STEP-BY-STEP PRODUCTION CONTROL "DRY EXTRACT TRIBULUS" FROM THE AERIAL PARTS OF Tribulus terrestris D.K. Mutalova, T.A. Khajibaev, R.M. Khalilov, Sh.Sh. Sagdullaev, R.G’. Axmadjonova S.Yu. Yunusov Institute of the Chemistry of Plant Substances Academy of sciences of the Republic of Uzbekistan st. Mirzo-Ulugbek, 77, 100170 Tashkent e-mail: noza-gold@mail.ru
We have developed a technology for obtainment and launched the serial production of
the substance "Dry extract Tribulus" with a content of furostanol saponins of at least 45%
in terms of protodioscin from the aerial part of
T. terrestris . The technology is as follows:
the aerial part of
T. terrestris is extracted six times with 70% ethanol at room temperature,
insisting for 8 hours. The combined and filtered extract is concentrated to a dry weight
content in the aqueous extract of 25%. The aqueous extract is treated three times with
chloroform and then twice with ethyl acetate. Furostanol saponins are extracted four times
from the purified aqueous extract with butanol. The butanol extract is thickened by
dissolving with water in a ratio of dry mass and water of 1.0 kg: 10.0 l. Then the aqueous
solution of saponins is concentrated to a dry residue content of 10%. An aqueous solution
of saponins is dried in a spray dryer at an inlet temperature of 170℃, an outlet of 90℃, a
solution feed rate of 70.0 l/h, and a spray head rotation speed of 7500 rpm.
To control the quality of the substance, appropriate methods were designed: the
authenticity of the substance was assessed using a qualitative reaction for saponins, the
identification of impurities was carried out by TLC, the quantitative determination was
carried out by spectrophotometry, and was developed for step-by-step control TLC and
spectrophotometry methods.
The results of the step-by-step control of furostanol saponins according to the above
technology are given in the table.
Table
Technology stages
Yield of total furostanol saponins, %
% by weight of
raw materials
% of the content in
raw materials
The aerial part of
Tribulus terrestris United extracts
Schroth
Chloroform extract
Ethyl acetate extract
Butanol extract
Residual solution
Spray dryer losses
Dry extract Tribulus
2,5
2,3
0,2
0,08
0,15
1,68
0,39
0,14
1,54
100,0
91,9
8,1
3,2
5,9
67,2
15,6
5,6
61,6
It was revealed that with the proposed technology, a large amount of furostanol
saponins remains in the residual solution after extraction with butanol. During spray
drying, the loss of the finished product is 10-12% of the loaded mass, which determines
the loss of furostanol saponins at this stage.