Original Article

Technological study of preparing gel from semi-solid

extract of Cacalia hastata L.
D. Jambaninj, Syed Azhar Syed
Sulaiman1, Syed Wasif Gillani1,
T. S. Davaasuren, G. Erdenetsetseg,
D. Dungerdorj
Department of Pharmacy Management
and Pharmaceutical Technology,
School of Pharmacy, Health Sciences,
University of Mongolia, 1Department
of Clinical Pharmacy, School of
Pharmaceutical Sciences,
Universiti Sains, Malaysia
J. Adv. Pharm. Tech. Res.
Abstract
Most of the drugs which are used for wound healing are imported in Mongolia. It is required
to develop drug formulation and increase local productions used for the treatment of wound
healing. For the purpose of solving the above problems, we aimed to prepare new drug
formulation from Cacalia hastata L. for the treatment of wound healing. Cacalia hastata L.
is a medicinal plant, member of the family Asteraceae. Cacalia hastata L. is widely used for
the Mongolian traditional medicine to treat wound healing, gastric ulcer, poisoning fever,
liver fever, bile fever, oral cavity, and gynecological diseases. We prepared Cacalia gel
from semi-solid extract of Cacalia hastata L. using various excipients such as gel former,
solvent, neutralizer, antimicrobial preservative, and humectant. Gel formulation was
standardized by such criteria, as the amount of biologically active compound, appearance
(color, smell), pH, viscosity, and bacterial contamination. Stability testing of gel formulation
was studied by long-term method. The quality of the Cacalia gel which was stored in room
temperature, its appearance, viscosity, and amount of biological active compound were
stable. The stability testing of the gel formulation from Cacalia hastata L. is continued.

Key words: Cacalia hastata L. carbomer (Carbopol 934), excipients, gel, semi-solid extract

INTRODUCTION Cacalia hastata L. is a medicinal plant of the family

Asteraceae. It grows in botanical and geographical
Nowadays, the vital problem of healthcare is to supply provinces such as Khangai, Khentii, Khuvsgul, and
population with highly effective medicine with no adverse Mongol Daguur in Mongolia.[2,3] Cacalia hastata L. has
reaction. The world attitude is focused on the use of pure pyrrolizidine alkaloids: Hastacine up to 0.1%, platyphylline;
natural, herbal and animal preparation rather than synthetic total carotenoids up to 310 mg%, organic acid up to 13%,
preparation.[1] ascorbic acid, polysaccharide, flavonoids, phenolic acid,
tannin, coumarin, and triterpenoids. [2-7] Hastacine is
Most of the drugs which are used for wound healing alkaloid similar to platyphylline for its structure and has
are imported in Mongolia. It is required to develop drug spasmolytic activity.[8] Flower and leaves of Cacalia hastata L.
formulation and increase local production of drugs used are widely used for the Mongolian traditional medicine to
for the treatment of wound healing. treat wound healing, gastric ulcer, poisoning fever, liver
fever, bile fever, oral cavity, and gynecological diseases.
Address for correspondence: It is also used to treat respiratory infection, cough, and
Dr. Syed Wasif Gillani, antihemorrhagic for the Tibetan medicine named “King of
Lecturer/Researcher, Department of Clinical Pharmacy,
hurt and break.”[3,4] Nowadays, extract of Cacalia hastata L.
School of Pharmaceutical Sciences, Universiti Sains Malaysia (USM),
Penang 11800, Malaysia. has been determined to have anti-inflammatory activity:
E-mail: wasifgillani@gmail.com Antibacterial, spasmolytic, antipyretic, gastroprotector, and
antihemorrhagic.[9,10]
Access this article online
Quick Response Code:
For the purpose of solving the above problems, we aimed
Website: to prepare new drug formulation from Cacalia hastata L. for
www.japtr.org the treatment of wound healing.

DOI: Carbomers are used in liquid or semisolid pharmaceutical

10.4103/2231-4040.93564 formulation as rheology modifiers. It includes creams, gels,
lotions, and ointments. In contrast, microorganisms grow

Journal of Advanced Pharmaceutical Technology & Research | Jan-Mar 2012 | Vol 3 | Issue 1 25
 Jambaninj, et al.: Technological study of preparing gel from semi-solid extract of Cacalia hastata L.
well in unpreserved aqueous dispersions, and therefore an
antimicrobial preservative such as 0.1% w/v chlorocresol,
0.18% w/v methylparaben - 0.02% propylparaben, or
0.1% w/v thimerosal should be added. The addition of
certain antimicrobials, such as benzalkonium chloride or
sodium benzoate, in high content rations (0.1% w/v), can
cause cloudiness and a reduction in viscosity of carbomer
dispersions. Carbomer aqueous gels are more viscous at
pH 6 to 11. The viscosity is considerably reduced at pH
values less than 3 or greater than 12, or in the presence of
strong electrolytes.[11]
Carboxymethyl cellulose sodium is widely used in oral and
topical pharmaceutical formulations, primarily for its viscosity-
increasing properties. Higher concentrations, usually 3% to 6%,
of medium-viscosity grade are used to produce gels; glycols
are often included in such gels to prevent them drying out.[11]
MATERIALS AND METHODS
Herb of Cacalia hastata L. was collected as a raw material
in Tuv Aimag province, Mongolia in July 2010 and was
identified by prof E. Ganbold, Sc.D in biology (voucher
number №00/28).
Methylparaben, propylparaben, and propylenglycol
were gift samples from Moncream Co. ltd, Ulaanbaatar,
Mongolia. Benzalkonium chloride was a gift sample from
Monchemo Co. ltd, Ulaanbaatar, Mongolia. Carbomer
(Carbopol 934P) and Sodium carboxymethyl cellulose were
bought (Thianjin Well-Real Chemical Technology Co. ltd,
China). All other chemicals were of analytical reagent grade.
The quantity of total alkaloids and total carotenoids are
determined by spectrophotometric, tannin by Lowenthal
permanganate titration method for standardization of gel
and semi-solid extract.
Determination of Total Carotenoids
Accurately weighed 1 g gel was dissolved in 50 ml of
water and shake well in 250 ml separation funnel. 50 ml
of hexane was added and separated two times. Hexane
solution was poured into 100 ml volumetric flask, diluted
with hexane to volume. Absorbance of the hexane solution
was determined at 450 nm. The total carotenoids content
(mg%) was calculated by the formula.
D×V×100×100×100
X=
2592×m
D is the absorbance of the solution, m is weight of gel, and
V is volume of solution. 2592 is specific absorbance E 1%
1cm
of
b- carotene in hexane, in 1 cm cuvette at 450 nm.[6]
Determination of Total Alkaloids
Accurately weighed 1 g gel was dissolved in 50 ml of
26 Journal of Advanced Pharmaceutical Technology & Research | Jan-Mar 2012 | Vol 3 | Issue 1
NH4OH and shake at well in 250 ml volumetric separation
funnel. 50 ml of chloroform was added and separated two
times. Evaporate the chloroform layer to dryness, add 2%
solution of hydrochloric acid then dissolve 50 ml methanol,
sonicate to dissolve and filter. Methanolic solution was
poured into 100 ml volumetric flask and diluted with
methanol to volume. Absorbance of the solution was
determined at 210 nm. The total alkaloids content (%) was
calculated by the formula.
D×V×100×100
X=
314.54×m
D is the absorbance of the solution, m is weight of gel,
and V is volume of solution. 314.54 is specific absorbance
of pyrrolizidine alkaloid presence of hastanecic acid in
methanol, in 1 cm cuvette at 210.3 nm.[7]
Determination of Tannins
Samples were analyzed by adding 1 ml sample and
5 ml indigo carmine to the 500 ml flask and adding
200 ml water. This is titrated against the Potassium
permanganate solution (N/40 or 0.005 M) until the royal
blue fades to a light green. Then, it is titrated drop-wise
until the lime green changes to yellow. This value is
record as X ml.
A blank titration using 5 ml of indigo carmine alone in
200 ml water should also be carried out. The blank value
should be 1 ml and should be recorded as Y ml.
Total Tannin (%) = (X–Y)×100 expressed as “tannic acid”
equivalents. 10
Preparation of Sodium Carboxymethyl Cellulose Gel
Bases
The sodium carboxymethyl cellulose gel bases were
prepared by dispersing the sodium carboxymethyl cellulose
of 6% and 10% w/w in half of total distilled water (20 ± 2°C).
The solution of humectant was prepared in the remaining
amount of water. The solution of humectants was added at
the end of dispersion stage. The pH value of gel bases was
measured using pH meter (Hanna 320, Germany) (n = 3).
Viscosity of gel bases was measured using Brookfield DV-III
Ultra programmable rheometer (Brookfield Engineering
Laboratories. Inc., USA) (n = 3).
Preparation of Carbomer gel Bases
We prepared various carbomer gel bases with different
ratio of gel former, antimicrobial preservative, neutralizer,
and humectant. At first stage, the solution of antimicrobial
preservative and neutralizer were prepared in half of
total water. At second stage, carbomer (1% or 2%) was
dispersed using mixer (Akira HM-202BSS) in the solution
of antimicrobial preservative and neutralizer. At third
 Jambaninj, et al.: Technological study of preparing gel from semi-solid extract of Cacalia hastata L.

stage, the humectants were added very slowly at the comparatively by its appearance (color, smell), pH,
dispersion stage. viscosity, and bacterial contamination.

Triethanolamine was used as a neutralizer and the pH
of the gel systems was adjusted by per cent of 1.1%,
1.15%, 1.2%, 1.25%, and 1.3% w/w. As a conserver
were used 0.18% methylparaben-0.02% propylparaben,
0.18% methylparaben, 0.02% propylparaben, and 0.01%
benzalkonium chloride. As a humectant were used
1% propylene glycol, 1% polyethylene glycol-400, and
10%glycerol. The pH value of gel bases was measured
using pH meter (Hanna 320, Germany) (n = 3). Viscosity
of gel bases was measured using Brookfield DV-III
Ultra programmable rheometer (Brookfield Engineering
Laboratories. Inc., USA) (n = 3).
Formulation of Cacalia Gel from Cacalia Hastata
Semi-solid Extract
Cacalia thick extract was added by 5% at the end of
the dispersion stage. The gels had specific smell, dark
brown to white brown color. The pH value of gels were
measured using pH meter (Hanna 320, Germany) (n = 3).
Viscosities of gels were measured using Brookfield DV-III
Ultra programmable rheometer (Brookfield Engineering
Laboratories. Inc., USA) (n = 3).
The quality of the gel formulation was investigated
Stability testing of gel formulation from Cacalia hastata L.
was studied by long-term method.
Bacterial and mould contamination was defined according
to MNS-5189-2002, MNS-5190-2002, MNS -5193-2002, and
MNS -5194-2002.[12-15]
Tests for significant differences between means were
performed by Student’s t-test or one-way ANOVA using the
software SPSS 16. Differences were considered significant
at P<0.05 and P<0.02 levels.
RESULTS
For choosing of appropriate gel former, gels were prepared
by 1% and 2% carbomer, 6% and 10% sodium carboxymethyl
cellulose. The result is shown in Table 1.
Gels with carbomer gel base were prepared with various
concentration triethanolamine and determined quality. The
result is shown in Table 2.
For the determination of the quality of gel dependence
on the antimicrobial preservative, we prepared gels using

Table 1: Quality of Cacalia gel with different concentration and various gel former
Gel former Quality criteria for gel formulation
Total Total carotenoids, pH Appearance (Specific Viscosity,
alkaloids, % mg% Mean±SD smell, dark brown color) (Pa × s)
Carbomer 1% 0.022 ± 0.012 12.5 ± 0.023 6.02 ± 0.045 + 70
Carbomer 2% 0.022 ± 0.012 12.5 ± 0.013 6.93 ± 0.067 + 138
Sodium carboxymethyl cellulose 6% 0.022 ± 0.011 12.5 ± 0.015 7.91 ± 0.077 + 12
Sodium carboxymethyl cellulose 10% 0.022 ± 0.013 12.5 ± 0.018 10.74 ± 0.059 + 25
+ Proper P<0.02 or the accuracy of the statistics 98%.

Table 2: Quality of Cacalia gel with different concentration triethanolamine

Neutralizer Quality criteria of gel formulation
Total Total carotenoids, pH Appearance Viscosity,
alkaloids,% mg% Mean±SD (Pa × s)
Triethanolamine 1.1% 0.012 ± 0.012 12.5 ± 0.023 5.79 ± 0.067 Specific smell, white brown color 50
Triethanolamine 1.15% 0.018 ± 0.012 12.3 ± 0.013 6.33 ± 0.045 Specific smell, white brown color 63
Triethanolamine 1.2% 0.022 ± 0.012 12.5 ± 0.015 7.02 ± 0.077 Specific smell, dark brown color 70
Triethanolamine 1.25% 0.020 ± 0.012 12.3 ± 0.018 7.13 ± 0.059 Specific smell, dark brown color 76
Triethanolamine 1.3% 0.0185 ± 0.012 12.0 ± 0.013 7.29 ± 0.077 Specific smell, dark brown color 85
P<0.05 or the accuracy of the statistics 95%.

Table 3: Microbial contamination of Cacalia gel with various antimicrobials

Antimicrobial preservatives
Methyl paraben-0.18% Methyl Propyl Benzalkonium
Propyl paraben-0.02% paraben-0.18% paraben-0.02% chloride-0.01%
Microbial contamination (not more than Not reported 0.1 × 102 1.1 × 102 3.1 × 102
1 × 104)
P<0.05 or the accuracy of the statistics 95%.

Journal of Advanced Pharmaceutical Technology & Research | Jan-Mar 2012 | Vol 3 | Issue 1 27
 Jambaninj, et al.: Technological study of preparing gel from semi-solid extract of Cacalia hastata L.

methylparaben-0.18%, propylparaben-0.02%, benzalkonium For preparing the semi-solid extract from leaves of Cacalia
chloride-0.01%, combined methylparaben-0.18%, and hastata L., it has been chosen by extraction method as a
propylparaben-0.02%. The result is shown in Table 3. percolation, as the solvents by 70% ethanol three times at
20 ± 2°C and by distilled water two times at 96 ± 2°C. 70%
Moisturizing effect of Cacalia gel was studied using ethanol 1:6 and distilled water 1:3 ratio was used as raw
various humectants such as propylene glycol, polyethylene material with solvents. After that, it was evaporated to
glycol-400, and glycerol. The result is shown in Table 4. have 25% of moisture by vacuum vapor. Thick extract from
Cacalia hastata L. has dark brown color, specific smell, and
Stability testing of gel formulation from Cacalia hastata L. bitter taste. It should have not less than 25% of moisture and
was studied by long-term method. The quality of the gel total alkaloids 0.36%, carotenoids 245 mg%, and tannins
was tested in each terms freshly prepared, after 2 weeks, 13.6%. Thick extract had no heavy metals and bacterial
30 days, 2 months, 3 months, and 4 months. The results are contamination.
shown in the Tables 5 and 6.
Cacalia gel was prepared with 5% semi-solid extract. Quantity
of total alkaloids and total carotenoids, the appearance
DISCUSSION
was not changed when using 1.2% triethanolamine when
pH = 7.02 ± 0.077, and, Cacalia gel containing 1% propylene
We prepared semi-solid extract by previous investigation.
glycol had good moisturizing effect and did not change
viscosity. These results were similar to the reference on the
Table 4: Quality of Cacalia gel with various Handbook of pharmaceutical excipients. [4] Furthermore,
humectant Cacalia gel base composition is similar to Indian researcher’s
Humectants gel composition. They prepared herbal gel containing
Propylene Polyethylene Glycerol Clerodendron infortunatum leaves extract with 1% carbomer,
glycol-1% glycol-400-1% 10% 0.2% methylparaben 0.1% propylparaben, 5% propylene
Moisturizing effect Good Average Bad glycol, and 1.2% triethanolamine.[16]
Viscosity, (Pa × s) 70 60 48
P<0.05 or the accuracy of the statistics 95%. The quality of the gel from Cacalia hastata L., which was
stored in room temperature, its appearance, viscosity, and
Table 5: Viscosity of Cacalia gel at various amount of biological active compound were comparative
storage condition (n = 3) stable. The stability testing of the gel formulation from
Date Viscosity (Pa × s) Cacalia hastata L. is continued.
Straight In room In
sunlight place temperature refrigerator CONCLUSION
(25°C ± (25°C ± (5°C ± 3°C)
2°C/60% 2°C/60% Appropriate composition of gel formulation for Cacalia
RH ± 5% RH) RH ± 5% RH) hastata L. was developed. The gel which used 1%
2011-04-27 70 70 70 carbomer as a gel former, 1.65% triethanolamine as a
2011-05-11 68 70 70 neutralizer, 0.18% methylparaben-0.02% propylparaben as
2011-05-25 67 70 69 an antimicrobial preservative, and 1% propylene glycol as a
2011-06-25 66 70 69 humectant completely satisfied the quality criteria. The gel
2011-07-25 65 70 67 of Cacalia hastata L., which was stored at room temperature
2011-08-25 50 70 56 (25°C ± 2°C/60% RH ± 5% RH), was stable.

Table 6: Amount of biological active compounds of Cacalia gel at various storage condition (n = 5)
Date Straight sunlight place In room temperature In refrigerator (5°C ± 3°C)
(25°C ± 2°C/60% RH ± 5% RH) (25°C ± 2°C/60% RH ± 5% RH)
Total Total carotenoids, Total Total carotenoids, Total Total carotenoids,
alkaloids,% mg% alkaloids,% mg% alkaloids,% mg%
2011-04-27 0.022 ± 0.01 12.5 ± 0.015 0.022 ± 0.01 12.5 ± 0.015 0.022 ± 0.01 12.5 ± 0.015
2011-05-11 0.022 ± 0.02 12.5 ± 0.013 0.022 ± 0.02 12.5 ± 0.015 0.02 ± 0.01 12.5 ± 0.015
2011-05-25 0.022 ± 0.03 12.5 ± 0.011 0.022 ± 0.01 12.5 ± 0.014 0.018 ± 0.02 11.5 ± 0.015
2011-06-25 0.022 ± 0.01 12.3 ± 0.012 0.021 ± 0.04 12.5 ± 0.015 0.015 ± 0.01 11.1 ± 0.015
2011-07-25 0.022 ± 0.01 12.1 ± 0.011 0.022 ± 0.01 12.5 ± 0.013 0.011 ± 0.03 10.3 ± 0.015
2011-08-25 0.021 ± 0.01 11.9 ± 0.011 0.022 ± 0.02 12.5 ± 0.012 0.008 ± 0.01 9.5 ± 0.015
P<0.05 or the accuracy of the statistics 95%

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 Jambaninj, et al.: Technological study of preparing gel from semi-solid extract of Cacalia hastata L.

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How to cite this article: Jambaninj D, Syed Sulaiman S, Gillani SW,
Davaasuren TS, Erdenetsetseg G, Dungerdorj D. Technological
study of preparing gel from semi-solid extract of Cacalia hastata
L.. J Adv Pharm Tech Res 2012;3:25-9.
Source of Support: Nil, Conflict of Interest: Nil.

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