Review on churna Kalpana and quality analysis of powder by different techniques

1. Review on churna
Kalpana and quality
analysis of powder by
different techniques

2. INTRODUCTION:
 Churna is fine dry powder of any single drug or more than one drug.
 Churna Kalpana is upkalpana of kalka Kalpana, because churna Kalpana is a dry
state of kalka Kalpana.
DEFINITION: (a/c to sa.m .6/1)
अत्यन्तशुष्क
ं यद् द्रव्यं सुपिष्टं वस्त्रगालितम् ।
तत् स्त्याच्चुर्णं रजः क्षोदस्त्तन्मारा कर्षसम्ममता । ।
Synonyms- क्षोद,रज
मारा-1 कर्ष (12 gm)

3. TYPES:(a/c to chakrapani)
चूर्णष कल्क एवान्तर्ाषवनीयं द्पवपवधो हि कल्कः-स द्रवोऽद्रवश्चेतत कृ त्वा।।
चूर्णष is included in itself dry kalka.
कल्क is 2 types- sadrava and adrava kalka
चूर्णष comes under adrava kalka
Prakshepa Dravya Matra In Churna: (Sa.m.6/2)
चुर्णे गुडः समो देयः शक
ष रा द्पवगुर्णा र्वेत्।
चुर्णेर्ु र्म्जषतं हिङ्गु देयं नोत््िेदकृ दर्वेत् । ।
गुड-सममारा
शक
ष रा-द्पवगुर्ण मारा
र्म्जषत हिङ्गु-न उत््िेदकृ त्

4. Churna Sevana Vidhi : (sa.m.6/3)
लििेच्चुर्णं द्रवैः सवैर्ृषताद्यैद्षपवगुर्णोम्न्मतैः।
पिबेच्चतुगुषर्णैरेव चूर्णषमािोडडतं द्रवैः ।।
 If churna is advise to consume in paste form with any liquid(ghrita, madhu) , than
the drava dravya should be taken double the quantity of churna i.e 2 karsha(24 gm).
 If churna is said to drink after mixing with liquid (dugdha, go mutra, takra) , than
the drava dravya quantity should be 4 times i.e. 4 karsha(48gm).

5. Anupana Of Churna:(Sa.m.6/4)
चूर्णषविेिगुहटकाकल्कानामनुिानकम्।
वातपित्तकफातङ्क
े त्ररद्व्येकििमािरेत्। ।
anupana of churna, avaleha, gutika and kalka:
Dosha Anupana matra
vata 3 pala
pitta 2 pala
kapha 1 pala

6. Dose:
1 Karsa = Approximately 12 grams
Preservation
Churna should be packed in airtight container.
Shelf life :
 2 months according to Sharangadhara
 2 years according to Official Gazette of India

7. PARAMETERS FOR STANDARDISATION OF CHURNA:
The guidelines prescribed by Ayurvedic Pharmacopoeia of India (API).
(A)Ayurvedic parameters:
The churna should be very fine ,amorphous (structureless) and moisture free.
(B)Modern parameters:
(a) Study of organoleptic characters-:
1. colour
2. odour
3. taste

8. (b)Physico-chemical evaluation:
Determination of moisture content[Loss on drying]
Determination of Ash value
Acid insoluble ash
Water soluble ash
 Water soluble extractive value
 Alcohol soluble extractive value
 pH determination

9. (C) Determinationof physicalcharacteristicsof powder
Bulk density
Tapped density
Angle of repose
 Hausner Ratio
Carr’s Index
(D) ) Determinationof physicalcharacteristicsof powder
limits for heavy metels
 microbial limits in ASU products
Pesticidal Residue & Aflatoxin Limits
(E) Chromatographically analysis

10.  Pharmacognostical study -
1. Determination of foreign matter
About 100 g of the sample was spread out as a thin layer.
Foreign matter was detected by inspection with the unaided eye or
by the use of a magnifying lens (6x), separated, weighed and the
percent foreign matter was calculated .
2. Organoleptic parameters
Organoleptic characters like colour, odour, taste, appearance and
texture of the ingredients and formulation samples were evaluated
using a reported method .

11.  3. Fluorescence analysis :
Fluorescence characters of powdered materials in different standard
reagent solutions in the ordinary visible light and ultraviolet light (both long
365 nm and short 254 nm wavelengths) were observed .
 4. Microscopic study
Five mg of the sieved (80#) powder samples (churna and ingredients) were
taken and washed with plain water.
Then the samples were treated separately with iodine, chloral hydrate,
pholorglucinol or potassium iodide; a drop of glycerine was added and
mounted.
The powder sample characters were then observed by a Carl Zeiss binocular
microscope attached with a camera according to the standard method .

12. DETERMINATION OF PARTICLE SIZE:
A suitable quantity of sample is weighed and transferred to set of sieves from
number 10 to 85. the sieves are taken in sieve shakers for about 30 minutes and the
residue on each sieve is weighed separately.
All particle pass
through sieve no
Not more than 40% pass
through
Coarse powder 10 44
Moderately coarse
powder
22 60
Moderately fine powder 44 85
Fine powder All pass through 85
numbered sieve
Very fine powder All pass through 120
numbered silk sieve

13. Physico - chemical evaluation
13
Determination Of MoistureContent(Loss On Drying)
Significance -The Loss on Drying Test is
designed to measuretheamount ofwaterand
volatilematters in a sample when the sample is
dried under specified conditions.
HOT AIR OVEN
IR MOISTURE
BALANCE

14. LOSS ON DRYING at 1050 c
10 gm Drug
powdered
drug in Petri
dish
Heat at 1050 c
for 5 hour
Cool & Weight
the air Dried
sample
LOSS ON DRYING %w/w – (W2-W3)×100
(W2-W1)
Wt of Petri dish =W1
Wt of Petri dish + sample = W2
After drying
Wt of Petri dish + sample = W3
0
14
0
Electronic weighing balance
Petri Dish
Hot Air Oven
Dessicator

15. Impact Of Moisture Content
Microbial Growth –Presence of moisture influences growth of
micro organisms.
Effectstheflow property of thepowders .
Effects Physical and Chemical stability of theProduct.
15

16. Determination OfAsh Value
TotalAsh
 Theresidueremainingafterincineration.Ashvalueis
useful in determining quality and purityof crude
drugs.
 Onincineration, crudedrugsnormally leaveanashusually
consisting of carbonates,phosphatesandsilicatesofsodium,
potassium, calciumand magnesium.
 Highashvalue isanindicativeof Contamination,substitution
,adulterationof carelessnessduring manufacturing .
 The maximum temperatureused for total ashshould be not more
then 4500C becausealkalichlorides thatmay be volatileinhigher
temperaturewould be lost.
MUFFLE FURNANCE
Electric
Bunsen
Burner

17. Total Ash
Total ash %by weight = W
eight of Ash x100
Weightof sample taken
Incinerate
2-3 gm
sample in
Silica
crucible
Set the temperature at
450 0 C and incinerate
until free from carbon
Calculate the
percentage of Ash
17

18. Acid InsolubleAsh
Acidinsolubleashmeanstheashinsolublein dilute
hydrochloric acid.
Acidinsolubleashvalueindicatessiliceousimpurities
18

19. Acid insolubleAsh
Boil the ash
obtained from
Ash value
determination
for 5 minutes
with 25 ml dil
hydrochloric
acid
Collect the
insoluble matter
in an ash less
filter
paper(Whattman
41)
. Acid Insloluble Ash % by weight =
Weight of Acid insoluble Ash
x100
Weight of Ash sample taken
Wash with
hot water
and ignite
to the
constant
weight .
Weigh the
ash
19

20. Water SolubleAsh
Thewater-solubleashisusedto detectthepresenceof material
exhaustedbywater.
20

21. Water solubleAsh
Boil the ash
obtained from
Ash value
determination
for 5 minutes
with 25 ml
water
Collect the
insoluble matter
in an ashless
filter
paper(Whattman
41)
x100
. Water soluble Ash % by weight =
Weight of Water soluble Ash
Weight of Ash sample taken
Wash with
hot water
and ignite
to the
constant
weight .
Weigh the
ash
21

22. Extractive Values
 Extractivevaluesareprimarilyusefulforthedeterminationof exhaustedor
adulterateddrugs.
 Theextractivevalueofthe crudedrugdeterminesthequalityaswell as
purity of the drugs.
 Exhaustingcrudedrugswithdifferentsolventsto evaluatethe
approximate measures of their chemical constituents
 Lessextractivevalue indicatesadditionof exhaustedmaterial,
adulterationor incorrectprocessing duringdrying or storageor
formulating 22

23. Extractive Values
23
 Water soluble Extractives -water-soluble constituents like tannins,
mucilages,carbohydrates,phenolics,glycosidesetc
 Alcohol Soluble Extractives- Alcohol soluble constituents essential oils ,
tannins, glycosides,resins,alkaloids,Organicacidsetc.
 EtherSolubleExtractives-Volatileoilsand fats

24. Alcohol Soluble Extractive Value
50
Macerate 5
g of
Powdered
drug + 100
ml of ethyl
alcohol
24 hrs ,shaking
frequently six
hours and allow
to stand for
eighteen hours.
Filter &
evaporate 25
ml of the filtrate
to
dryness,drying
at 1050 c to
constant wt
Calculate the
percentage of
alcohol-soluble ext
Alcohol soluble extractive value (% ) =Wt of the ext ×Vol of Alcohol
Wt of sample × Vol of the filtrate
× 100

25. Water Soluble Extractive Value
5
1
Macerate 5
g of
Powdered
drug + 100
ml of
Distillled
water
24 hrs ,shaking
frequently six
hours and allow
to stand for
eighteen hours.
Filter &
evaporate 25
ml of the filtrate
to
dryness,drying
at 1050 c to
constant wt
Calculate the
percentage of
water soluble ext
Water soluble extractive value (% ) =Wt of the ext ×Vol of water
Wt of sample × Volof the filtrate
× 100

26. DETERMINATION OF pH VALUES :
The pH value of an aqueous liquid may be defined as the common logarithm of the
reciprocal of the hydrogen ion concentration expressed in g per litre.
For the purpose of pharmacopeia pH is defined as the value given by a suitable ,
properly standardised , pH meter capable of reproducing pH value to 0.05ph unit using
an indicator electrode sensitive to hydrogen-ion activity , the glass electrodes and a
suitable reference electrode.

27. Determination of pH
Afigure expressing the acidity or alkalinity of a solution
on a logarithmicscaleon which7isneutral,lowervalues
aremore acid and highervaluesmorealkaline
58

28. Determination of physical characteristics of powder
Bulk density
• It is the ratio of given mass of powder and its bulk volume. It is determined by
transferring an accurately weighed amount of powder sample to the graduated
cylinder with the aid of a funnel. The initial volume was noted. The ratio of
weight of the volume it occupied was calculated. As shown in fig no- 1
• Bulk density=W/V0 g/ml
• Where, W = mass of the powder, V0 = untapped volume

29. Tapped density:
• It is measured by transferring a known quantity (25g) of powder into a bulk density
apparatus and tapping it for 100 times.
• The initial volume was noted. The graduated cylinder was tapped continuously for a
period of 10-15 min.
• The density can be determined as the ratio of mass of the powder to the tapped
volume.
• As shown in fig no 2
• Tapped volume= W/Vf g/ml
• Where, W = mass of the powder, Vf = tapped volume

30. Angle of repose – The main application of the angle of repose is to assess the
flowability of a granular material
The internal angle between the surface of the pile of powder and the horizontal
surface is known as the angle of repose.
The powder is passed through funnel fixed to a burette at s height of 4 cm.
A graph paper is placed below the funnel on the table. The height and the radius of
the pile were measured.
 Angle of repose of the powder was calculated using the formula; as shown in fig
no 3
 Angle of repose= tan-1(h/r) ,
 Where, h=height of the pile
, r = radius of pile.

33. HAUSNER RATIO:
Hausner’s ratio: It indicates the flow properties of the powder.
The ratio of tapped density to the bulk density of the powder is called
Hausner ratio.
[Hausner ratio= Tapped density/bulk density]

34. CARR’S INDEX (Compressibility Index)
The Carr’s index is an indication of the compressibility of a powder.
The Carr’s index is calculated by;
Carr’s index=(Pₜ-Pb)/pt×100
Pₜ -Tapped density
Pb-Bulk density

36. Limits For HeavyMetals
Heavy metals AYUSH Limit WHO USFDA HAS
Singapore
Lead 10ppm 10ppm 10 ppm 20ppm
Arsenic 3ppm 3 ppm 10 ppm 5ppm
Mercury 1ppm 1ppm 1 ppm 0.5ppm
Cadmium 0.3 ppm 0.30ppm 0.30 ppm 0.05ppm
Determination of contaminants

37. Microbial Limits InAsu Products
Parameter Specifications
Total Bacterial count 1×10 5 CFU/gm
Yeast & Mould 1×10 3 CFU/gm
E Coli Absent
Salmonella Absent
P .aeruginosa Absent
S .aureus Absent

38. PesticidalResidue &Aflatoxin Limits
Parameter Specifications
Pesticidal Residue –
Organochloro group
Less than 1ppm
Aflatoxin B1-0.5 ppm
G1-0.5 ppm
B2 -0.1 ppm
G2-0.1 ppm

39. Chromatographic Techniques
TLC/HPTLCTechniques(WithMarker
compounds)

40. DETERMINATIONOF THIN-LAYRER CHROMATOGRAPHY :
APPARATUS REQUIRED: TLC Plates Development Chamber
Glass capillaries Conical Flasks
Sprayer UV Chamber Hot air oven
 Chromatography is any one of the several processes for separating and analysing
various gaseous or dissolved chemical material according to difference in their absorbency
with respect to a specific substance and according to their different pigments.
 The separation of chemical substances and particle by differential movement through
a two-phase system is called as chromatography.
stationary phase - for adsorption form
mobile phase - for liquid form
 The result of chromatography separation are expressed in the term of Rf value. It
defined as the distance travelled by the sample substance /distance travelled by the solvent

41. CONCLUSION -
In the last some years, the use of herbal drugs has been increased all over the world due
to their huge therapeutic effect and less adverse effects as compared to other medicines.
 The rising use of herbal drug by the human is forcing the driving force to evaluate the
health claim of these agents and to develop standards of quality, purity, safety and
efficacy of the drug.
 Mostly herbal drugs are effective but due to adulteration and lack of standardization, the
effectiveness of the herbal drug is decreased. So there is need of development of
standardization parameters.
 In the standardization of the herbal drug the physical, chemical, biological, analytical
parameters are carried out. It assures the quality, purity and safety of herbal drug.
For the quality assured herbal products, the standardization is required.
 In standardization, the above mentioned parameters i.e. authenticity, biological
parameter, chemical parameter, physical parameter and analytical profiling gives the
quality assured herbal products. HPTLC tool is mostly used for identification of the
compound.

42. THANK YOU