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Proximate analysis & Optimization of extraction condition 32 3.3 Habitat Argemone mexicana linn., is a species of poppy found in Mexico and now widely naturalized in many parts of the world. An extremely hardy pioneer plant, it is tolerant of drought and poor soil, often being the only cover on new road cuttings or verges. 3.3.1 Classification Botanical Name : Argemone mexican linn. Family : Papaveraceae 3.3.2 Common Name Tamil : Kurukkum Telugu : Bhrahmadandi Malayalam : Bhrahmadanti Hindi : Satyanashi Gujarati : Darudi Orissa : Kantakusham Marathi : Pivla Dhotra 3.3.3 Reported phytochemical constituents Alkaloids isocorydine, (+)-reticuline, protopine, allocryptopine 1 , berberin 2 , dehydrocheilanthifoline, coptisine, argemexicaine A, argemexicaine B, chelerythrine, sanguinarine, (-)-tetrahydroberberine, O-methylzanthoxyline, arnottianamide, (±)-6-acetonyldihydro- chelerythrine 3 , dehydrocorydalmine, jatrorrhizine, columbamine, oxyberberine 4 , cryptopine, ( -)-cheilanthifoline, (-)-scoulerine, (-)- stylopine, nor-sanguinarine, nor-chelerythrine 5 , muramine, oxyhydrastinine, thalifoline, 8-acetonyl dihydrosanguiranine 6 , protomexicine, 13-oxoprotopine.8-methoxydihydrosanguiranine 7 , (+)-

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Page 1: 3.3 Habitat - INFLIBNETshodhganga.inflibnet.ac.in/bitstream/10603/44178/9/09_chapter 3.pdf · Argemone mexicana linn., is a species of poppy found in Mexico and now widely naturalized

Proximate analysis &

Optimization of extraction condition

32

3.3 Habitat

Argemone mexicana linn., is a species of poppy found in Mexico

and now widely naturalized in many parts of the world. An extremely

hardy pioneer plant, it is tolerant of drought and poor soil, often being

the only cover on new road cuttings or verges.

3.3.1 Classification

Botanical Name : Argemone mexican linn.

Family : Papaveraceae

3.3.2 Common Name

Tamil : Kurukkum

Telugu : Bhrahmadandi

Malayalam : Bhrahmadanti

Hindi : Satyanashi

Gujarati : Darudi

Orissa : Kantakusham

Marathi : Pivla Dhotra

3.3.3 Reported phytochemical constituents

Alkaloids

isocorydine, (+)-reticuline, protopine, allocryptopine1, berberin

2,

dehydrocheilanthifoline, coptisine, argemexicaine A, argemexicaine B,

chelerythrine, sanguinarine, (-)-tetrahydroberberine,

O-methylzanthoxyline, arnottianamide, (±)-6-acetonyldihydro-

chelerythrine3, dehydrocorydalmine, jatrorrhizine, columbamine,

oxyberberine4, cryptopine, (-)-cheilanthifoline, (- )-scoulerine, (- )-

stylopine, nor-sanguinarine, nor-chelerythrine5, muramine,

oxyhydrastinine, thalifoline, 8-acetonyl dihydrosanguiranine6,

protomexicine, 13-oxoprotopine.8-methoxydihydrosanguiranine7, (+)-

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Proximate analysis &

Optimization of extraction condition

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cheilanthifoline8, argemexirine, (±)-tetrahydrocoptisine,

dihydrocoptisine9, (+)-argenaxine, (+)-higenamine, N-

demethyloxysanguinarine, pancorine, dihydrochelerythrine, angoline10

,

dihydrosanguiranine11

.

Terpenoids

trans-phytol10

, β-amyrin12

Steroids

stigma-4-en-3,6-dione10

, β-sitosterol13

Carbohydrates

Lactose, arabinose14

Amino Acid

Cysteine, phenylalanine12

Flavonoids

Luteolin, eriodictyol15

, isorhamnetin-3-O-β-Dglucopyanoside16

,

isorhamnetin13

, isorhamnetin-7-O-β-D-diglucopyanoside17

,

isorhamnetin-3,7-O-β-D-digluco pyanoside18

, quercetin, rutin, mexitin19

.

Phenolic Acid

tannic acid, caffeic acid, ferulic acid20

3.4 Therapeutic Claims

Antidiabetic activity21

, Antioxidant activity22

, Wound Healing

activity23

, Antihelmintic activity24

, Larvicidal activity25

,

Hepatoprotective activity26

and Anticancer activity27

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Proximate analysis &

Optimization of extraction condition

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3.5 Pharmacology

A. Argemone mexicana linn. is used in the treatment of tumors,

warts, skin diseases, inflammations, rheumatism, jaundice,

leprosy, piles, warm infestations and dysentery.

B. Leaf decoction is used to cure malarial fever and ulcers. Seeds

are efficient in treating leprosy, dropsy and jaundice. Juice of the

plant is used as a remedy against Scorpion bite 28.

3.6 Proximate analysis

All the plant material are or natural herbs are usually put in

seclusion store and therefor it remain for a long time. As a time of

storage of such plant material or crude drug to maintain the proper

ventilation, suitable temperature, humidity control and light should be

maintain for their pharmacological action however it is observed that,

crude plant materials before being taken for processing are not analyzed.

It will changes its original characteristics. To avoid this, the crude drugs

should be tested for the following tests as per the USP and Indian herbal

Pharmacopoeia (IHP)29-33

.

foreign organic matter

water soluble extractives

ethanol soluble extractives

ether soluble extractives

total ash content

acid soluble ash

water soluble ash

sulphated ash

loss on drying

percentage moisture content.

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Optimization of extraction condition

35

3.6.1 Foreign organic matter

Medicinal plant material should be entirely free form visible

signs of contamination, i.e. insects, mould and other animal

contamination. It is rarely possible to obtain plant material that is

entirely free from foreign matter. However no dangerous, harmful or

poisonous foreign material should be allowed.

It is required to remove any sand, soil, dust and other foreign

organic matter after the cutting of medicinal plant for testing.

Macroscopic examination can conveniently be employed for the

determination of the foreign matter in whole plant material.

Foreign matter is a material consisting all of following:

Dust, soil, sand, stone and other minerals which are not adhering

to medicinal plant material.

Any medicinal plant material or the material other than named

with limits specified for the plant material concerned.

Any organism and product of organism are present.

Procedure

The plant material was washed with water and the dust particles

were removed from the surface of the leaves. Excess water was allowed

to drain off by spreading the leaves on filter paper. The 500gm of

washed and drained leaves were taken and spread as a thin layer on a

white cloth. Foreign matter was sorted by visual inspection by using

magnifying lens. The portions of the sorted foreign matter were weighed

and the content of foreign matter in g per 100 g of the sample was

calculated. The procedure was carried out for the total of three sets.

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Proximate analysis &

Optimization of extraction condition

36

Observation

It was observed that the percentage of foreign organic matter in

Argemone mexicana linn. was 0.02 gm. The results are shown in the

table.

Calculations

% Foreign organic matter = (M1-M)x100

M2

Where

M= Weight of empty dish in g.

M1= Weight of dish with foreign matter in g.

M2 = Weight of sample in g.

% Foreign matter content = (42.86-42.84)X100

500

Table 1 Percentage of foreign organic matter

Sample % of Foreign Organic Matter

% of Means

Argemone mexicana linn.

0.02

0.02

0.02

0.02

Extractable matter

The use of this method to determine the amount of phyto

constituents extracted with solvent from a given amount of medicinal

plant material. As per the Herbal Pharmacopoeia water, ethanol and

petroleum ether used as solvent to determine the extractable matter.

3.6.2 Procedure for water extractable matter

Accurately weighed of 4gm of Argemone mexicana linn. whole

plant powder was taken in 250ml round bottom flasks for three times.

To each flask, 100ml of water was added. All flasks were stirring

frequently for six hours and then put it eighteen hours. Then filter it

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Proximate analysis &

Optimization of extraction condition

37

through whatman filter paper no. 1 avoid the loss of solvent. The

filtrates were transfered to previously weighing clean beaker and

evaporated to dryness on a water bath after evaporation the extract was

dried at the1040 C for six hours kept in desiccator for cooling the

substance. The beaker was weighed and percentage of extractable matter

in water was calculated.

Observation

The percentage extractable matter in water of Argemone

mexicana linn. is between the 18.65 – 19.05%.

Table 2 Percentage of water extractable matter

Sample % of water extract % of Means

Argemone mexicana linn.

18.65

18.84

19.05

18.84

3.6.3 Procedure for ethanol extractable matter

As above take accurately weighed of 4gm of Argemone mexican

linn. whole plant powder was taken in 250ml round bottom flasks for

three times. To each flask, 100ml of water was added. All flasks were

stirring frequently for six hours and then put it eighteen hours. Then

filter it through whatman filter paper no. 1 avoid the loss of solvent. The

filtrates was transfer to previously weighing clean beaker and

evaporated to dryness on a water bath after evaporation the extract was

dried at the1040 C for six hours kept in desiccators for cooling the

substance. The beaker was weighed and percentage of extractable matter

in water was calculate.

Observation

The percentage extractable matter in ethanol of Argemone

mexicana linn. is between the 5.49 – 5.90%.

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Proximate analysis &

Optimization of extraction condition

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Table 3 Percentage of ethanol extractable matter

Sample % of ethanol extract % of Means

Argemone mexicana linn.

5.49 5.60 5.90 5.66

3.6.4 Procedure for ether extractable matter

As above take accurately weighed of 4gm of Argemone mexicana

linn. whole plant powder was taken in 250ml round bottom flasks for

three times. To each flask, 100ml of petroleum ether was added. All

flasks were stirring frequently for six hours and then put it eighteen

hours. Then filter it through whatman filter paper no. 1 avoid the loss of

solvent. The filtrates was transfer to previously weighing clean beaker

and evaporated to dryness on a water bath after evaporation the extract

was dried at the 1050 C for six hours kept in desiccator for cooling the

substance. The beaker was weighed and percentage of extractable matter

in enter was calculate.

Observation

The percentage extractable matter in ether of Argemone mexicana

linn. is between the 0.49 – 0.50%.

Table 4 Percentage of ether extractable matter

Sample % of ether extract % of Means

Argemone mexicana linn.

0.49

0.50

0.50

0.50

3.6.5 Ash content

The ash content is received after the ignition of herbal plant

materials is determined by different type of method.

total ash

acid insoluble ash

water insoluble ash

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Proximate analysis &

Optimization of extraction condition

39

sulphated ash

The total ash method is designed to measure the total amount of

material remaining after ignition. This include both physiological ash

which is derived from plant tissue itself and non-physiological ash,

which is the residue of the extraneous matter (e.g. soil and sand)

adhering to the plant surface.

Acid insoluble ash is the residue obtained after boiling the total

ash with dilute hydrochloric acid and ignite the remaining insoluble

matter. This measures the amount of the silica and sand.

Water soluble ash is the difference in weight between the total

ash and the residue after treatment of the total ash with water.

Sulphated ash is the residue of the inorganic sulphates obtained

after treatment of substance with concentrated sulphuric acid, which

decomposes and oxidizes the organic matter. This measures the amount

of nonvolatile impurities present in organic substances.

3.6.6 Total Ash

Apparatus - Silica crucible, muffle furnace, desiccators, hot air oven

Procedure

Weighing the 2 gm of the dried material was taken in a silica

crucible and then ignited with the flame of Bunsen burner for one hour.

After the completion of the ignition it was kept in the muffle furnace at

5500 C till the gray ash was obtained. It was then cooled in a desiccator

and weighted. The process was repeated three times and all valued are

mean of three reading.

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Proximate analysis &

Optimization of extraction condition

40

Observation

It was observed that the percentage total as content of Argemone

mexicana linns. of whole plant powder were between 9.25-9.46%.

Table 5 Percentage of total ash content

Sample % of total ash content % of

Means

Argemone mexicana linn.

9.25

9.33

9.46

9.34

3.6.7 Acid insoluble ash

Chemicals- dilute HCl, 5N HCl, and AgNO3

Apparatus - Silica crucible, muffle furnace, desiccators, hot air oven,

water bath.

Procedure

Weighing the 2gm of the dried whole plant material powder was

taken in silica crucible and ignite with the flame of Bunsen burner for

about one hour. The silica crucible was kept in a muffle furnace at 5500

C till the gray ash was obtained. The ash was moistened by the

concentrated HCl and evaporate to dryness after which was kept in hot

air oven at 1350 C for three hours. After cooling the crucible 25ml of

dilute HCl was added and heated on water bath for half hour. It was

allowed the cool and filtered through whatman filter paper No. 1. The

residue was then washed with hot water till washing were free from

chloride it was checked by AgNO3 Soln. The filter paper and residue

were put in a dish and ignite in a muffle furnace at 5500

C for one hour.

Observations

It was observed that the percentage of acid insoluble ash content

of Argemone mexicana linn. whole plant powder were between 0.28-

0.30%.

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Proximate analysis &

Optimization of extraction condition

41

Table 6 Acid insoluble ash content

Sample % of Acid insoluble ash content % of

Means

Argemone mexicana linn.

0.28

0.34

0.31

0.31

3.6.8 Water soluble ash

Chemicals - Distilled Water

Apparatus - Silica dish, desiccator, hot air oven, muffle furnace

Procedure

Take 25ml distilled water add in silica crucible containing the

total ash boiled for ten minutes. The insoluble ash was collect on the

filer paper. The residue was washed with hot water and ignited in a

crucible for fifteen minutes at a temperature of 4500 C. The water

soluble ash was calculated by subtracting the weight of the residue from

the weight of the total ash.

Observation

It was observed that the percentage of water soluble ash content

of Argemone mexicana linn. powder was found between 3.22-3.44%.

Table 7 Water soluble ash content

Sample % of Water soluble ash content % of

Means

Argemone mexicana linn.

3.22

3.36

3.44

3.34

3.6.9 Sulphated ash

Chemicals - Sulphuric acid

Apparatus - Silica crucible, desiccator, hot air oven muffle furnace.

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Proximate analysis &

Optimization of extraction condition

42

Procedure

Accurately weighed 2 gm of dried whole material powder was

taken in silica crucible. The material was ignited, at first until the

substance was thoroughly charred. The crucible was then cooled and the

residue was moistened with 1 ml of concentrate sulphuric acid. The

crucible was heated and ignited at 8000

C, till at the black particles

disappeared the cooled the crucible and add a few drop of sulphuric acid

and heating was repeated.

Observation

It was observed that the percentage sulphated ash content of

Argemone mexicana linn. was found to be between 12.77-13.43%.

Table 8 Sulphated ash

Sample % of Sulphated ash content % of

Means

Argemone mexicana linn. 12.77 12.98 13.43 13.06

3.6.10 Loss on Drying

Apparatus - ASTM SIEVE (85/BS Sieve), wide mouth stoppered

weighing bottle, desiccator, hot air oven.

Procedure

5 gm of Argemone mexicana linn. whole plant powdered samples

were weighed separately in wide mouth stoppered weighing bottle. The

bottle were then placed with lid open in a hot air oven and maintained at

1000C ± 2. The samples were kept in an oven for 2 hours. The bottle

were the remove, covered and placed in a desiccator. The bottles were

weighed after cooling to room temperature and weighed

The bottles were again kept in the hot air oven for 2 hours and the

above procedure was repeated till the difference the weight between two

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Proximate analysis &

Optimization of extraction condition

43

successive weighing was less than 1mg. Three readings for each sample

were recorded.

Observations

It was observed that the percentage of loss on drying for

Argemone mexicana linn. whole plant powder were found to be a 8.43. –

9.20%.

Table 9 Percentage of loss on drying

Sample % of loss on drying

% of

Means

Argemone mexicana linn.

8.43

9.20

8.65

8.76

3.7 Optimization of extraction condition

There are number of methods for extraction, purification and isolation of

compounds. The first fractionation step is general extraction of secondary

metabolites which is done either by using single solvents such as methanol or

by using petroleum ether to defatted the material. Methanol dissolves most of

the secondary metabolites and enhancing their release from cellular matrix/cell

sufrace34,35

. Filtration or centrifugation is the first basic technique used to

separate insoluble material and filtrate that contain dissolved secondary

metabolite. The choice of extraction procedure and extraction solvent depends

on the physicochemical nature of secondary metabolite, nature of plant material

(dried parts) and their physical state (particle size). An idea about properties of

interfering compound provides best criteria for solvent selection for extraction

and to select method of extraction, so prior to extraction a major emphasis must

be given on nature of interfering compounds.

Extraction involves solvent penetration into herb cells/tissues,

solubilization of secondary metabolites and finally release the dissolved

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Proximate analysis &

Optimization of extraction condition

44

secondary metabolites in solvent of extraction. Solvents of varying polarity are

used alone or in combinations for extraction depend on component, so a large

proportion of the unwanted material is removed. This includes class of

preparation known as decoctions, infusions, fluid extracts, tinctures, and

powder extracts.

The techniques usually employed for extraction are ultrasonic, rotary

evaporators, hydro distillation, super critical fluid chromatography, multiple

solvent extraction, liquid chromatography.

The present research work concerns primarily with the basic extraction

procedures for crud drugs to obtain the therapeutically desirable portion and

eliminate the unwanted material by treatment with a selective solvent, known

as the menstrum. The principle methods of extraction are maceration,

percolation, decoction, digestion and infusion. The quality of the finished

product can be enhanced by optimization of primary extracts. The USP (United

State Pharmacopeia) provides general guidelines for maceration and

percolation.

Maceration

In this process of maceration the solid ingredients are placed in a

stoppered flask with prescribed volume of solvent and allowed to stand in a

warm place with frequent agitation, until soluble matter is dissolved. The

mixture is filtered and after most of the liquid has drained off, the residue is

washed with sufficient quantity of the prescribed solvent.

Percolation

The powdered drug is mixed within appropriate quantity of the

prescribed solvent to make it evenly and uniformly humid. It is allowed to

stand for 15 minutes and then transferred to a percolator. Sufficient prescribed

solvent is added to saturate the drug. The percolation is allowed to proceed at

specified rate gradually adding sufficient solvent.

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Optimization of extraction condition

45

Decoction

This is one of the most popular processes which extracts water soluble

and heat stable constituents from crude drugs by boiling in a water for 15

minutes, cooling, straining and passing sufficient cold water through the drug

to produce the required volume.

Digestion

This is a form of maceration in which gentle heat is used during the

process of extraction. It is used when moderately elevated temperature is not

objectionable and the solvent efficiency of the menstrum is increased thereby.

Infusion

An Infusion is a dilute solution of the readily soluble constituents of

crude drugs. Fresh infusions are prepared by macerating the drugs for a short

period of time with ether or boiling water.

In the present research work, the plant materials selected were subjected

to extraction using various solvents and from the extraction efficiency the best

solvent was selected. In addition the parameters chosen for the optimization of

the experimental conditions, for getting the best extraction efficiency were

amount of the solvent

time of extraction and

number of extractions.

Choice of Extracting Solvent

To obtain proper extraction of a given plant material, the ideal solvent is

obviously one that has maximum selectivity, best capacity for extraction in

terms of coefficient of the product in the medium and is compatible with

properties of the material to extract.

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Optimization of extraction condition

46

Usually secondary metabolites have different degrees of polarity so the

solvent(s) should be chosen for the extraction should be considered carefully to

ensure dissolution of secondary metabolites under study.

Solvent should have following properties:

1. easy to remove

2. inert

3. nontoxic

4. not easily inflammable

5. no interaction or less chemical interaction

Solvent is employed to dissolve the secondary metabolite and finally to

diffuse out the dissolved solute into bulk solvent phase.

Solvent employed are:

1. Polar: Water

2. Non-polar: Petroleum ether, chloroform,

3. Semi polar: Ethanol, Methanol

Polar Solvents

The polar components like polysaccharides, phenols, aldehydes,

ketones, amines, and other oxygen containing compounds dissolve in water due

to formation of hydrogen bonding. The solubility of aliphatic alcohol increases

the solubility of the compound in water decreases. Additional polar groups are

present in the molecule, as found in propylene glycol, glycerin, and tartaric

acid, water solubility increases greatly due to addition of polar groups.

Branching of the carbon chain reduces the nonpolar effect and leads to

increased water solubility (tertiary butyl alcohol is miscible in all proportions

with water, whereas n-butyl alcohol dissolves to the extent of about 8g/100 ml

of water at 20°C). The polar solvents such as water act as solvents according to

the following mechanisms:

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Proximate analysis &

Optimization of extraction condition

47

1. Normally polar solvents have high dielectric constant which reduces the

force of attraction between oppositely charged ions in crystals such as

sodium chloride or molecule. Polar solvent like water has a dielectric

constant of 80 while which dissolve polar component rapidly than non-

polar solvent chloroform, which has a dielectric constant of 5 and due to

low dielectric constant, ionic compounds are practically insoluble in

non-polar organic solvents.

2. Polar solvents break covalent bonds of potentially strong electrolytes by

acid-base reactions since these solvents are amphiprotic. For example,

water brings about the ionization of HCI as follows:

a. Weak organic acids are not ionized appreciably by water

b. Their partial solubility is attributed instead to the hydrogen bond

formation by with water. Phenols and carboxylic acids, however,

are readily dissolved in solutions of strong bases.

3. Polar solvents has property of dipole interaction forces, particularly

hydrogen-bond formation due to which solvating molecules and ions

become soluble and which leads to the solubility of the compound. The

solubility of sodium salt of oleic acid and water is due to ion-dipole

interaction.

Non-polar Solvents

Non-polar solvents have low dielectric constants and dissolve non-polar

solutes with similar internal pressures through induced dipole interactions.

Ionic and polar solutes are insoluble or slightly soluble in non-polar solvents.

Weak Van-Der-Waals and London forces are responsible for the solubility of

molecules.

Semi-polar Solvents

Semi-polar solvents like ketones and alcohols can induce a certain

degree of polarity in non-polar solvent like benzene is readily polarizable,

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Optimization of extraction condition

48

becomes soluble in alcohol. Semi-polar compounds act as intermediate solvents

which bring about miscibility of polar and non-polar liquids.

Influence of Solvents

A component may behave like strong electrolyte or non-electrolyte,

depending on pH of solution. Precipitation of components occurs, when the pH

of solution is adjusted to such a value at which un-ionized molecules are

produced in sufficient concentration to exceed its solubility36

.

Solvent-Solute interactions

Polar solvents like water is a good solvent for salts, sugars etc while

non-polar solvents like mineral oil and benzene are often solvents for

substances that are normally only slightly soluble in water. It proves the

doctorine of “like dissolves like".

In the present work different solvent (non-polar to polar) were used to

optimize the extractive values of Argemone Mexicana Linn. They were

methanol, ethanol, chloroform, ethyl acetate, n-hexane and petroleum ether.

3.7.1 Optimization of Solvent

In this work the amount of Argemone mexicana linn. whole plant

powder was kept constant throughout the experiment. In different set of round

bottom flasks, accurately weighed Argemone mexicana linn. whole powder was

taken. In this different sets of round bottom flasks, equal amount of different

solvent were added separately and kept for one hour. Then these extract were

filtered through whatman filter paper (No. 41) in previously weighed dry

beakers separately and solvent were evaporated to dryness on a water bath. The

dried residues were weighed and the percentage extraction of various solvent

was calculated. From the percentage extraction values, the best solvent was

optimized. The results are given in below table.

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49

Table 10 Optimization of solvent for extraction

Sr. Solvent Weight of

Powder (g)

Amount of

solvent (ml)

% of

Extraction

1 Petroleum ether 1.0 10.0 0.53

2 n-Hexane 1.0 10.0 1.54

3 Chloroform 1.0 10.0 1.78

4 Ethyl acetate 1.0 10.0 2.32

5 Ethanol 1.0 10.0 5.46

6 Methanol 1.0 10.0 8.06

In this experiment, the amount of Argemone mexicana linn. whole plant

powder taken was kept constant throughout the experiment. In different set of

round bottom flasks, accurately weighed Argemone mexicana linn. whole plant

powder was taken. In this different sets of round bottom flasks, different

amount of methanol were added and kept for one hour. Then these extracts

were filtered through whatman filter paper no.41 in pre weighed dry beaker

separately and solvent was evaporated to dryness on a water bath. The dried

residue was then weighed and the percentage extractions were calculated. From

percentage extraction values, the amount of solvent was optimized.

From graph of volume of solvent versus percentage extraction as shown

in figure 1, it was observed that the percentage extraction levels remain

constant after certain volume of a solvent used for extraction. The amount

of methanol added and the corresponding percentage extraction is given in

table 11.

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Optimization of extraction condition

50

Table 11 Optimization of amount of solvent for extraction

Sr. Weight of Powder (g) Amount of solvent (ml) % Extraction

1 1.0 10.0 7.73

2 1.0 25.0 8.26

3 1.0 50.0 9.96

4 1.0 75.0 10.43

5 1.0 100.0 11.26

Each observation is mean of three extractions.

Figure 1 - Optimization of Amount of Solvent

7.738.26

9.9610.43

11.26

0

2

4

6

8

10

12

10 25 50 75 100

% o

f Ex

trac

tio

n

Amount of Solvent

Optimation of Amount of Solvent

3.7.2 Optimization of Time

For optimization of time of contact between powder and solvent, the

optimized volume of solvent was added to the sample and the contents in the

flasks were filtered after different time intervals. The above procedure was

repeated and the percentage extractives values were calculated. From the

percentage extractive values, the optimization time was determined.

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Proximate analysis &

Optimization of extraction condition

51

For optimization of time, methanol was added to the sample kept in

different flasks. The contents in the flasks were filtered after different time

intervals and the percentage extractives value were calculated.

From the graph of time in minutes versus percentage extraction as

shown in figure 2 it was observed that the percentage extraction levels after

certain time of extraction remains constant. The time in minutes and

corresponding percentage extractive values are given in Table 12

Table 12 Optimization of time for extraction

Sr.No. Solvent Weight of

Powder(g)

Time of

extraction

(min.)

%of Extract

1 Methanol 1.0 30 7.58

2 Methanol 1.0 60 8.90

3 Methanol 1.0 90 10.80

4 Methanol 1.0 120 11.28

5 Methanol 1.0 150 11.72

Figure 2 - Optimization of time

7.58

8.9

10.811.28 11.72

0

2

4

6

8

10

12

14

30 60 90 120 150

% o

f Ext

ract

ion

Time

Optimization of Time for Extraction

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Optimization of extraction condition

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3.7.3 Optimization of number of extraction

For optimization of the number of extractions, the optimized amount of

selected solvent was added to the sample in different sets of flasks and these

flasks were kept aside for 90 minutes (optimized time) for plant. Then the

content of the flasks were filtered separately through whatman filter paper no.

41 in pre-weighed dry beakers. The residues were again taken in a flask and

extracted again using methanol for 90 minutes (optimized solvent and time).

The above procedure was repeated.

The percentage extraction values were calculated. From these values

number of extractions was optimized37-40

.

From the graph of extraction versus percentage extraction it was

observed that the percentage extraction level after certain number of extraction

remain constant.

The number of extractions and the corresponding percentage extraction

for methanol is given in Table 13.

Table 13 - Optimization of number of extractions

Sr. No. Weight of Powder (g) No. of Extraction (n) % Extraction

1 1.0 1 9.86

2 1.0 2 10.90

3 1.0 3 12.60

4 1.0 4 13.38

5 1.0 5 13.86

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Proximate analysis &

Optimization of extraction condition

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Figure 3 - Optimization of number of extraction

9.8610.9

12.613.38 13.86

0

2

4

6

8

10

12

14

16

1 2 3 4 5

% o

f Ex

trac

tio

n

Number of Extraction

Optimization of Number of Extraction

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