Preparation
and Structural Characterization of Kajjali
: An Ayurvedic formulation
ABSTRACT:
The present study deals with the preparation of Kajjali using equal proportions of mercury and sulphur. Prior to preparation, mercury and sulphur were purified according to procedure mentioned in
Ayurvedic literature. The final product, Kajjali, was analysed
for various parameters like Physical characterization, Elemental analysis by
Inductive Coupled Plasma (ICP), Energy Dispersive X-ray Analysis (EDAX),
Particle Size distribution and Determination of Particle shape by Particle size
analyzer. Some of the results obtained can be used for standardization of Kajjali.
KEYWORDS AND PHRASES: Kajjali, analysis, Inductive Coupled Plasma, Energy Dispersive
X-ray Analysis.
INTRODUCTION:
Ayurveda has its existence from prevedic
period. According to Yajurveda, God Rudra is an original preceptor of divine type of medicine.
The divine type of medicine may be divided in two divisions: First consists of
mantra, japa and yagya
while the second one consists of Rasa- special type of medicine1.
Rasashastra describes the use of metals, gems,
minerals and poisons to produce special formulations that combat acute
conditions or serious diseases. Rasa’s mainly comprises of metallic
ashes called bhasmas.
These bhasmas or lighter forms of metals are
contained in organo-metallic compounds that work as
carriers known as Yogavahi.
By this they make the drug available at the site of action very fast and also
act as catalyst so as to increase the bioavailability of herbs2, 3. Kajjali is used in many Ayurvedic
formulations as a bioavailability enhancer.
Kajjali is a powder preparation obtained by triturating
mercury with sulphur in different proportions. The
final product is said to be completely prepared when it complies with the tests
and observations described in Ayurvedic texts4, 5. The first test
confirms the small particle size of the drug. The second test confirms the
absence of free metallic mercury. These tests tell whether the formulation has
been prepared or not and do not give any information regarding composition and
structural properties. Only few reports are regarding the analysis and
structural characterization of Kajjali. Thus
it becomes necessary to characterize Kajjali
and intermediates obtained during the preparation. In the present work, Kajjali along with various intermediates obtained
during the preparation are characterized by using X-ray diffraction and
Particle size analyzer. According to the Ayurvedic medicinal system the
assimilation of a drug into the body fluid is a function of its particle size
of the drug. Hence, it is important to determine the particle size of Kajjali. Furthur
determination of particle size of the intermediates obtained during the
preparation would indicate how the particle size and shape changes during preparation.
EXPERIMENTAL:
Preparation
of Kajjali:
To prepare kajjali, raw mercury (RM) was triturated with an equal
quantity of garlic paste for 24 hours. After 24 hours the resultant mixture was
treated with water and mercury was separated out from the mixture (M-1)
Raw Sulphur (RS) was mixed
with ghee obtained from cow’s milk and heated till it just melted. The hot
mixture was poured into cold milk. On cooling the milk was filtered. The
residual sulphur cake was crushed to get a fine
powder (S-1).
The samples M-1 and S-1 were taken in equal
proportions, mixed together and triturated. Intermediate samples were taken
after every four hours and denoted with K-1, K-2 and K-3. After sixteen hours
of trituration it gives a fine black powder without
any luster was obtained. This product is Kajjali
(K-4).
Sample
details
|
Sample code |
Description |
|
RM |
Raw mercury |
|
RS |
Raw sulphur |
|
M-1 |
Mercury obtained after garlic paste treatment |
|
S-1 |
Sulphur obtained after ghee
treatment |
|
K-1 |
in process kajjali
after 4 hours trituration |
|
K-2 |
in process kajjali
after 8 hours trituration |
|
K-3 |
in process kajjali
after 12 hours trituration |
|
K-4 |
in process kajjali
after 16 hours trituration |
Analysis of
Raw materals, intermediates and final product:
Kajjali was prepared according to the method mentioned in the
ancient Ayurvedic text Rastrangini. RM, M-1 and K-4 were analysed by Inductive Coupled Plasma for detection of trace
metals. RS, S-1 and K-4 were analysed by EDAX to
determine the relative atomic percentages of the major and minor elements
JOEL-JSM-5200 Scanning Electron Microscope with energy dispersive X-ray
analysis.K-1, K-2, K-3 and K-4 were analysed by
Particle size analyzer and XRD for the determination of particle size and phase
composition respectively.
Inductive
coupled plasma:
Kajjali was digested with 10 ml HNO3 for 10 minutes
and then to it add 10 ml HCl and again heated for 10
minutes. It was then diluted with 20 ml double distilled water (DDW)
This solution was filtered and filter paper washed
thoroughly with water. The volume of the clear solution was made up to 100 ml
and stored in a tightly caped plastic bottle. The clear solution of Kajjali prepared was used directly for determination of
mineral elements.
Particle size
distribution:
Particle size distribution of K-1, K-2, K-3 and K-4
were determined using a particle size analyzer Fritsch particle sizer Analysette 22 model.
Powder XRD
studies:
All the samples were scanned on Rigaku-D-max
powder X-ray Diffractometer using Ni-filter, Cu k
α radiation (λ= 1.5406) and NaI scintillator. The samples were scanned in the 2 θ
range 20-1000 for a period of ten seconds in step scan mode. The phase
composition was determined using JCPDS library.
RESULTS AND DISCUSSIONS:
Presence of various elements present in RM and M-1 analysed by Inductive Coupled Plasma is shown in Table I.
RM shows the presence of Arsenic, Stannous and Ferrous in 26.9 ppm, 12.9 ppm and 1.6 ppm respectively. After purification of RM, M-1was obtained
and its analysis indicated reduction in concentration of arsenic while stannous
and ferrous were found below detectable limit (BDL).
The data of EDAX analysis of RS and S-1 is given in
Table II. RS shows the presence of arsenic which is removed by purification of
RS as it was not found in S-1.
The data obtained after elemental analysis of final
product Kajjali (K-4) by Inductive Coupled
Plasma and EDAX is given in Table III and Table IV. The results of ICP shows
that concentration of toxic elements like Arsenic, Stannous, Ferrous ,
Antimony, Bismuth and Lead was found to be below detection limit and the data of EDAX analysis of K-4 does not
show presence of arsenic as it was present in raw sulphur,
which shows the significance of purification steps of raw mercury and raw sulphur.
The particle size distribution of samples K-1, K-2, K-3
and K-4 is given in Fig 1(a), 1(b), 1c), 1(d) .The particle size distribution
for various samples is given in Table V. The data indicates the distribution of
particles over wide range of sizes ranging from 2.10 µm to 237.38 µm.
Sample K-1, K-2,K-3 and K-4 shows the particle size
distribution between 7.85 µm to 273.38 µm, 3.69 µm to 125.64 µm ,3.27 µm to
90.88 µm and 2.10 µm to 64.67 µm respectively. From these results it is very
clear that the particle size range of the final product was found to be narrow
indicating that maximum particles are of same size. This is the reason that Kajjali is used as Yogavahi in
many Rasa preparations.
Fig.2 (a), 2(b), 2(c), 2(d) gives the multiple plots of
the powder X-ray diffraction patterns of the Kajjali
samples. The sharp peaks in the powder for all the samples suggest the high crystallinity of the Kajjali
powders. The phase present in the samples determined by powder XRD are found to
be cubic in all the samples.
Various tests mentioned in the Ayurvedic literature to
check the formation of the Kajjali are
given in Table VI. These tests are well designed to confirm that mercury does
not remain in a metallic form in the sample and that the Kajjali
has a small particle size. These tests are unable to detect the presence of
other impurities in the Kajjali samples. These
tests were designed with the limitations of the analytical support in the olden
days. Today with the sophistication in the analytical techniques available, the
appropriate use of these techniques for characterization and standardization of
the Kajjali is required.
Table I: Percentage of various mineral elements
present in RM and PM
|
Elements |
Mean
concentration (Percentage
weight) In
RM |
Mean
concentration (Percentage
weight) In
PM |
|
As |
0.00269 |
0.00228 |
|
Sb |
BDL |
BDL |
|
Sn |
0.00129 |
BDL |
|
Bi |
BDL |
BDL |
|
Fe |
0.00016 |
BDL |
|
Pb |
BDL |
0.00001 |
BDL: Below Detection Limit
|
Sample ID Raw Sulphur (RS) |
|
Elements
|
Mean
concentration (Percentage
weight) |
|
As |
12.56 |
|
S |
87.44 |
|
TOTAL |
100 |
Table III: Percentage of various mineral elements
present in sample K-4
|
Sample
ID Kajjali Sample K-4 |
|
Element
|
Mean
concentration (Percentage
weight) |
|
As |
0.00239 |
|
Sb |
0.00001 |
|
Sn |
BDL |
|
Bi |
BDL |
|
Fe |
0.06371 |
|
Hg |
39.446 |
|
Pb |
BDL |
|
Sample
ID Kajjali Sample K-4 |
|
|
Elements |
Mean
concentration (Percentage
weight) |
|
C |
44.80 |
|
O |
5.59 |
|
S |
15.60 |
|
Hg |
34.01 |
|
TOTAL |
100 |
Table V:
particle size distribution of samples
|
Particle size less than (microns) |
||||
|
% of particle |
K-1 |
K-2 |
K-3 |
K-4 |
|
10 |
7.85 |
3.69 |
3.07 |
2.10 |
|
50 |
80.79 |
27.68 |
22.95 |
12.75 |
|
90 |
273.69 |
125.64 |
90.88 |
64.67 |
|
99 |
398.33 |
218.04 |
150.11 |
97.14 |
|
Test |
Observation
|
Evaluation
|
|
Nischandratva:Sample +
drop of water, rub on finger & see in sunlight |
No
brightness observed |
Absence
of free
metallic mercury |
|
Sample
+ lemon juice, rub on copper sheet |
Absence
of silver like coating |
Absence
of free metallic
mercury |
ACKNOWLEDGEMENT:
Authors are thankful to A.R. College of Pharmacy and
Sophisticated Instrumentation Centre For Applied
Research and Technology, V.V Nagar for providing research facilities.
REFERENCES:
1.
Anonymous, Atharvaveda, commentary by Vishva Bandhu, (Vishveshvaranand Vedic Research Institute, Hoshiarpur), 1960, 5/4/1, 1/12/3.
2.
Anonymous, Regveda, Commentary by Vishva Bandhu, (Vishveshvaranand Vedic Research Institute, Hoshiarpur), 1965, 10/97/17.
3.
Charaka, Charaka Samhita, Commentary by Shastri,
Kashinath, (Chaukhambha
Sanskrit academy, Varanasi), 1991, Sutra sthan, 1/24.
4.
Mishra, sidhinandan. Ayurvediya rasashastra,
Chaukambha orientalia,
Ninth edition, 1999, p. 92.
5.
Dr. K. Raghunanathan, Pharmacopoeial
Standards for Ayurvedic Formulations, Central Council for Research in
Indian Medicine and Homoeopathy, New Delhi, 1976, p. A -12
Received
on 13.12.2011
Modified on 20.12.2011
Accepted on 24.12.2011
© A&V Publication all right reserved
Research Journal of Pharmacognosy and Phytochemistry.
4(1): Jan. - Feb. 2012, 33-38