2 nd International Conference on chemical Process and Product Engineering

(ICCPPE) 2019
Semarang, September 25-26, 2019

ULTRASONIC EXTRACTION OPTIMIZATION (ULTRASOUND-ASSISTED

EXTRACTION) SAPONIN FROM LERAK (SAPINDUS RARAK DC) USING
THE RESPONSE SURFACE METHODOLOGY (RSM)
Dyah Rosita Heny, Nita aryanti*

Chemical Engineering Department, Faculty of Engineering,

Diponegoro University, Semarang, Indonesia

*Corresponding Address: nita.aryanti@che.undip.ac.id

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 Outline
Introduction

Objective

Method

Results and Discussion

Conclusion

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 What is the Saponin Lerak ?

Lerak belongs to the family of Sapindaceae . In Java,This plant

has a Lerak name. In this piece of flesh contains saponins
compounds that are quite strong poison (Sugianto,1984).
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 Introduction - 1
Sapindus rarak DC

Centrifuge
Dried, Peeled

Ultrasonic-Assisted
Extraction SAPONIN
with controlled temperature, Analysis and
time and wavelength Kinetic Study
Grinded to powder

Saponin of Lerak ultrasound-Assisted Extaction

Sapindus often called the fruit of the Lerak, containing
saponins about 38% (Burkil,1966), in addition to containing
strong toxins, Lerak fruit also contains a type of oil that is not
easy to dry that is about 26% consisting of glycerides, acids
Palmitate and stearic acid (Biecher,1960).
(UAE)
• Saponin forms a colloidal solution in water and
forms a steady foam if shaken and not lost with the
addition of acids (Harbrone, 1996). Saponin active
compounds strong surface and cause foam when
shaken with water. Some saponins work as anti-
microbial.

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 Introduction - 2
The dry fruits of the Sapindus are milled
and filtered through a 80-sieve mesh to
obtain a homogeneous fine powder

Phytochemical Analysis of Saponins:

a. Saponin inspection
Lerak Extrac then added several Liberman Bouchardat (LB) reagents. If formed b. Test the color
brown or violet rings then indicates the presence of Triterpene saponins, while the green or
c. FTIR
blue color indicates the presence of steroidal saponins (Pratama, et al., 2012)

In this study used ultrasound-Assisted

Central composite Extraction (UAE)
Design (CCD)

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 Objective

In this study used Central composite Design (CCD)

Three factors, to see the optimum condition of
treatment effect (the ratio of the lerak to the
ethanol solvent, the concentration of ethanol,
extraction time) to the yield.

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 Materials and methods - 1
• Saponin was isolated from Sapindus rarak using ultrasound-Assisted Extraction
(UAE) Wu et.,al, 2001
• Ethanol (96%) Merck
• Standard saponins (Sigma Aldrich).
• Liberman Bouchardat (LB) reagents
• Chloroform, Merck

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Drying temperature: 50oC (Roy et al., 1997) Drying time: 120 minutes (Roy et al., 1997) Powder Size: 80 mesh (Sarvin et al., 2018) Extraction pressure: 1 atm Temperature: 40 oC Ex

Materials and methods - 2

Control variable Independent variable
• Dryng temperature : 50 C • Dissolved: Solvent Ratio(X1)= 1:5, 1:10,1:15,1:20
• Concentration of Ethanol (X2)= 90%;80% 70 %; 60%;50%
• Dryng Time : 120 C • Extraction Time (X3) = 10,15,20,25, 30 minute
• Powder size : 80 mesh
• Extraction Pressure : 1 atm
• ExtractionTemperature : 40 C Dependent variable
• Extraction method : UAE • Yield

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 Central composite Design (CCD)
Variabel Level limits
-1 0 +1
Ratio lerak : etanol 1: 15 1 : 20 1: 25
,X1 (gg-1)
Solvent 70 % 80 % 90 %
concentrastion
etanol, X2( %)
Extraction Time 15 20 25
(menit)

Tabel 1. central composite Design Variabel

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 Equation
• At this stage there will be a mathematical equation with the
second order polynomial model which is the following
quadratic functions:
•
• Y = β0 + β1X1+ β2X2+ β3X3+ β11X12+ β22X22+ β33X32+ β12X1X2+
β13X1X3+ β23X2X3 ……...(2)

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 Results and discussion - 1
Solvent

Run
concentrastion etano,l
X2
Ratio lerak : ethanol,
X1
Extraction Time
X3 Yield
Y = 44.48380 + 4.31743X1-9.04776X2+4.42095X3-
1 70 (-1) 15 (-1) 15 (-1) 10.6798 5.37434X12+5.149537X22-8.72956X32+ 0.11317X1X2+ 3.51067
2 70 (-1) 15 (-1) 25 (+1)
115.7198 X1X3+ 1.05067 X2X3
3 70 (-1) 25 (+1) 15 (-1) 19.0098

4 70 (-1) 25 (+1) 25 (+1) 18.5198

5 90 (+1) 15 (-1) 15 (-1) 10.9698

6 90 (+1) 15 (-1) 25 (+1) 20.3198

7 90 (+1) 25 (+1) 15 (-1) 10.0198

8 90(+1) 25 (+1) 25 (+1) 33.31

9 63.18207 (-α) 20 (0) 20 (0) 10.2198

10 96.81793 (+α) 20 (0) 20 (0) 38.9198

11 80 (0) 11.59104 (-α) 20 (0) 23.8998

12 80 (0) 28.40896 (+α) 20 (0) 46.0198

13 80 (0) 20(0) 1111.59104 (-α) 15.6198

14 80 (0) 20(0) 28.40896 (+α) 35.3198

15(C) 80 (0) 20(0) 20 (0) 43.0098

16(C) 80 (0) 20(0) 20 (0) 44.0098

Tabel 2. Second order polynomial Table 3. Coefisien Equation

Model
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 Results and discussion - 2
• Figures 3A and 3B indicate that the greater the
concentration ratio of ethanol (X1) is used, the
yield gained is also increasing. At extraction
time less than 20 minutes, the yield of saponins
Lerak reaches 46.0198%. Thus, the extraction
time of less than 25 minutes of the saponins of
the bark contained in the material has been
completely extracted.
Figure. 3A. Plot Contour and 3B surface relation yield Lerak (Y1) with a
comparison of the concentration of ethanol (X1) with extraction time
(X3)

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 Results and discussion - 3

• In Figure 4A and 4B, it is noted that

increasing the volume of ethanol is not
able to increase the resulting yield of
saponins lerak.
• At the ratio of the Lerak with ethanol
1:25 GG-1, and the extraction time
varies, indicating that the extraction
less than 25 minutes, will be obtained
high yield saponins is 33.31%.
Figure 4A. Plot contour and 4B yield surface link Lerak (Y1) By
comparison of the ratio of the Lerak: Ethanol (X2) with extraction time
(X3)

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 Results and discussion - 4

• Characterization of saponins using the infrared

absorption functional group has been performed on
Lerak, Quilaja Saponaria (Almutairi and Ali, 2014),
Basellasaponin (Toshiyuki et al., 2001) and steroidal
saponins (DaSilva et al., 2002). Previous studies
reported that existence – OH, C-H, C = C, and C-O-C
were identified as saponins of Triterpenoid
Oleanane (Kareru et al., 2008).
Figure 5A. Plot Contour and 5B surface relationship
• Shows that the Lerak saponins used in this study Yield (Y1) with a comparison of the concentration of
had compatibility with saponins from the standard ethanol (X1) Lerak ratio: ethanol (X2)
saponins. The molecular structure of the saponins
of the Rarak Sapindus is also provided by Morikawa
et al. (2009).

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 Surface tension test Compound Saponin Lerak
Fig. 7. obtained the surface voltage measurement of the A1
extract, obtained equation of the line: y =-49.333 x + 48,829
and y =-0.5705 x + 24769 so that after calculating the results
obtained x = 2.11 Thus the value of CMC for the extract of
Lerak at 2% concentration.
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• CMC can occur with the addition of surfactants in
the solution will cause a decrease in the surface
tension of the solution. After achieving a certain
concentration, the surface tension will be constant
even though surfactant concentrations are
increased. When surfactants are added over this
concentration the Surfactants aggregate form the
Misel. The concentration of the formation of this
misel is called Critical Micelle Concentration (CMC).
The surface tension will decrease until CMC is
reached. Once the CMC is reached, the surface
tension will be constant indicating that the interface
becomes saturated and forms the misel that is in
balance.
 Conclusions
Factor Observed Min Critical values Observed
Maximum
conc. ethanol 63.18207 83.16278 96.81793
• The highest yield optimization of the extraction
experiment was obtained by 47.15952% with the ratio Ratio 11.59104 22.26180 28.40896
of the Lerak to ethanol 1:22.2618 GG-1, the lerak:ethanol
concentration of ethanol 83.162785 and the
extraction time of 21.92 minutes can be seen in table Extraction 11.59104 21.92890 28.40896
5 time
• The results of identification with UV-VIS Yield 47.17592
spectrophotometry have the absorbantion value of
saponins compounds of 4281.45 at a maximum
wavelength of 320. From isolates of identified Table 5. Extraction Experiment Optimization Results
saponins compounds containing the O-H, C-H, C=C, C-
O-c, -CHO, =CH, dan pironosa sugar.
• Lerak Saponins Extract has a saponins content that
has properties can lower the surface tension with the
CMC value at a concentration of 2.11%.
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