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B. Tech. (Dairy Technology) ► DT-2 ► Resources ► Lesson 31. FRACTIONATION OF MILK FAT
Lesson 31
FRACTIONATION OF MILK FAT
31.1 Introduction
The physical properties such as melting point and consistency of butter are depending on
chemical composition of the milk fat. The different triglycerides have different melting
points and can therefore easily divided into different fractions consists of different fatty
acids. When molten milk fat is slowly cooled, a crystalline solid and an uncrystallized liquid
phase are formed. Separation of these phases yields fractions with high and low softening
points respectively. Due to the fact that fat is composed of triglycerides of various
molecular weights with different physical properties, fractionation of milk fat into fractions
markedly different from one another in composition and physical properties is the most
logical basis of modification. Economic fractionation of milk fat into oil and hard fat
fractions will facilitate an increased utilization of milk fat in many food applications, such
as chocolate, confectionary and bakery products and in developing new convenient (e.g.
freeze spreadable) and dietetic (e.g. cholesterol reduced and short and medium chain
enriched triglycerides) butter types. Differences in molecular weight, melting temperatures
(molecular weight and entropy of fusion), volatility and intermolecular interaction energy
of constitutive triglycerides, can provide the physical basis for fractionation of milk fat
triglycerides. Fractional crystallization is most promising process to separate milk fat, a
laboratory method of fractional crystallization is explained in detail in following paragraph.
More than 400 fatty acids have been identified in milk fat and their melting point varies
from - 40°C to 40°C. This is due to variation in the composition of milk fat with season,
region, breed of cows and type of feed. Following tables gives the melting point of major
fatty acids of milk fat.
Table 31.2 Melting point characteristics of common fatty acids of milk fat
Another method which is widely used for crystallization is Solid layer melt crystallization.
This process has only recently been applied to fractionation of milk fat (4–6) although it is
widely used in the chemical processing industry. In layer crystallization processes, crystals
generally grow on the cooled surface of a specially designed multi-tube or plate heat
exchanger. The crystalline product is removed by re-melting crystals after draining the
residual melt.
On laboratory method is explained below, wherein milk fat was melted completely and
washed several times with warm water, dried under vacuum and filtered at 50-60°C.
500g sample was melted in a beaker which is kept in thermostat controlled water bath at
600C. Fat was stirred at about 100rpm. Then crystallization temperature was adjusted
from 25°C to 32°C at an interval of 1°C for six hours. After crystallization at one of these
temperatures fat was filtered on a Buchner funnel resulting in a liquid and a solid fraction
at each of the selected temperatures. Fatty acid composition was determined using gas-
liquid chromatographic determination.
The solid fraction (stearin) and the liquid fraction (olein) displayed a different
triacylglycerol (TG) composition. Stearin fraction was enriched in long-chain fatty acids,
whereas olein fraction was enriched in short-chain and unsaturated fatty acids.
Determinations of fatty acid composition by GLC showed that unsaturated and short chain
fatty acids were present in increased concentration in the liquid fraction (average 37·8 and
12·4% as compared with 32·1 and 10·8% in the original milk fat) and long chain saturated
acids in the solid fraction (average 57·8 as compared with 53·8%). There was some
concentration of carotene and vitamin A, and to a lesser extent of cholesterol, in the liquid
fraction
This process involves dissolving melted milk fat in a solvent prior to crystallization.
Solvents employed are generally acetone, ethanol, pentane or hexane. Melting temperature
used is similar to dry fractionation. Crystals separation is done by filtration. Fractions are
heated to remove the solvent. However, the costs incurred by solvent recovery, the
hazardous nature of the operation, and the process losses make this process less frequently
used than crystallization and filtration.
Isopropanol is used as solvent for fraction of milk fat. It should be added (4 mL/g butter
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oil), to butter oil. Mixture should keep at different temperature viz., 15, 20, 25 and 30°C
and stirred by a low-speed mechanical stirrer for 1 h. Then, solid part and liquid part were
separated by filtration under vacuum. The fractions were desolventized at 80°C for 1 h at
10 mm Hg pressure, weighed, and stored in a refrigerator.
Both the stearin fractions and the olein fractions show differences in the fatty acid
compositions as reported by Bhattacharyya et al., 2000 The stearin shows higher content
of short-chain acids and other saturated acids than the oleins.
The melting point of the stearin fraction at 15°C has increased from original butter oil by
4.1°C due to the increase in both palmitic acid (from 31.7 to 39.1%) and stearic acid (from
14.0 to 21.3%). On the other hand, in the olein fraction, palmitic acid and stearic acid have
both decreased from 31.7 to 24.7% and 14.0 to 12.6%, respectively, while oleic acid has
increased. The fatty acid compositions of the stearin and olein fractions obtained at 30°C
and also at 25°C from isopropanol closely matches with the pattern composition of fatty
acids of the corresponding fractions isolated by dry fractionation technique.
The SFC of the stearin fractions indicated significant values, viz. 62–67 at 10°C, 39–51 at
20°C, and 21–34 at 30°C. The stearin fractions obtained at 30, 25, and 20°C are all fairly
similar in properties. This suggests that the temperature of fractionation, between 30, 25,
and 20°C, does not lead to significant differences in physical characteristics.
The removal of cholesterol and fractionation of butteroil with supercritical fluids have been
reported. The use of co-solvents to improve the removal efficiency in the extraction of
cholesterol with supercritical CO2 have been evaluated. It has been reported that only 5%
of the cholesterol in the initial butter using supercritical extraction followed by adsorption
on silica gel.
In one study conducted by Torres et al.,( 2009), wherein butteroil is fractionated based on
the individual fatty acid types via countercurrent CO2 extraction at pressures ranging from
8.9 to 18.6 MPa and at 2 different temperatures (48 and 60°C). Using this methodology,
fractions as high as 70% of SCFA and MCFA ethyl esters were obtained. Figure 13.3
shows a flow diagram of the countercurrent supercritical fluid extraction system employed
in this study.
The countercurrent extraction column (316 stainless steel) is 100 cm × 12 mm i.d. and is
packed with Fenske rings (3 × 0.5 mm). The countercurrent supercritical fluid extraction
device also includes 2 separator cells (S1 and S2) of 270 mL capacity each (where a
cascade decompression takes place) and a cryogenic trap at atmospheric pressure. Both
CO2 and liquid feed sample were preheated at the exit of their respective pumps before
introduction into the extraction column. All units were equipped with electrical thermostats.
The device has computerized programmable logic controller-based instrumentation and a
control system with several safety devices including valves and alarms. During the
extraction, a continuous flow of CO2 was introduced into the column through the bottom.
When the operating pressure and temperature were reached, the liquid sample was
pumped (100 mL/h) from the top during the entire extraction time (60 min). The first
separator was maintained at 6 MPa and 20°C and the second separator cell was
maintained at low pressure and temperature (2 MPa and 10°C). The raffinate and liquid
fractions collected in the separators were weighted and analyzed. The material balance
closed in all experiments with an inaccuracy <7.4%.
solvent recovery
i. Can be used as shortening to provide crusty, flaky texture to croissants and pastries
iv. Hard fraction can improve the whipping properties of cream which is desirable in
ice cream manufacturing
DT-2