Proximate Analysis

What is proximate analysis?

It is a system of analysis that provides top level

results in analytical determinations of food
and feed component as moisture content,
protein , crude fat, crude fiber, ash, total lipids
and total sugars.
Moisture
 Moisture Content

Determination of moisture defines the dry

matter composition of food.
Determination of moisture content based on
physical removal of water
 Oven drying at 105 o

Applicable in most foods except those rich in

sugar and fat causes caramelization of sugars
and degradation of unsaturated fats.
Sample is heated in an oven at 105o for 5 hou rs.
Kjeldahl Method
Method used for protein determination
through total nitrogen.
Uses Selenium mixture as catalyst.
Adds Sodium thiosulphate in the
solution to prevent and break
ammonium and catalyst complex
Digestion with sulphuric acid

Oxidation of oxygen and hydrogen

into carbon dioxide and water.
Conversion of bound nitrogen into
ammonium ion.
Results in colorless solution.

Sample + H2SO4 (NH4)2SO4(aq) + CO2(g) +

SO2(g) + H2O(g)
Distillation with naoh
(NH4)2SO4 is distilled with NaOH
which is then converted to
ammonia. Consequently, the
generated gas is trapped in Boric
acid upon distillation.

(NH4)2SO4(aq) + 2NaOH Na2SO4(aq) +

2H2O(l) + 2NH3(g)

B(OH)3 + NH3 NH4+ + H2BO3

Titration with acid
The generated ammonium
ion is in equilibrium with
boric acid, thus titration with
acid (HCl) of the boric acid
gives the amount of total
nitrogen present in the
sample.

H2BO3 + H3O+ + B(OH)3(aq) + H2O

Crude Fat
 goldfisch method
Continuous solvent extraction method
Solvent continuously boils over sample held in
ceramic thimble.
Extracts lipids through non-polar solvents like
diethyl ether, hexane, petroleum ether or
methylene chloride
 Extraction times range from 4-16 hrs
Solvent is removed by evaporation
Fat content is measured by weight loss of the
sample or by weight of fat removed.
 Weende Method
Developed in 1884 by Hennenburg and
Stohman for determiation on crude
fiber.
Uses boiling sulphuric acid to to
separate fiber from other component
by hyrolyzing carbohydrates and other
protein components.
 Uses Sodium hydroxide as alkali
slution for saponifying remaining
lipids and dissolving remaining
minerals.
Sample is ignited at 600o to oxidize
fiber.
ASH
 Gives an index of total mineral content of
the sample
Can detect possible adulterations in the
sample such as soil, salt, dirt etc.
 Sample is ignited at 600o until white ash.
Ash content is determined through
difference in sample weight.
 Phenol-Sulphuric method
Sample is degraded by
sulphuric acid to furfural
Addition of phenol creates
a orange colored complex
 Color intensity is
related to sugar
content
Sugar content is
measured
spectrophotometrically
at 490nm.
Phosphorus
Ascorbic acid method

Requires full conversion of phosphorus

content to orthophosphate
Uses acidic medium for reaction to tae
place
 Ammonium-molybdate and antimony-
potassium tartrate reacts with
orthophosphate dilute solution to form
intense blue complex.
Complex not stable so must be read within
30 min upon addition of mixed reagent.
 Formed complex is proportional to the
Phosphorus content and thus
spectroscopic analysis at 880 nm gives
total phosphorus content.
Nesvita Cereal
Milk Drink
Experimental Results
 Moisture content

Weight of container + sample, g 25.6852 28.1863

Constant wt. of sample upon drying, g 25.614 28.1188
% moisture content 0.277 % 0.2394 %
Average moisture content, % 0. 2563 %
Literature value n/a
 ASh

Weight of container + sample, g 23.0186 26.4774

Constant wt. of sample upon ignition, g 22.7328 25.2412
% ash content 8.1202% 4.195%
Average ash content, % 6.1577%
Literature value 7.333%
 Crude Fat

Weight of sample, g 1.0077 1.0103

Constant wt. of goldfisch beaker, g 54.0026 63.7501
Constant wt. of sample upon analysis, g 54.0618 63.8053
% crude fiber content 5.875 % 5.464%
Average crude fiber content, % 5.669%
Literature value 7.667%
 Crude Fiber

Weight of sample, g 0.2980 0.2960

Constant wt. of sample before ignition, g 25.5280 17.6608
Constant wt. of sample after ignition, g 25.5186 17.6546
% crude fiber content 3.1543 % 2.0946 %
Average crude fiber content, % 2.584%
Literature value 6.333%
 Crude Protein

Weight of sample, g 0.1012 0.1009

Normality of HCl, N 0.1010 0.1010
Average Normality of HCl, N 0.1022
% Total N 2.373 % 2.554 %
% crude protein content 14.00 % 15.07 %
Average crude fiber content, % 14.53%
Literature value 12.oo%
 Total Sugars

Weight of sample, g 0.0515 0.0498

Absorbance reading at 490 nm (corrected) 0.026 0.032
Concentration of sample, mg/ml 57.4667 64.2570
Average Concentration of sample, mg/ml 60.8619
Literature value 66.67%
 Total Phosphorus

Weight of sample, g 1.1858 1.2900

Absorbance reading at 490 nm (corrected) 0.619 0.734
Concentration of sample, mg/100 g 16.129 18.186
Average Concentration of sample, mg/100 g 17.157
Literature value n/a
 Conclusion

The experimental value of the Nesvita Cereal

Milk drink is almost as close to the literature
value cited from the product.
Some errors
For moisture analysis- excess experimental
value could be attributed to formation of
milliard product (protein:carbohydrate
complex) which can be mistaken for moisture
loss.
 For ash- volatilization of some elements due to
hi temperature process

For fat- incomplete extraction may have made

 For protein slight difference may be due to
assumption that all nitrogen present is in the
form of protien.
 For fiber- acid and base solubilize some of the
true fiber (particularly hemicellulose, pectin
and lignin)
Cellulose too is partially lost. Hence, crude
fiber underestimates true fiber.
THE END