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Microencapsulacion de Cafe Verde Con MD y Leche Descremada
Microencapsulacion de Cafe Verde Con MD y Leche Descremada
Abstract
19.1% calculated from population aged of variables on the response formed (Montgomery,
15 years and above. The prevalence of obesity 2001). Therefore, this study aimed to deter-
is expected to increase according to age, mine the percentage of maltodextrin and
increase in population, diet, and lifestyle. optimal skim milk to produce dietary supple-
Obesity will cause several diseases such as ment preparations and to find out the quality
high blood pressure, coronary heart disease, of dietary supplement preparations obtained
diabetes, stroke, and cancer (Husnah, 2012). in form of microencapsulation.
Therefore, it is necessary to do research on
dietary supplements that produce high total
polyphenols and antioxidants with the addition
MATERIALS AND METHODS
of optimal fillers. Microencapsulation is one of The material used in this research is
important process to make bioactive component Robusta coffee beans from Argopuro, Jember,
more stable. East Java. Raw materials were obtained from
Method of microencapsulation can be Jember, harvested in July 2018 and processed
used to make herbal supplement. Spray drying by dry process and no pretreatment was carried
process with the addition of maltodextrin as out. The filling material used were maltodextrin
a coating material that will protect the extract and skim milk, and commercial green coffee
from high temperatures so that important supplement. The research was conducted at the
components in it are not damaged and skim Laboratory of Entrepreneurship and Bioindustry
milk as a protein material. Spray drying is a of Faculty of Agricultural Technology, Brawijaya
method used to convert liquid feed into University and the Laboratory of Pharmacy
powder (Dewi & Loekman, 2015). According Biology, Faculty of Science and Mathematics,
to Heldman et al. (1981), the advantages of Indonesian Islamic University.
the spray drying process are the relatively The research used response surface
fast drying cycles, the retention of the product method (RSM) in two factors that are the
in a short drying chamber, and the finished percentage of maltodextrin and the percentage
product that has been dried ready to be pack- of skim milk so that 13 experimental design
aged. Maltodextrine and skim milk are kind combinations were obtained. The response
of carrier material that will protect bioactive used in this study was total phenolic content
component from high temperature on spray and antioxidant activity. The results of opti-
drying process. mization in the Design Expert 7.1.5 Portable
The optimization method that can be used software were validated by extracting in
is the response surface method (RSM) with accordance with the optimal treatment results
central composite design (CCD). According from the prediction of the response surface
to Aritonang (2014), RSM is used for research then testing the total phenolic content and
that has complex processes and is widely used antioxidant activity.
in food technology research. The RSM method The level used for the percentage of
is able to explore correlations between many maltodextrin was 8.50 as the lower limit and
factors to get the most optimal production 9.50 as the upper limit, while for skim milk
conditions (Chang et al., 2006). In RSM, was 2.20 as the lower limit and 6.60 as the
CCD is used to build a polynomial model of upper limit so that 13 experimental design
a mathematical function of the independent combinations were obtained as in Table 1.
Coffee Powder Microencapsulation were then analyzed for total phenolic content
and antioxidant activity.
Green coffee beans were aerated at room
temperature for two hours to reduce water
content. Furthermore, the coffee beans were Total Phenolic Content (TPC)
grinded using a disk mill in stages and then
A response to optimization process of
sieved (40 mesh) to produce green coffee powder.
microencapsulation of green coffee was total
The ground coffee obtained were stored in plastic
phenolic content. Every samples was analyzed
containers at room temperature. The green
total phenolic content. The optimum treatment was
coffee powder that did not pass the sieve
analyzed of TPC and compared with commercial
was then grinded again using a blender.
green coffee supplement.
Green coffee powder was taken as much
Standard curves of chlorogenic were set
as 10 g and then macerated in 100 mL of
up by weighing chlorogenic acid powder as
distilled water for 24 hours at room tempera-
much as 0.01 g, then put into 100 mL volu-
ture (± 25OC) without stirring. The extraction
metric flask and added distilled water to mark
results were filtered with a paper filter and
the limit and homogenized to form 100 ppm.
stored in glass bottles in cold temperatures.
The solvent was diluted with concentrations
of 0 ppm, 20 ppm, 40 ppm, 60 ppm, 80 ppm
Coffee Extract Microencapsulation and 100 ppm. Each concentration was taken
0.5 mL and added 2.5 mL of 10% folin
100 mL of green coffee extract was reagent then homogenized and incubated
added with maltodextrin and skim milk using 5 minutes in the dark. After that, 2 mL of
several proportions according to the experi- 7.5% Na 2 CO 3 was added and incubated
mental design. The three ingredients was 30 minutes in the dark. Absorbance measure-
then mixed for 15 minutes for homogeni- ment using 765 nm wavelength was then
zation. The spray drying process was then plotted into a curve where X is the concen-
carried out with an inlet temperature of tration of gallic acid and Y is the absorbance
120OC, an outlet temperature of 60-80OC for so that the regression formula Y = aX + b is
30 minutes. The microcapsules produced obtained.
The solvent for analyzed was prepared incubated 30 minutes in the dark. Absor-
by encapsulation powder samples weighed bance measurements used wavelength of 517
as much as 0.01 g and dissolved in 10 mL of nm. DPPH uptake values before and after
distilled water. The solvent was taken 0.5 mL sample addition were calculated as percent
and put in a dark test tube. The solvent was inhibition (% inhibition) by the formula:
mixed with 2.5 mL of Folin C reagent 10% A control - A sample
distilled water and then homogenized and % Inhibition = x 100%
incubated 5 minutes in the dark and at room A sample
temperature. Then it was added with 2 mL
Then the results are entered into the linear
of Na2CO 3 solution, 7.5% distilled water,
regression equation Y = aX + b where Y is
homogeneous, and incubated 30 minutes in
the percent inhibition and X is the concen-
the dark. The blank used was 0.5 mL distilled
tration. The equation was used to determine
water added with 2.5 mL of 10% folin reagent
the LC50 value of each sample. The LC 50
and 2 mL of 7.5% sodium carbonate solution.
value was the half maximal inhibitory
Absorbance measurement used 765 nm
concentration.
wavelength. The amount of phenolic compounds
was measured based on gallic acid standard The chlorogenic acid sample test was
curves and expressed as mg chlorogenic carried out with LC-MS/MS equipment.
acid equivalent (CGAE/g extract). The levels of The column used was the Hypersil Gold
phenolic compounds in extracts were calculated specification (50 mm x 2.1 mm x 1.9 µm).
by the equation: UHPLC brand ACCELLA type 1250 made by
Thermo Scientific which consisted of a vacuum
c x fk x V
C= g degasser, quartener pump, thermostatic auto-
C = concentration of total phenolic content (mg CGAE/g) sampler controlled by a personal computer
c = concentration of chlorogenic acid (µg CGAE/mL) through the x-calibur 2.1 program. Solvent
V = volume of the extract solvent taken for analyzed (mL)
g = extract weights used for analyzed (g) A consisted of 0.1% formic acid in aquabidest,
fk = conversion factor solvent B consisted of 0.1% formic acid in
acetonitrile. A linear gradient with a velocity
Antioxidant Activity of 300 µL/min with the following mobile phase
The second response from optimization adjustments: a) 0–0.6 minutes 95% A; 0.6–
process was antioxidant activity. Analysis 3.0 minutes 75% B; 3.0–3.5 minutes 75% B;
of antioxidant activity was carried out by 3.5–4.0 minutes 75% B and 4.0-5.5 minutes
the DPPH method by means of 0.01 g of 95% A. The injection volume at LC is 2 µL.
microcapsule powder dissolved in 10 mL The column was controlled at 30OC, and the
of methanol to obtain a 1000 ppm solvent. autosampler compartment was set to 16OC.
The solvent was diluted at concentrations
of 60 ppm, 70 ppm, 80 ppm, 90 ppm and RESULTS AND DISCUSSION
100 ppm. Samples at each concentration
were taken 2 mL and put in a dark test tube. Response data of total phenol was in
Each test tube was added with 1 mL DPPH the range of 17.03-61.00 mg GAE/gr while
0.2 mM, homogenized, and incubated in the LC50 value response data was in the range
dark for 30 minutes. The control solvent of 62.69-100.08 ppm. The results of a cen-
was made by 1 mL DPPH 0.2 mM put into tralized composite design analysis can be
2 mL of methanol then homogenized and seen in Table 2.
effect. The graph also shows a linear model, (Siska & Wahyono, 2013). According to Al
in which total phenols will increased along Fakkar (2018), the combination of skim milk
with low concentrations of maltodextrin and and green coffee extract will produced total
skim milk. Based on these results, maltodextrin phenol, antioxidants, and high chlorogenic
will protect the material from nutrient released acid content which was useful as a dietary
due to high temperatures, but the higher the supplement.
percentage of maltodextrin and skim milk,
the lower the total phenol content. This was
Antioxidant Activity
due to the increasing number of total solids
contained in the material so that it can reduce Antioxidant activity value was carried
the intensity of the blue color in folin reagents out to find out how strong the antioxidant
6.60
Total phenolic content
Design port
61
17.0274
5.50
X1 = A: % maltodextrine
X2 = B: % skim milk
4.40
3.30
2.20
8.50 8.75 9.00 9.25 9.50
Figure 1. Contour plot response percentage of maltodextrin and percentage of skim milk to response
total phenolic content microencapsulation of green coffee extract
61
17.0274
X1 = A: % maltodextrine
X2 = B: % skim milk
6.60 9.50
5.50 9.25
4.40 9.00
3.30 8.75
2.20 8.50
Figure 2. Response surface curve percentage of maltodextrin and percentage of skim milk to response
total phenolic content microencapsulation of green coffee extract
activity was in the microencapsulation powder LC50 (Y2) which is influenced by the percentage
of green coffee extract produced. Antioxidant factor of maltodextrin (X1) and the percentage
activity can be seen from the LC50 value where of skim milk (X2) is as follows:
the smaller LC50 value, will make antioxidant Y1 = 71.55+8.44X 1+5.58X 2–1.52X 1X 2+6.68 X 12+
activity higher. Based on the data obtained 9 X22 …..................................................... (1)
it can be seen that the response of antioxidant Y1 = 2 0 5 5 . 1 0 - 4 5 8 . 2 4 X 1 - 1 . 3 8 0 6 X 2 -
activity had the lowest LC50 value of 62.68 1.3838X1X2+26.734X12+1.8604X22 ... (2)
at 8.5% maltodextrin percentage and 2.2%
skim milk percentage which means it had high In response surface optimization for LC50
antioxidant activity while the highest LC50 values, the most influential factor is the per-
value was 100.08 at percentage of malto-dex- centage of maltodextrin (X1) with a coefficient
trin 9% and percentage of skim milk 7.51% value of -458.24, which indicates that the
which means it had low antioxidant activity. percentage factor of maltodextrin gives an
The research data obtained indicate that the effect of -458.24 for every one point increase.
antioxidant activity will increase along with Next is the percentage factor of skim milk
the reduction in the composition of additional (X2) with a coefficient value of -1.3806 which
ingredients in green coffee extracts. The more shows that the percentage factor of skim milk
composition of maltodextrin and skim milk gives an effect of -1.3806 every increase of
were added, the lower the antioxidant activity one point. The contour plot of the percentage
as indicated by the higher LC50 value. factor of maltodextrin and percentage of skim
milk to the LC50 value of microencapsulated
These results were linier with the research
green coffee extract can be seen in Figure 3.
of Yuliawaty & Wahono (2015), the addition of
higher concentrations of maltodextrin cause Based on Figure 3, it shows that the
a decrease in levels of antioxidant activity. higher the LC50 value means that antioxidant
This was presumed by the increasing number activity is lower. Conversely, the lower LC50
of total solids contained in the material, namely value means that antioxidant activity is
maltodextrin as a filler so that the measured higher. In addition, in the graph there are
antioxidant activity was reduced, so that with also different colors where the redder the
increasing total solids in an ingredient, the antioxidant activity the smaller and the darker
measured antioxidant activity levels will be blue the color shown, the higher the anti-
smaller. In addition, it was also thought to be oxidant activity.
caused by changes in antioxidant compounds The contour plot of the total phenolic
due to the heating process, namely vitamin content response was different from the plot
C and other oxidized phenol compounds. It contour of the LC50 value response. The dif-
was possible that warming causes the phenol ference was seen from the contour color
compound to decompose so that its ability where the expected total phenolic content
as an antioxidant had decreased. plot response contour was red, the highest
The results of data processing using RSM total phenol content. In contrast, the contour
show that the chosen model was quadratic. color of the expected LC50 response was blue,
The percentage factor of maltodextrin was which is the lowest LC50 value so that it
significant for the response but the percentage has high antioxidant activity. The surface
factor for skim milk was not significant for curve of the maltodextrin percentage response
the response. The polynomial equation for and the percentage of skim milk to the LC50
the quadratic model on the response value of value response is presented in Figure 4.
Based on these curves it can be seen that higher causes a decrease in the level of anti-
both factors affect the LC50 value, but the oxidant activity. More total solids are present
percentage of maltodextrin was more dominant in the material, namely maltodextrin as a filler
factor affecting the yield. The graph also and skim milk as a source of protein, which
shows a quadratic model, where it was causes measurably less antioxidant activity.
shown through optimum conditions at the The antioxidant content was also thought
peak then decreased based on the two factors to be affected by the heating process, namely
used. vitamin C and other oxidized phenol com-
The percentage of maltodextrin and the pounds. It was possible that warming causes
percentage of skim milk generally affect the the phenol compound to decompose so that
antioxidant activity produced. Increasing the its ability as an antioxidant had decreased
concentration of maltodextrin which was (Yuliawaty & Wahono, 2015).
6.60
5.50
B = % Skim milk
4.40
3.30
2.20
8.50 8.75 9.00 9.25 9.50
A = % maltodextrine
Figure 3. Contour plot response percentage of maltodextrin and percentage of skim milk to response
LC50 value microencapsulation of green coffee extract
100
90.5
81
71.5
62
6.60 9.50
100 9.25
4.40 9.00
3.30 8.75
B = % Skim milk A = % Maltodextrine
2.20 8.50
Figure 4. Response surface curve percentage of maltodextrin and percentage of skim milk to response
LC50 value microencapsulation of green coffee extract
Optimum Solution for the Response desirability value was the value of the objec-
tive optimization function that shows the
The study was conducted to determine
ability of the program to fulfill desires based
the optimal solution results from the opti-
on the final predetermined criteria whose
mization of the percentage of maltodextrin
values range from 0 to 1. The closer to 1
and the percentage of skim milk in the
the value of desirability shows the ability
microencapsulation process of green coffee
of the program to achieve the more perfect
extract by optimizing the total phenol and
optimization goals.
the antioxidant activity. Limitations of opti-
mization for responses and factors can be Based on Figure 5 it was shown that
seen in Table 3. Both responses were selected the value of desirability was 0.926. The
with maximum targets because the aim of more outgoing the smaller the desirability
the study was to obtain the highest total phenol value. The results of optimization carried
yield and antioxidant activity from several out produce desirability values that are in the
treatment variations. Based on the limita- red contour, the highest contour. This shows
tions in Table 3, the optimum solution results that the program can achieve near-perfect
obtained by expert design software 7.1.5 can optimization goals. Besides desirability, it was
be seen in Table 4. In addition to the optimal also shown by the response surface curve
solution results predicted by the program, of the optimization results of total phenolic
there is also an estimate of the lowest to content response and antioxidant activity
highest value of the responses presented in which can be seen in Figure 6.
Table 5. Through the table, the prediction The results of the calculation of green
value can be known for both responses. coffee microencapsulation powder samples
The results of the optimization of total can be seen in Table 6. The chlorogenic acid
phenolic content response and antioxidant content of green coffee extracts was 1.19%.
activity were also presented in the form of Chlorogenic acid percentage increase with
desirability which can be seen in Figure 5. increasing levels of caffeine. In the study
According to Nurmiah et al. (2013), the of Urakova et al. (2008), determination of
chlorogenic acid levels was carried out on is different from particles in microcapsules
unroasted coffee bean extracts (0.86%). oleoresin ginger pulp that there is a lot of
Determination of chlorogenic acid levels in adhesion between particles one with the
coffee beans is also done by Belay et al. other particles.
(2008), obtained chlorogenic acid levels of
0.33% and 0.23%.
Comparison with Other Products
The appearance of microencapsulation
of green coffee extract indicates a rift on Microencapsulation products that have
the surface of the microcapsule caused by been produced were then compared with
high temperature. This embezzement can be similar products on the market. It aims to
caused by high temperature spray drying. determine the quality and position of the
This can lead to the loss of volatile compo- products produced with products that were
nents from within the microcapsules already known in the market. The parameters
(Reineccius, 1988). Microcapsule particles compared were total phenolic content, anti-
in the control tend not to stick between the oxidant activity, and solubility. The results
particles one with the others. This condition of the comparison can be seen in Table 7.
0 5.50
X1 = A: % maltodextrine
X2 = B: % skim milk
4.40
3.30
2.20
8.50 8.75 9.00 9.25 9.50
Figure 5. Desirability results of optimization of total phenolic content and antioxidant activity response
6.60 9.50
5.50 9.25
4.40 9.00
3.30 8.75
B = % Skim milk 2.20 8.50 A = % Maltodextrine
Figure 6. Response surface curve rsults optimization response of total phenolic content and antioxidant
activity
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