatty acids
Phase of sample for Dried and finely ground Liquid; Tempered Liquid: weighed then Dried and Dried and ground (cereal
preparation to 38 °C mixed with H2O and ground should only contain 0.5-
NH4OH; warmed/ 13% total fat)
heated then cooled