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Tariq et al., IJPSR, 2014; Vol. 5(1): 171-177.

E-ISSN: 0975-8232; P-ISSN: 2320-5148

IJPSR (2014), Vol. 5, Issue 1

(Research Article)

Received on 11 August, 2013; received in revised form, 11 September, 2013; accepted, 17 December, 2013; published 01 January, 2014

FORMULATION
AND
CHARACTERIZATION
FORMULATION: KUSHTA QALAI

OF

A

TRADITIONAL

UNANI

Mohd. Tariq*1, Khaleequr Rahman 1, Shahid Shah Chaudhary 1 and Shaikh Imtiyaz 2
Department of Ilmul Saidla (Pharmacy), National Institute of Unani Medicine 1, Bangalore 560091,
Karnataka, India
Department of Moalajat (Medicine), National Institute of Unani Medicine 2, Bangalore 560091, Karnataka,
India
Keywords:
Aspgol, Kushta, Qalai,
Standardization, Unani Medicine
Correspondence to Author:
Mohd Tariq (M.D.)
C-102, Third Floor, Street no. 3,
West Gorakh Park, Shahdara, Delhi110032 , India
E-mail:drtariqnium@gmail.com

ABSTRACT: Kushta literally means burning of drugs of metallic,
mineral or animal origin into their ash. Qalai (tin) based Unani compound
formulation Kushta qalai (KQ) is used since antiquity for the treatment of
various ailments. Although it is used on consistent basis by Hakims but at
present there are no scientific data available about its quality control
parameters. So, in this research article an emphasis is given on
preparation and physicochemical assessment of KQ using classical as
well as modern scientific parameters with an eye towards its
standardization. In finished product floating test, grain floating test,
thumb finger test and fineness test were positive. The mean value of bulk
density and tapped density were 1.32±0.00gm/ml and 2.24±0.02gm/ml
respectively. Hausner’s Ratio and Compressibility Index were 1.77±0.02
and 44.15±0.86% respectively. pH in 1% and 10% solution were
10.47±0.00 and 11.17±0.02 respectively. Loss of weight on drying was
0.019±0.00%. Total ash, acid insoluble ash, water soluble ash and water
insoluble ash were 96.47±0.07%, 36.87±0.06%, 5.1±0.10% and
91.64±0.20% respectively. The water soluble extractive value was
0.34±0.00%. The results obtained might be treated as standard for future
references.

INTRODUCTION: Kushta (organo-metallic
preparation) is the finest class of solid dosage
forms 1 used in Unani system of medicine obtained
by incineration of metals, minerals or animal origin
drugs with herbal extracts. These are administered
orally in minute quantity with appropriate vehicle
to make them biocompatible and are used for broad
range of therapeutics 2.
QUICK RESPONSE CODE
DOI:
10.13040/IJPSR.0975-8232.5(1).171-77

Article can be accessed online on:
www.ijpsr.com
DOI link: http://dx.doi.org/10.13040/IJPSR.0975-8232.5(1).171-77

They address different ailments depending upon
their method of preparation. Qalai (tin) is one of
the most popular metal renowned for its wide
spread applicability since Vedic period 3, It is used
internally in the form of kushta. It is known by
diverse vernacular names like rasas in Arabic, urziz
in Persian, rang in Hindi, vanga in Sanskrit and
kalai in Guajarati. It occurs as silver like metal,
softer than gold, harder than lead, malleable and
sparingly ductile with little elasticity 4. There are
two varieties of qalai viz. khuraka and mishraka,
only the former being acceptable for therapeutic
applications. Samples having the characteristics;
bright white in color, soft, shiny, smooth, easily
melts and heavy are identified as Khuraka tin 5.

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Tariq et al., IJPSR, 2014; Vol. 5(1): 171-177.

E-ISSN: 0975-8232; P-ISSN: 2320-5148

Qalai which is available in the market is almost
pure and is not adulterated with any other metal. So
it is not a necessary to purify it 6 but reports are
available that showed raw tin or improperly
prepared kushta qalai may cause various ill
effects like diabetes (ziabetus), leprosy (juzam),
abdominal tumor, cardiac diseases (amraz qalb),
spasmodic pain, piles (bawaseer), gout (niqras),
goiter, cough (sual), dyspnoea (usr-e-tanaffus),
weakness (zof)and vomiting (qai) 7.
So in this study, before using qalai, it was
subjected to tasfiya or shodhana (purification)
which makes it compatible for the body 8. Qalai is
used chiefly in diseases of genitourinary organs 9,
blood and lungs. In the west oxide of tin is
preferred as therapeutic agent for staphylococcal
infections 4. KQ is considered to be highly efficient
in spermatorrhoea (jiryan), leucorrhoea (sailan ur
rehem), gonorrhea (sozak) 10, 11. It is also used as a
remedy for premature ejaculation as an enhancer of
viscosity of seminal fluid 12.
Earlier few clinical researches have been
documented regarding the efficacy of KQ in certain
diseases. But till date no systematic effort has been
carried out on this preparation with respect to
physicochemical classification, which is an integral
part for drug standardization. So in this research
work KQ was prepared according to the classical
text of Unani literature by employing Electric
Muffle Furnace as heating device for incineration.
To ensure the proper preparation of kushta,
classical standard tests were performed. Further
KQ was subjected for modern quality control
parameters of analysis. The results obtained are
taken as standard for kushta qalai for future
references.

FIG. 1: RAW QALAI

FIG. 2: QALAI MUSAFFA (DETOXIFIED TIN)

Method of preparation of Kushta qalai: Kushta
was prepared as per Kitab ul taklees14 with a minor
modification, that instead of using the cowdung
cakes it was prepared in Muffle Furnace because of
ease of preparation and better temperature control.
In 120 gm aspgol husk 150 ml water was added
which was absorbed till morning (Fig. 3).

MATERIALS AND METHODS: Qalai, haldi
(Curcuma longa- root) powder and aspgol
(Plantago ovata) were purchased from the local
market in Bangalore.
Method of detoxification: Raw Qalai (Fig. 1) was
melted and dipped in aab sambhalu (Vitex negundo
decoction) in which a pinch of haldi (Curcuma
longa) was added. The procedure was repeated
three times 13. By this procedure qalai musaffa
(detoxified tin) was obtained (Fig. 2).

FIG.3 ASPGOL (PLANTAGO OVATA)

In the morning, two pellets of aspgol were made
and 12 gm qalai musaffa was placed between
them14. Heating was given as per Parmar et al. The
peak temperature maintained was 1008°C for 35±5
minutes, above 800°C temperature was maintained
for 20±5 minutes and above 600°C temperature
was maintained for 40±5 minutes 8.

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Tariq et al., IJPSR, 2014; Vol. 5(1): 171-177.

After completion of heating Kushta was taken out
from the furnace (Fig. 4) and was triturated
separately in mortar and pestle and finished product
obtained i.e. Kushta qalai (Fig. 5) was preserved in
an air tight clean bottle.

E-ISSN: 0975-8232; P-ISSN: 2320-5148

Bulk density and tapped density: LBD (Loose
Bulk Density) and TBD (Tapped Bulk Density)
were ascertained by following method 15. 2 g KQ
was placed into a 10 ml measuring cylinder and the
initial volume was noted. Then tapping was done.
The tapping was continued until no further change
in volume was observed. LBD and TBD were
calculated by the following equation.
LBD = Weight of the powder / volume of the
packing. TBD = Weight of the powder / Tapping
volume of the packing.

FIG. 4 KUSHTA TAKEN OUT FROM FURNACE

Hausner’s ratio: Hausner’s ratio was determined
as the ratio between the tapped density to bulk
density and was calculated by the following
equation 16.
Hausner’s ratio = Tapped density / Bulk Density
Carr’s index: Carr’s compressibility index was
calculated by 17;
Carr’s index = (T.d – B.d)/T.d ×100
Where T.d=Tapped density, B.d- Bulk density

FIG. 5 KUSHTA QALAI

Physico-chemical parameters: The prepared KQ
was evaluated for classical parameters like
organoleptic properties, floating test, fineness test,
wall stick test, thumb finger test as well as modern
scientific parameters like bulk density, tapped
density, Hausner’s ratio, Carr’s compressibility
index, pH, loss of weight on drying at 1050C, total
ash, acid insoluble ash, water soluble ash, water
insoluble ash and water soluble extractive value.
Quantitative estimation of tin and qualitative
estimation of other metals was also performed. The
tests were repeated thrice to obtain mean values.
Floating test: If a small quantity of kushta is
sprinkled on water surface it should float on the
surface.
Fineness test: On rubbing a small quantity of the
kushta between the fingers it should enter into the
lines on the fingers.
Loss of metallic lustre: When visually examined
preferably in presence of sun light no metallic
luster should be observed.

Loss of weight on drying at 105°C: 200 mg of
kushta was spread homogeneously in petridish and
was heated at 105oC then cooled in a desiccator and
weighed. The process was repeated till two
consecutive weights were constant. The percent
loss in weight was calculated18.
Determination of pH in 1% solution and 10%
solution
The pH value of 1% solution: 1 gm KQ was
dissolved in 100 ml distilled water and filtered
through whatman filter paper and pH was measured
with digital pH meter 18.
The pH value of 10% solution: 10 gm KQ was
dissolved in 100 ml distilled water and filtered
through whatman filter paper and pH measured
with a digital pH meter18.
Determination of total ash: 2 g kushta qalai was
incinerated in silica dish at a temperature not
exceeding 450oC. The percentage of ash was
calculated with reference to air dried drug19.
Determination of acid-insoluble ash: To the
crucible containing total ash 25 ml of dilute Hcl

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Tariq et al., IJPSR, 2014; Vol. 5(1): 171-177.

was added. The insoluble matter was collected on
Whatman ash less filter paper and washed with hot
water until the filtrate is neutral. The filter paper
containing the insoluble matter was transferred to
the original crucible, dried on a hot-plate and
ignited to constant weight. The residue was
allowed to cool in a suitable desiccator for 30
minutes and weighed without delay. The content of
acid-insoluble ash was calculated with reference to
the air-dried drug 20.
Determination of water soluble ash: The ash was
boiled for 5 minutes with 25 ml of water and
insoluble matter was collected in a crucible or on
an ashless filter paper and wash with hot water, and
ignited for 15 minutes at a temperature not
exceeding 450oC. The weight of the insoluble
matter was subtracted from the weight of the ash;
the difference in weight represents the watersoluble ash 21.
Determination of extractive value: 4.0g of kushta
was accurately weighed and put in a conical flask.
100 ml of water was added and weighed to obtain
the total weight including the flask. It was shaked
well and was allowed to stand for 1 hour. A reflux
condenser was attached to the flask and boiled for 1
hour. 25 ml of the filtrate was transferred to a tared
petridish and evaporated to dryness on water-bath
then dried at 105°C for 6 hours. Then it was cooled
in a desiccator for 30 minutes and weighed 22.

E-ISSN: 0975-8232; P-ISSN: 2320-5148

Qualitative
estimation
of
Aluminium
compounds: 20-25 gm kushta was dissolved in 1
ml distilled water then 0.5 ml hydrochloric acid
was added followed by 0.5 ml thioacetamide
reagent.
Drop wise 2 M sodium hydroxide was added, a
gelatinous white precipitate appeared that got
dissolved in an excess of sodium hydroxide
solution. Gradually 2 M ammonium chloride
solution was added, the gelatinous white precipitate
reappeared 24.
Qualitative estimation of Lead compound: 20-30
mg of kushta was dissolved in 1 ml of 5 M acetic
acid and 5 ml of distilled water was added followed
by 0.2 ml of potassium iodide. A yellow precipitate
was formed 24.
RESULTS AND DISCUSSION: The colour of
KQ was light grey. It was odorless, tasteless,
lusterless, smooth to touch, and very fine (Table
2). Floating test (Fig. 6), grain floating test (Fig. 7),
thumb finger test (Fig. 8) and fineness test were
positive (Table 3). All these parameters satisfied
the standards of a kamil kushta (ideal kushta) on
classical parameters.

Quantitative estimation of qalai (Tin): 0.5g of the
Kushta qalai was taken in 250 ml beaker and
dissolved in 25ml distilled water. 10ml
concentrated Nitric acid was added into solution
and the solution was digested, diluted and boiled on
water bath. After cooling the solution was filtered
through whatman 42 number filter paper. The
precipitate was washed several times with 1% hot
Nitric acid solution and dried. The precipitate was
transferred along with filter paper to the weighed
silica crucible which was then heated. The process
of heating and cooling was repeated till the
constant weight was obtained as Tin oxide 23.
Qualitative estimation of Iron compounds: 20-25
mg kushta was dissolved in distilled water; 1 ml of
5% w/v solution of potassium ferrocyanide was
added. A dark blue colour precipitate appeared
which was insoluble in 5 ml of 2M HCl 24.

International Journal of Pharmaceutical Sciences and Research

FIG. 6

FLOATING TEST

FIG. 7 RICE FLOATING ON WATER

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Tariq et al., IJPSR, 2014; Vol. 5(1): 171-177.

E-ISSN: 0975-8232; P-ISSN: 2320-5148

Less extractive values again confirm that kushta
was prepared properly and finished product was
free from organic material. The analytical results of
kushta qalai showed that the mean percentage of
the tin oxide in Kushta qalai was 90.04±0.04%
(Fig. 11). It indicated that majority of the kushta
was in oxide form. Qualitative test showed
presence of iron, aluminium and absence of lead
(Table 5).
FIG. 8 FINENESS TEST

The mean value of bulk density and tapped density
of KQ were 1.32± 0.00 gm/ml and 2.24±0.02
gm/ml respectively (Fig. 9). Density is defined as
mass of a substance per unit volume 25. Bulk
density largely depends upon particle shape. As the
particle size increases bulk density decreases. High
value of bulk density of KQ indicates very small
particle size 26. The mean value of Hausner’s ratio
and Compressibility index were 1.77±0.02 and
44.15±0.86 % respectively (Table 4). Hausner’s
ratio of KQ was greater than 1.2 (Fig. 9), indicated
poor flow properties 27.
More compressible the drug, less flowable the
powder will be25. Compressibility higher than 38
indicates very, very poor flowability of KQ16, 28.
pH in 1% and 10% solution were 10.47±0.00 and
11.17± 0.02 respectively (Table 4). It is mentioned
that most of the kushtajat are alkaline 29. It may
also be concluded that the finished product was
content of metallic oxides (stannous oxide) as the
fact that pH value of water solutions of metal
oxides is basic 30.
The mean percentage of loss of weight on drying
was 0.019±0.00% (Table 4). As the prepared
kushta showed very less weight loss on drying, it
could be assumed that the finished product was
devoid of water and organic matters. The mean
percentage value of the total ash, acid insoluble
ash, water soluble ash and water insoluble ash were
96.47±0.07%, 36.87±0.06%, 5.1±0.10% and
91.64±0.20% respectively (Table 4). High ash
value (Fig. 10) shows the presence of very high
inorganic content. The mean percentage of the
water soluble extractive value was 0.34±0.00%
(Table 4). Extractive values help in the
determination of the adulteration and is an index of
the purity of the drugs. In case of kushta extractive
value is performed to extract out organic matter if
present 31.

TABLE 1: PHYSICAL PROPERTIES OF RAW QALAI
Properties
Raw Qalai
Nature
Hard
Color
Silvery white
Lusture
Metallic
Streak
White
Transparency
Opaque
TABLE 2: ORGANOLEPTIC PROPERTIES OF RAW
QALAI AND KUSHTA QALAI
Properties
Raw Qalai
Kushta Qalai
Color
White
Light grey
Odor
Odorless
Odorless
Taste
Tasteless
Tasteless
Touch
Smooth
Smooth
Appearance
Metallic
Lusterless
TABLE NO. 3: PRELIMINARY TEST OF KUSHTA
QALAI
Positive
Floating test
Very fine
Fineness test
Positive
Wall stick test
Positive
Finger test
TABLE 4: PHYSICOCHEMICAL TESTS OF KUSHTA
QALAI (n=3)
Parameters
Mean ± SEM
Bulk density (gm/ml)
1.32± 0.00
Tapped Density (gm/ml)
2.24±0.02
Hausner’s ratio (HR)
1.77±0.02
Compressibility index (%)
44.15±0.86
pH (1%)
7.35±0.00
pH (10%)
7.22± 0.00
Loss of weight on drying (%)
0.019±0.00
Total ash (%)
96.47±0.07
Acid insoluble ash (%)
36.87±0.06
Water insoluble ash (%)
91.64±0.20
Water soluble ash (%)
5.1±0.10
Extractive value (%)
0.34±0.00
Tin oxide (%)
90.04±0.04
Table 5: Qualitative estimation of Kushta Qalai
Present
Iron
Present
Aluminium
Absent
Lead

International Journal of Pharmaceutical Sciences and Research

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Tariq et al., IJPSR, 2014; Vol. 5(1): 171-177.

E-ISSN: 0975-8232; P-ISSN: 2320-5148

As no standard physicochemical profile of kushta
qalai is reported till date, the current data may be
considered as standard for future studies. The
analytical result shows the presence of Iron and
Aluminum in KQ whereas only pure tin was taken
for the preparation of kushta.

FIG. 9: BULK DENSITY, TAPPED DENSITY AND
HAUSNER’S RATIO OF KUSHTA QALAI

The method of preparation of KQ consists of the
treatment of qalai with aab sambhalu (Vitex
negundo), haldi (Curcuma longa) during
detoxification process and aspgol (Plantago ovata)
during calcination procedure therefore these herbs
might be the source of iron and aluminum in the
finished product. These two components might
have synergistic effect as therapeutic agent instead
of providing any harmful and undesirable effects.
REFERENCES
1.

2.
3.

FIG. 10: TOTAL ASH, WATER INSOLUBLE AND
ACID INSOLUBLE ASH OF KUSHTA QALAI

4.
5.

6.
7.

8.

9.

FIG. 11: QUANTITATIVE ESTIMATION
STANNOUS OXIDE IN KUSHTA QALAI

OF

CONCLUSION: Metal and mineral preparations
used in Unani-Tibb are regularly subjected to
scientific analysis and research laboratories now
and then publish articles about the existence of
heavy metals in Unani compound formulations.
However, it is necessary to take into consideration
that many metals are essential components of vital
molecules of the body. This study gave detailed
information about the method of preparation and
standardization parameters of kushta qalai on
classical as well as modern parameters.

International Journal of Pharmaceutical Sciences and Research

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How to cite this article:
Tariq M, Rahman K, Chaudhary SS and Imtiyaz S: Formulation and characterization of a traditional Unani formulation:
Kushta Qalai. Int J Pharm Sci Res 2013; 5(1): 171-77.doi: 10.13040/IJPSR. 0975-8232.5(1).171-77
All © 2013 are reserved by International Journal of Pharmaceutical Sciences and Research. This Journal licensed under a Creative Commons Attribution-NonCommercial-ShareAlike 3.0 Unported License.

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Formulation and characterization of a traditional unani formulation kushta qalai

  • 1. Tariq et al., IJPSR, 2014; Vol. 5(1): 171-177. E-ISSN: 0975-8232; P-ISSN: 2320-5148 IJPSR (2014), Vol. 5, Issue 1 (Research Article) Received on 11 August, 2013; received in revised form, 11 September, 2013; accepted, 17 December, 2013; published 01 January, 2014 FORMULATION AND CHARACTERIZATION FORMULATION: KUSHTA QALAI OF A TRADITIONAL UNANI Mohd. Tariq*1, Khaleequr Rahman 1, Shahid Shah Chaudhary 1 and Shaikh Imtiyaz 2 Department of Ilmul Saidla (Pharmacy), National Institute of Unani Medicine 1, Bangalore 560091, Karnataka, India Department of Moalajat (Medicine), National Institute of Unani Medicine 2, Bangalore 560091, Karnataka, India Keywords: Aspgol, Kushta, Qalai, Standardization, Unani Medicine Correspondence to Author: Mohd Tariq (M.D.) C-102, Third Floor, Street no. 3, West Gorakh Park, Shahdara, Delhi110032 , India E-mail:drtariqnium@gmail.com ABSTRACT: Kushta literally means burning of drugs of metallic, mineral or animal origin into their ash. Qalai (tin) based Unani compound formulation Kushta qalai (KQ) is used since antiquity for the treatment of various ailments. Although it is used on consistent basis by Hakims but at present there are no scientific data available about its quality control parameters. So, in this research article an emphasis is given on preparation and physicochemical assessment of KQ using classical as well as modern scientific parameters with an eye towards its standardization. In finished product floating test, grain floating test, thumb finger test and fineness test were positive. The mean value of bulk density and tapped density were 1.32±0.00gm/ml and 2.24±0.02gm/ml respectively. Hausner’s Ratio and Compressibility Index were 1.77±0.02 and 44.15±0.86% respectively. pH in 1% and 10% solution were 10.47±0.00 and 11.17±0.02 respectively. Loss of weight on drying was 0.019±0.00%. Total ash, acid insoluble ash, water soluble ash and water insoluble ash were 96.47±0.07%, 36.87±0.06%, 5.1±0.10% and 91.64±0.20% respectively. The water soluble extractive value was 0.34±0.00%. The results obtained might be treated as standard for future references. INTRODUCTION: Kushta (organo-metallic preparation) is the finest class of solid dosage forms 1 used in Unani system of medicine obtained by incineration of metals, minerals or animal origin drugs with herbal extracts. These are administered orally in minute quantity with appropriate vehicle to make them biocompatible and are used for broad range of therapeutics 2. QUICK RESPONSE CODE DOI: 10.13040/IJPSR.0975-8232.5(1).171-77 Article can be accessed online on: www.ijpsr.com DOI link: http://dx.doi.org/10.13040/IJPSR.0975-8232.5(1).171-77 They address different ailments depending upon their method of preparation. Qalai (tin) is one of the most popular metal renowned for its wide spread applicability since Vedic period 3, It is used internally in the form of kushta. It is known by diverse vernacular names like rasas in Arabic, urziz in Persian, rang in Hindi, vanga in Sanskrit and kalai in Guajarati. It occurs as silver like metal, softer than gold, harder than lead, malleable and sparingly ductile with little elasticity 4. There are two varieties of qalai viz. khuraka and mishraka, only the former being acceptable for therapeutic applications. Samples having the characteristics; bright white in color, soft, shiny, smooth, easily melts and heavy are identified as Khuraka tin 5. International Journal of Pharmaceutical Sciences and Research 171
  • 2. Tariq et al., IJPSR, 2014; Vol. 5(1): 171-177. E-ISSN: 0975-8232; P-ISSN: 2320-5148 Qalai which is available in the market is almost pure and is not adulterated with any other metal. So it is not a necessary to purify it 6 but reports are available that showed raw tin or improperly prepared kushta qalai may cause various ill effects like diabetes (ziabetus), leprosy (juzam), abdominal tumor, cardiac diseases (amraz qalb), spasmodic pain, piles (bawaseer), gout (niqras), goiter, cough (sual), dyspnoea (usr-e-tanaffus), weakness (zof)and vomiting (qai) 7. So in this study, before using qalai, it was subjected to tasfiya or shodhana (purification) which makes it compatible for the body 8. Qalai is used chiefly in diseases of genitourinary organs 9, blood and lungs. In the west oxide of tin is preferred as therapeutic agent for staphylococcal infections 4. KQ is considered to be highly efficient in spermatorrhoea (jiryan), leucorrhoea (sailan ur rehem), gonorrhea (sozak) 10, 11. It is also used as a remedy for premature ejaculation as an enhancer of viscosity of seminal fluid 12. Earlier few clinical researches have been documented regarding the efficacy of KQ in certain diseases. But till date no systematic effort has been carried out on this preparation with respect to physicochemical classification, which is an integral part for drug standardization. So in this research work KQ was prepared according to the classical text of Unani literature by employing Electric Muffle Furnace as heating device for incineration. To ensure the proper preparation of kushta, classical standard tests were performed. Further KQ was subjected for modern quality control parameters of analysis. The results obtained are taken as standard for kushta qalai for future references. FIG. 1: RAW QALAI FIG. 2: QALAI MUSAFFA (DETOXIFIED TIN) Method of preparation of Kushta qalai: Kushta was prepared as per Kitab ul taklees14 with a minor modification, that instead of using the cowdung cakes it was prepared in Muffle Furnace because of ease of preparation and better temperature control. In 120 gm aspgol husk 150 ml water was added which was absorbed till morning (Fig. 3). MATERIALS AND METHODS: Qalai, haldi (Curcuma longa- root) powder and aspgol (Plantago ovata) were purchased from the local market in Bangalore. Method of detoxification: Raw Qalai (Fig. 1) was melted and dipped in aab sambhalu (Vitex negundo decoction) in which a pinch of haldi (Curcuma longa) was added. The procedure was repeated three times 13. By this procedure qalai musaffa (detoxified tin) was obtained (Fig. 2). FIG.3 ASPGOL (PLANTAGO OVATA) In the morning, two pellets of aspgol were made and 12 gm qalai musaffa was placed between them14. Heating was given as per Parmar et al. The peak temperature maintained was 1008°C for 35±5 minutes, above 800°C temperature was maintained for 20±5 minutes and above 600°C temperature was maintained for 40±5 minutes 8. International Journal of Pharmaceutical Sciences and Research 172
  • 3. Tariq et al., IJPSR, 2014; Vol. 5(1): 171-177. After completion of heating Kushta was taken out from the furnace (Fig. 4) and was triturated separately in mortar and pestle and finished product obtained i.e. Kushta qalai (Fig. 5) was preserved in an air tight clean bottle. E-ISSN: 0975-8232; P-ISSN: 2320-5148 Bulk density and tapped density: LBD (Loose Bulk Density) and TBD (Tapped Bulk Density) were ascertained by following method 15. 2 g KQ was placed into a 10 ml measuring cylinder and the initial volume was noted. Then tapping was done. The tapping was continued until no further change in volume was observed. LBD and TBD were calculated by the following equation. LBD = Weight of the powder / volume of the packing. TBD = Weight of the powder / Tapping volume of the packing. FIG. 4 KUSHTA TAKEN OUT FROM FURNACE Hausner’s ratio: Hausner’s ratio was determined as the ratio between the tapped density to bulk density and was calculated by the following equation 16. Hausner’s ratio = Tapped density / Bulk Density Carr’s index: Carr’s compressibility index was calculated by 17; Carr’s index = (T.d – B.d)/T.d ×100 Where T.d=Tapped density, B.d- Bulk density FIG. 5 KUSHTA QALAI Physico-chemical parameters: The prepared KQ was evaluated for classical parameters like organoleptic properties, floating test, fineness test, wall stick test, thumb finger test as well as modern scientific parameters like bulk density, tapped density, Hausner’s ratio, Carr’s compressibility index, pH, loss of weight on drying at 1050C, total ash, acid insoluble ash, water soluble ash, water insoluble ash and water soluble extractive value. Quantitative estimation of tin and qualitative estimation of other metals was also performed. The tests were repeated thrice to obtain mean values. Floating test: If a small quantity of kushta is sprinkled on water surface it should float on the surface. Fineness test: On rubbing a small quantity of the kushta between the fingers it should enter into the lines on the fingers. Loss of metallic lustre: When visually examined preferably in presence of sun light no metallic luster should be observed. Loss of weight on drying at 105°C: 200 mg of kushta was spread homogeneously in petridish and was heated at 105oC then cooled in a desiccator and weighed. The process was repeated till two consecutive weights were constant. The percent loss in weight was calculated18. Determination of pH in 1% solution and 10% solution The pH value of 1% solution: 1 gm KQ was dissolved in 100 ml distilled water and filtered through whatman filter paper and pH was measured with digital pH meter 18. The pH value of 10% solution: 10 gm KQ was dissolved in 100 ml distilled water and filtered through whatman filter paper and pH measured with a digital pH meter18. Determination of total ash: 2 g kushta qalai was incinerated in silica dish at a temperature not exceeding 450oC. The percentage of ash was calculated with reference to air dried drug19. Determination of acid-insoluble ash: To the crucible containing total ash 25 ml of dilute Hcl International Journal of Pharmaceutical Sciences and Research 173
  • 4. Tariq et al., IJPSR, 2014; Vol. 5(1): 171-177. was added. The insoluble matter was collected on Whatman ash less filter paper and washed with hot water until the filtrate is neutral. The filter paper containing the insoluble matter was transferred to the original crucible, dried on a hot-plate and ignited to constant weight. The residue was allowed to cool in a suitable desiccator for 30 minutes and weighed without delay. The content of acid-insoluble ash was calculated with reference to the air-dried drug 20. Determination of water soluble ash: The ash was boiled for 5 minutes with 25 ml of water and insoluble matter was collected in a crucible or on an ashless filter paper and wash with hot water, and ignited for 15 minutes at a temperature not exceeding 450oC. The weight of the insoluble matter was subtracted from the weight of the ash; the difference in weight represents the watersoluble ash 21. Determination of extractive value: 4.0g of kushta was accurately weighed and put in a conical flask. 100 ml of water was added and weighed to obtain the total weight including the flask. It was shaked well and was allowed to stand for 1 hour. A reflux condenser was attached to the flask and boiled for 1 hour. 25 ml of the filtrate was transferred to a tared petridish and evaporated to dryness on water-bath then dried at 105°C for 6 hours. Then it was cooled in a desiccator for 30 minutes and weighed 22. E-ISSN: 0975-8232; P-ISSN: 2320-5148 Qualitative estimation of Aluminium compounds: 20-25 gm kushta was dissolved in 1 ml distilled water then 0.5 ml hydrochloric acid was added followed by 0.5 ml thioacetamide reagent. Drop wise 2 M sodium hydroxide was added, a gelatinous white precipitate appeared that got dissolved in an excess of sodium hydroxide solution. Gradually 2 M ammonium chloride solution was added, the gelatinous white precipitate reappeared 24. Qualitative estimation of Lead compound: 20-30 mg of kushta was dissolved in 1 ml of 5 M acetic acid and 5 ml of distilled water was added followed by 0.2 ml of potassium iodide. A yellow precipitate was formed 24. RESULTS AND DISCUSSION: The colour of KQ was light grey. It was odorless, tasteless, lusterless, smooth to touch, and very fine (Table 2). Floating test (Fig. 6), grain floating test (Fig. 7), thumb finger test (Fig. 8) and fineness test were positive (Table 3). All these parameters satisfied the standards of a kamil kushta (ideal kushta) on classical parameters. Quantitative estimation of qalai (Tin): 0.5g of the Kushta qalai was taken in 250 ml beaker and dissolved in 25ml distilled water. 10ml concentrated Nitric acid was added into solution and the solution was digested, diluted and boiled on water bath. After cooling the solution was filtered through whatman 42 number filter paper. The precipitate was washed several times with 1% hot Nitric acid solution and dried. The precipitate was transferred along with filter paper to the weighed silica crucible which was then heated. The process of heating and cooling was repeated till the constant weight was obtained as Tin oxide 23. Qualitative estimation of Iron compounds: 20-25 mg kushta was dissolved in distilled water; 1 ml of 5% w/v solution of potassium ferrocyanide was added. A dark blue colour precipitate appeared which was insoluble in 5 ml of 2M HCl 24. International Journal of Pharmaceutical Sciences and Research FIG. 6 FLOATING TEST FIG. 7 RICE FLOATING ON WATER 174
  • 5. Tariq et al., IJPSR, 2014; Vol. 5(1): 171-177. E-ISSN: 0975-8232; P-ISSN: 2320-5148 Less extractive values again confirm that kushta was prepared properly and finished product was free from organic material. The analytical results of kushta qalai showed that the mean percentage of the tin oxide in Kushta qalai was 90.04±0.04% (Fig. 11). It indicated that majority of the kushta was in oxide form. Qualitative test showed presence of iron, aluminium and absence of lead (Table 5). FIG. 8 FINENESS TEST The mean value of bulk density and tapped density of KQ were 1.32± 0.00 gm/ml and 2.24±0.02 gm/ml respectively (Fig. 9). Density is defined as mass of a substance per unit volume 25. Bulk density largely depends upon particle shape. As the particle size increases bulk density decreases. High value of bulk density of KQ indicates very small particle size 26. The mean value of Hausner’s ratio and Compressibility index were 1.77±0.02 and 44.15±0.86 % respectively (Table 4). Hausner’s ratio of KQ was greater than 1.2 (Fig. 9), indicated poor flow properties 27. More compressible the drug, less flowable the powder will be25. Compressibility higher than 38 indicates very, very poor flowability of KQ16, 28. pH in 1% and 10% solution were 10.47±0.00 and 11.17± 0.02 respectively (Table 4). It is mentioned that most of the kushtajat are alkaline 29. It may also be concluded that the finished product was content of metallic oxides (stannous oxide) as the fact that pH value of water solutions of metal oxides is basic 30. The mean percentage of loss of weight on drying was 0.019±0.00% (Table 4). As the prepared kushta showed very less weight loss on drying, it could be assumed that the finished product was devoid of water and organic matters. The mean percentage value of the total ash, acid insoluble ash, water soluble ash and water insoluble ash were 96.47±0.07%, 36.87±0.06%, 5.1±0.10% and 91.64±0.20% respectively (Table 4). High ash value (Fig. 10) shows the presence of very high inorganic content. The mean percentage of the water soluble extractive value was 0.34±0.00% (Table 4). Extractive values help in the determination of the adulteration and is an index of the purity of the drugs. In case of kushta extractive value is performed to extract out organic matter if present 31. TABLE 1: PHYSICAL PROPERTIES OF RAW QALAI Properties Raw Qalai Nature Hard Color Silvery white Lusture Metallic Streak White Transparency Opaque TABLE 2: ORGANOLEPTIC PROPERTIES OF RAW QALAI AND KUSHTA QALAI Properties Raw Qalai Kushta Qalai Color White Light grey Odor Odorless Odorless Taste Tasteless Tasteless Touch Smooth Smooth Appearance Metallic Lusterless TABLE NO. 3: PRELIMINARY TEST OF KUSHTA QALAI Positive Floating test Very fine Fineness test Positive Wall stick test Positive Finger test TABLE 4: PHYSICOCHEMICAL TESTS OF KUSHTA QALAI (n=3) Parameters Mean ± SEM Bulk density (gm/ml) 1.32± 0.00 Tapped Density (gm/ml) 2.24±0.02 Hausner’s ratio (HR) 1.77±0.02 Compressibility index (%) 44.15±0.86 pH (1%) 7.35±0.00 pH (10%) 7.22± 0.00 Loss of weight on drying (%) 0.019±0.00 Total ash (%) 96.47±0.07 Acid insoluble ash (%) 36.87±0.06 Water insoluble ash (%) 91.64±0.20 Water soluble ash (%) 5.1±0.10 Extractive value (%) 0.34±0.00 Tin oxide (%) 90.04±0.04 Table 5: Qualitative estimation of Kushta Qalai Present Iron Present Aluminium Absent Lead International Journal of Pharmaceutical Sciences and Research 175
  • 6. Tariq et al., IJPSR, 2014; Vol. 5(1): 171-177. E-ISSN: 0975-8232; P-ISSN: 2320-5148 As no standard physicochemical profile of kushta qalai is reported till date, the current data may be considered as standard for future studies. The analytical result shows the presence of Iron and Aluminum in KQ whereas only pure tin was taken for the preparation of kushta. FIG. 9: BULK DENSITY, TAPPED DENSITY AND HAUSNER’S RATIO OF KUSHTA QALAI The method of preparation of KQ consists of the treatment of qalai with aab sambhalu (Vitex negundo), haldi (Curcuma longa) during detoxification process and aspgol (Plantago ovata) during calcination procedure therefore these herbs might be the source of iron and aluminum in the finished product. These two components might have synergistic effect as therapeutic agent instead of providing any harmful and undesirable effects. REFERENCES 1. 2. 3. FIG. 10: TOTAL ASH, WATER INSOLUBLE AND ACID INSOLUBLE ASH OF KUSHTA QALAI 4. 5. 6. 7. 8. 9. FIG. 11: QUANTITATIVE ESTIMATION STANNOUS OXIDE IN KUSHTA QALAI OF CONCLUSION: Metal and mineral preparations used in Unani-Tibb are regularly subjected to scientific analysis and research laboratories now and then publish articles about the existence of heavy metals in Unani compound formulations. However, it is necessary to take into consideration that many metals are essential components of vital molecules of the body. This study gave detailed information about the method of preparation and standardization parameters of kushta qalai on classical as well as modern parameters. International Journal of Pharmaceutical Sciences and Research 10. 11. 12. 13. 14. 15. 16. Anonymous: National Formulary of Unani Medicine. Central Council of Research in Unani Medicine, New Delhi, Part 1, 2006: 66, 74, 329. Hiremath R, Jha CB and Narang KK: Vanga Bhasma and its XRD Analysis. Ancient Sci of Life 2010; 29(4): 24 -28. Jani JH, Patgiri BJ, Ravishankar B and Prajapati PK: The Role of Media in the Preparation of Vanga Bhasma. Jour of Res in Ayurveda 2009; 30 (2): 211-216. Nadkarni KM: Indian Materia Medica. Popular Prakashan Pvt. Ltd, Bombay, 1976: 116. Galib, Barve M, Mashru M, Jagtap C, Patgiri BJ and Prajapati PK: Therapeutic potentials of metals in ancient India: A review through Charaka Samhita. Jour of Ayurveda & Integ. Med. 2011; 2(2): 55-63. Kareem BH and Ferozuddin CH: Miftahul Khazain. Idara Kitabus shifa, New Delhi, YNM: 249. Sarkar PK, Das S and Prajapati PK: Ancient concept of metal pharmacology based on Ayurvedic literature. Ancient Sci of Life 2010; 29 (4): 1-6. Parmar DK, Patgiri BJ and Prajapati PK: Standardization of Gaja Puta and Ardha Gaja Puta in the preparation of Vanga Bhasma. Jour of Res in Ayurveda 2010; 31(4): 511-516. Nagaraju V, Joshi D and Aryya NC: Study on the vrsya property (testicular regenerative potential) of vanga bhasma. Ancient sci of life 1985; 5(1): 42 – 48. Tariq NA: Tajul Mufradat. Idara Kitab Usshifa, New Delhi, 2010: 375. Kabiruddin M: Makhzanul Mufardat. Idara Kitab Usshifa, New Delhi, 2007: 420. Said HM: Hamdard Pharmacopoeia of Eastern Medicine. Sri Satguru Publication, New Delhi, 1997: 232. Hafeez A: Sanatal Taklees. Central Council of Research in Unani Medicine, New Delhi, YNM: 79. Kabeeruddin HM: Kitabul Taklees. Central Council of Research in Unani Medicine, New Delhi, YNM: 181. Farzana A, Halder S, Shuma ML and Rouf AS: In Vitro Release Kinetics Study of Indomethacin 12Hr Matrix Tablet From Methocel K4M CR and Methocel K15M CR. Jour of Biomed and Pharm Res. 2012; 1(3): 60-65. Nuka R, Potu AR and Nandan R: Formulation Development and In-Vitro Evaluation of Ramipril Micropellets. World jour of pharma res 2012; 2(1): 76-87. 176
  • 7. Tariq et al., IJPSR, 2014; Vol. 5(1): 171-177. 17. Ramanjaneyulu M, Kumar MS, Bairam R and Babu PM: Formulation and Evaluation of Oral Disintegrating Release Dosage Form Containing Meclizine Hcl. Int jour of pharm 2012; 2(4): 717-726. 18. Anonymous: Physicochemical Standards of Unani Formulations. Central Council of Research in Unani Medicine, New Delhi, 2006: 142-145. 19. Anonymous: The Ayurvedic Pharmacopoeia of India. GOI. Dept. of AYUSH, New Delhi, Vol. 2, 2008: 160. 20. Anonymous: The Unani Pharmacopoeia of India. GOI. Dept. of AYUSH, New Delhi, Vol. 2, 2007: 116. 21. Anonymous: The Unani Pharmacopoeia of India. GOI. Dept. of AYUSH, New Delhi, Vol. 3, 2007: 134. 22. Anonymous: Quality Control Methods for Herbal Materials. WHO, Geneva, 2011: 31. 23. Sharma PV and Singh VP: Standardization of an Ayurvedic Drug: Trivanga Bhasma. Ancient Sci of Life 1987; 10 (3): 148-149. 24. Anonymous: Physicochemical Standards of Unani Formulations. Central Council of Research in Unani Medicine, New Delhi, Part 4, 2006: 142-150. E-ISSN: 0975-8232; P-ISSN: 2320-5148 25. William L and Wilkins: Remington: The Science and Practice of Pharmacy. Wolters Kluwer Health Pvt Ltd, New Delhi, 21st ed, Vol. 1, 2006: 110. 26. Lachman L, Liberman HA and Kanig JL: The Theory and Practice of Industrial Pharmacy. Varghese Publishing House, Mumbai, 1991: 316. 27. Aulton EM: Aultons Pharmaceutics. Churchill Livingstone, London, 2009: 176-178. 28. Qiu Y, Chen Y, Geoff G, Zhang Z, Liu L and Porter W: Developing Solid Oral Dosage Forms: Pharmaceutical Theory & Practice. Academic press, USA, 2009: 170. 29. Qasmi IA: Kitabul Taklees. Aligarh Muslim University, Aligarh, YNM: 36. 30. Pant KM, Gill JS, Jain SC, Joshi R, Agarkar SC and Srivastava VP. Science and Technology. Class 8th, Publication department NCERT, New Delhi, 2003: 67, 83. 31. Rasheed A, Marri A and Naik MM: Standardization of Bhasma: importance and prospects. Jour of Pharm Res 2011; 4 (6): 1931-1933. How to cite this article: Tariq M, Rahman K, Chaudhary SS and Imtiyaz S: Formulation and characterization of a traditional Unani formulation: Kushta Qalai. Int J Pharm Sci Res 2013; 5(1): 171-77.doi: 10.13040/IJPSR. 0975-8232.5(1).171-77 All © 2013 are reserved by International Journal of Pharmaceutical Sciences and Research. This Journal licensed under a Creative Commons Attribution-NonCommercial-ShareAlike 3.0 Unported License. This article can be downloaded to ANDROID OS based mobile. Scan QR Code using Code/Bar Scanner from your mobile. (Scanners are available on Google Playstore) International Journal of Pharmaceutical Sciences and Research 177