Title of Invention	"AN IMPROVED PROCESS FOR THE PRODUCTION OF DRY AQUEOUS EXTRACT OF VIJASAR (PTEROCARPUS MARSUPIUM)"
Abstract	The invention relates to an improved process for the production of dry aqueous extract of vijaysar heartwood (Petrocarpus marsupium) .The product is prepared by standardised extraction, concentration and spray drying techniques using minimum quantity of water and optimizing heat load and time of extraction of the said process. The process steps are: a) crushing of the pterocarpus marsupium (vijaysar) heart wood into wood chips,b) extracting the wood chips twice successively with water under refluxing conditions in the minimum ratio of 1:5, for a period of 5 hours each in a closed extractor with reflux condenser,c) filtering each water extract.,d) concentrating the filtrate in wiped film evaporator under vacuum at temperature ranging from 35°C- 65°C ,under reduced pressure ranging from 40-200 mg of Hg, e) Drying the concentrate by spray drying method to obtain the aqueous extract in powder form.

Title of Invention

"AN IMPROVED PROCESS FOR THE PRODUCTION OF DRY AQUEOUS EXTRACT OF VIJASAR (PTEROCARPUS MARSUPIUM)"

Abstract

The invention relates to an improved process for the production of dry aqueous extract of vijaysar heartwood (Petrocarpus marsupium) .The product is prepared by standardised extraction, concentration and spray drying techniques using minimum quantity of water and optimizing heat load and time of extraction of the said process. The process steps are: a) crushing of the pterocarpus marsupium (vijaysar) heart wood into wood chips,b) extracting the wood chips twice successively with water under refluxing conditions in the minimum ratio of 1:5, for a period of 5 hours each in a closed extractor with reflux condenser,c) filtering each water extract.,d) concentrating the filtrate in wiped film evaporator under vacuum at temperature ranging from 35°C- 65°C ,under reduced pressure ranging from 40-200 mg of Hg, e) Drying the concentrate by spray drying method to obtain the aqueous extract in powder form.

Full Text	The present invention relates to an improved process for the production of dry aqueous extract of vijaysar heartwood (Petrocarpus marsupium). The present invention particularly relates to an economic process for the preparation of stable dry powder from aqueous extract of heartwood of Bijasar (Pterocarpus marsupium) by standardised extraction, concentration and spray drying techniques using minimum quantity of water and optimizing heat load and time of extraction of the said process. Pterocarpus marsupium Roxb. (N.O. Leguminoseae) the Indian Kino tree, indigenously known as Vijaysar, Bija, Bijasar, Pitasal, Piyasal etc. is a large deciduous tree of central and South India and Srilanka, extending northwards as far as the hills of Bihar, Binda and Kumaon Terai. The tree yields the gum kina and its wood contains a dye soluble in water, having a blue flourescence. It was a popular belief that watery extract of the wood is cure for diabetes. Some medical practitioners maintain that the sugar content of the urine is reduced by drinking water from vessels of vijaysar. Vessels made of vijaysar have a popular reputation for transferring to their contents anti diabetic qualities (Trotter - The common commercial Timber of India and their uses, 156, 1944). Ojha, K.N et. al. [Ojha, K.N., Pabrai, Paramjit R. and Venkatachalam, K., Indian J. Pharmacology II, 188 (1949)] have reported that aqueous extract of Pterocarpus marsupium Roxb. given orally is effective in lowering blood sugar in rabbits as well as in diabetic patient, without any toxic symptoms. Seshadri (Seshadri, T.R. Phytochemistry 11, 881 (1972)) has reported Pterocarpus marsupium to be rich source of Polyphenolic compounds. Various researchers have isolated a number of compounds from extracts of Pterocarpus marsupium. Some of them are as follows: Stilbene, pterostilbene (Mathew, J., Subba Rao, A.V., and Subba Rao, N.V., Current Sci., 46, 337 (1997)); the sesquiterpene alcohols, (3-eudesmol, triterpene alcohol, erythrodiol-3-monoacetate [Adinarayana, D., Syamadunder, K.V., Phytochemistry, 21, 1083 (1982)]; catechin, epicatechin [Chakravarthy, B.K., Gupta, S., Gambir, S.S., and Gode, K.D., Life Sci, 29, 2043 (1981)]; the flavonoids, pseudobaptigenin liquiritigenin, garbanzol, 5-deoxykaempferol, chalcone, isoliquiritigenin, dihydrochalcone.pterosuprin and aromatic aldehyde, p-hydroxybenzaldehyde [Adinarayana, D., Syamasunder, K.V., Seliqmann, O., and Wagner, H, Z. Naturforsch 37C, 145 (1982)]; the isoflavonoid glycol, marsupol (4,4' dihydroxy-L-methylthydro benzoin) [ Subba Rao, A.V., and Mathew, J., Phytochemistry, 21, 1837 (1982)]; pterocarpols A and B [Bhargava, P.N. Proc. Ind. Acad. Sci. 24, 496 (1946)] and other phenolic compounds from extract of heart wood of P. marsupium (Maurya, R., Ray, A.B., J. of Natural Product Vol.-4 179-181 (1984). The process for production of aqueous extract of vijaysar (Pterocarpus marsupium) known for centuries is still being used commercially.(Caraka Samhita of Agnivesa, 194 A.D.) This process involves cutting of vijaysar heartwood, slicing the same and crushing it to 25-50 mm length with 5-10 mm width/height. The crushed wooden pieces are put in the open pan type steam extractor and 16 times water is added to these wooden chips. The mixture is heated by steam in the jacket or by direct fire and concentrated, until the volume of the mixture is reduced to % of its original volume. The concentrated mixture is filtered in ordinary filters and the filtrate is further concentrated in electrically heated vessels until, bone dry product is obtained. The total dry, water soluble extract obtained is around 8% of the crushed mass of the wood. And it takes around 72 hours for a batch of 100 kg of crushed wood to produce 8 kg of the product. Dry aqueous extract of vijaysar obtained from the above cited method, is only product known in Ayurveda. The time of extraction is very long and yield of the product thus obtained is low. The steam/electricity consumption is also very high. Further following disadvantages have been observed in the process described in the prior art. 1. The process involves boiling wood and water in the ratio of 1:16 and then concentrating the same to % of its original volume, making the process energy intensive with lot of wastage of steam/vapour in open pan. 2. Drying/further concentration step in electrically heated vessels is also energy intensive and the drying is not uniform. The final texture of the product is also dark brown. 3. Some of the bioactive constituents are likely to be lost or damaged with some loss of bioactiviety as a net result. Whereas, in the present invention authors have used novel, extraction with refluxing, vacuum concentration, and spray drying method, thereby reducing time of processing to 18 hours and consequent reduction in steam consumption and increasing the yield from 8% to 10.5%. The novelty of this invention resides in the use carrying out only two extractions of 5 hour each of the crushed heart wood with water, using wood:water ratio of 1:5 only, in each extraction. The extraction system is fully closed with reflux condenser. There has been no improvement in the process described in the literature ever since. The main objective of the present invention is to provide a faster and an economic process for the production of dried aqueous extract of vijaysar heartwood. The another objective is to concentrate the extract under vacuum, filtering and spray drying the material into a uniform powder. Yet another objective is to get powder having uniform hue and is stable at ambient temperature. Still another objective is to make the process cost effective and easy to operate, while retaining the original bioactivity. Accordingly the present invention provides an improved process for the production of dry aqueous extract of pterocarpus marsupium heartwood, consisting of the following steps: a) crushing of the pterocarpus marsupium (vijaysar) heart wood into wood chips, b) extracting the wood chips twice successively with water under refluxing conditions in the minimum ratio of 1:5, for a period of about 5 hours each in a closed extractor with reflux condenser, c) filtering each water extract., d) concentrating the filtrate in wiped film evaporator under vacuum at temperature ranging from 35°C- 65°C under reduced pressure ranging from 40-200 mg of Hg, e) drying the concentrate by spray drying method to obtain the aqueous extract in powder form and standardizing the product by HPLC profile . The total processing time for 5 kg batch is 11 hours and that for 100kg batch is 18 hours. In an embodiment of the present invention the extraction may be carried in closed extractor with reflux condensers having wood to water ratio of 1:5 and time of each extraction as five hours. In another embodiment the concentration of the filtrate may be carried out in vacuum operated wiped film evaporator. In yet another embodiment the spray drying may be carried out in a spray dryer at chamber temperature of 160-170°C. The present invention provides an improved and economic process for the production of aqueous extract of vijaysar heartwood, which comprises of crushing the heart wood in chips, followed by two water extractions of wood chips in water in the ratio of 1:5 under re fluxing condition for 5 hours each, concentration of the filtrate from extraction in vacuum operated, wiped film evaporator and spray drying the concentrate to get dry powder of extract. The process of the preparation of dry powder of aqueous extract of vijaysar heart wood (Pterocarpus marsupium) is described in detail as given below which is provided by way of examples for illustrations only and therefore should not be construed to limit the scope of the present invention. Experiment-1 ( 5 kg scale ) 5 kgs of crushed vijaysar heartwood is mixed with 25 litres of water in an extractor fitted with reflux condenser. The mixture is brought to the boiling temperature and refluxed for 5 hours. After this the water extract is (drained and filtered and sent to wiped film evaporator for concentration under vacuum. In the mean time 25 litres of fresh water are added to the already extracted vijaysar heartwood chips. The contents are once again boiled and refluxed for 5 hours. After draining and filtration the filtrate is taken to wiped film evaporator for vacuum concentration. In vacuum evaporator, concentration of filtrate is carried out at around 35°C and 40 mm of Hg (reduced pressure). The total volume of filtrate from two water extractions is about 45 litres as 5 litres is hold-up in the crushed wood. This 45 litres contains about 0.5 kg ( i.e.about 1%) of water solubles. The concentration of this lean mixture is increased to about 25-30% i.e. out of 45 litres, approximately 43 litres of water are evaporated. The final 25% concentrate is dried in spray dryer to obtain dry powder of extract of vijaysar heartwood. The yield of the final dry product is 0.50 kgs. Time cycle - Extraction - 10 hours Concentration 45 minutes. @ 1-1.5 litre/minute. Spray drying 15 minutes Total 11 hours Experiment-2 ( 5 kg scale ) 5 kgs of crushed vijaysar heartwood is mixed with 25 litres of water in an extractor fitted with reflux condenser. The mixture is brought to the boiling temperature and refluxed for 5 hours. After this the water extract is drained and filtered and sent to wiped film evaporator for concentration under vacuum. In the meantime 25 litres of fresh water are added to the already extracted vijaysar heartwood chips. The contents are once again boiled and refluxed for 5 hours. After draining and filtration the filtrate is taken to wiped film evaporator for vacuum concentration. In vacuum evaporator, concentration of filtrate is carried out at around 50°C and 100 mm of Hg (reduced pressure). The total volume of filtrate from two water extractions is about 45 litres as 5 litres is hold-up in the crushed wood. This 45 litres contains about 0.5 kg (i.e.about 1%) of water solubles. The concentration of this lean mixture is increased to about 25-30% i.e. out of 45 litres, approximately 43 litres of water are evaporated. The final 25% concentrate is dried in spray dryer to obtain dry powder of extract of vijaysar heartwood. The yield of the final dry product is 0.52 kgs. Time cycle - Extraction - 10 hours Concentration 45 minutes. @ 1-1.5 litre/minute. Spray drying 15 minutes Total 11 hours Experiment-3 ( 5 kg scale ) 5 kgs of crushed vijaysar heartwood is mixed with 25 litres of water in an extractor fitted with reflux condenser. The mixture is brought to the boiling temperature and refluxed for 5 hours. After this the water extract is drained and filtered and sent to wiped film evaporator for concentration under vacuum. In the meantime 25 litres of fresh water are added to the already extracted vijaysar heartwood chips. The contents are once again boiled and refluxed for 5 hours. After draining and filtration the filtrate is taken to wiped film evaporator for vacuum concentration. In vacuum evaporator, concentration of filtrate is carried out at around 65°C and 200 mm of Hg (reduced pressure). The total volume of filtrate from two water extractions is about 45 litres as 5 litres is hold-up in the crushed wood. This 45 litres contains about 0.5 kg (i.e.about 1%) of water solubles. The concentration of this lean mixture is increased to about 25-i.e. out of 45 litres, about 43 litres of water are evaporated. The final 25% concentrate is dried in spray dryer to obtain dry powder of extract of vijaysar heartwood. The yield of the final dry product is 0.51 kgs. Time cycle - Extraction - 10 hours Concentration 45 minutes. @ 1-1.5 litre/minute. Spray drying 15 minutes Total 11 hours Experiment - 4 (100 kg scale) 100 kg of crushed heartwood of vijaysar is taken in the extractor fitted with reflux condenser. 500 litres of water are thereafter added to it and extractor is bolted. The mixture is boiled and refluxing carried out for 5 hours. After 5 hour of extraction, the mixture is filtered and sent for vacuum concentration in wiped film evaporator. In the meantime 500 litres of water are once again added to the already extracted material and the mixture again boiled under refluxing conditions for 5 more hours. The extract from the extractor is again filtered and sent for vacuum concentration in wiped film evaporator at 50°C and 100 mm of Hg (reduced pressure). The total volume of the filtrate from two water extractions is about 900 litres and hold up is 1:1 i.e. about 100 litres. The filtrate contains about 1% solids as water solubles. The concentration of these water solubles is increased to 25% i.e. about 860 litres of the water is evaporated, leaving concentrated mixture of about 40 litres. The remaining concentrate is spray dried to yield dry powder of aqueous extract of vijaysar. The yield of the final dry product is 10.55 kgs. Time cycle - Extraction =10 hours Concentration @ 3 litre/minute = 5 hours Spray drying @ 10 lit./Hr. = 3 hours Total = 18 hours Experiment - 5 (100 kg scale) 100 kg of crushed heartwood of vijaysar is taken in the extractor fitted with reflux condenser. Thereafter 600 litres of water are added to it and extractor is bolted. The mixture is boiled and refluxing carried out for 5 hours. After 5 hour of extraction, the mixture is filtered and sent for vacuum concentration in wiped film evaporator. In the meantime 600 litres of water are once again added to the already extracted material and similarly the mixture is again boiled under refluxing conditions for 5 more hours. The second extract from the extractor is filtered and sent for vacuum concentration in wiped film evaporator at 65°C and 200 mm of Hg (reduced pressure). The total volume of the filtrate from two water extractions is about 1100 litres and hold up is 1:1 i.e. about 100 litres. The filtrate contains about 1% solids as water solubles. The concentration of these water solubles is increased to 25% i.e. about 1060 litres of the water is evaporated, leaving concentrated mixture of about 40 litres. The remaining concentrate is spray dried to yield dry powder of aqueous extract of vijaysar. The yield of the final dry product is 10.50 kgs. Time cycle - Extraction =10 hours Concentration @ 3 litre/minute = 6 hours Spray drying @ 10 lit./Hr. = 3 hours Total = 19 hours The wood to water ratio of 1:5 and Extraction time of 5 hours were obtained after optimizing these two parameters on both 5 kg and 100 kg. scale with respect to total quantity of dry extract obtained. ADVANTAGES OF OUR PROCESS 1. The total time of Extraction, concentration under vacuum and spray drying for 100 kg batch is 18 hours only. 2. For two Extractions, wood to water ratio of only 1:10 is used. And there is practically no steam wastage, as all the processes are carried out under closed conditions. 3. There is a lot of energy saving in this process. 4. Concentration under vacuum saves time and energy costs. 5. Spray drying makes final product uniform with pleasing brown colour. It also saves time and therefore the cost. 6. The Quality and bioactivity of the final dry product as determined by HPLC is at par with that obtained by the conventional process. (,TABLE - I to 4, Figure- I & II.) Quality Control Parameters of Spray Dried and Conventional extracts of Vjjaysnr Heart Wood (Table Removed) Table 1 & 2. Hypoglycaemic activity of Vijaysar extract prepared by conventional method and spray drying method II (525mg/kg P.o) in 18 hr fasted rats. Absorption at 505 wavelength Vijaysar (525mg/kg wt.) conventional (Table Removed-I) Vijaysar Spray dryied sample II (525 rug/kg wt.) (Table Removed-II) Table 3 & 4. Hypoglycaemic activity of Vijaysar extract prepared by conventional method and spray drying method (525mg/kg P.o) in glucose loaded rats Vijaysar (525mg/kg wt.) conventional (Table Removed-III) Vijaysar Spray dryied sample II (525 mg/kg wt. ) (Table Removed-IV) We claim 1. An improved process for the production of dry aqueous extract of pterocarpus marsupium heartwood, consisting of the following steps: a) crushing of the pterocarpus marsupium (vijaysar) heart wood into wood chips, b) extracting the wood chips twice successively with water under refluxing conditions in the minimum ratio of 1:5, for a period of 5 hours each in a closed extractor with reflux condenser, c) filtering each water extract., d) concentrating the filtrate in wiped film evaporator under vacuum at temperature ranging from 35°C , 65°C, ,under reduced pressure ranging from 40-200 mg of Hg, e) drying the concentrate by spray drying method to obtain the aqueous extract in powder form and standardizing the product by HPLC profile . 2. A process as claimed in claim 1 of the present invention, concentration of the filtrate from the extractor is carried out under vacuum in wiped film evaporator at 50°C and 100 mm of Hg (reduced pressure). 3. A process as claimed in claims 1-2, of the present invention, spray diying is carried out in a spray dryer at chamber temperature of 160-170°C. 4. A process as claimed in claims 1-3, of the present invention, the total processing time for 5 kg batch is 11 hours and that for 100kg batch is 18 hours. 5. A process as claimed in claims 1-3 wherein the product obtained by the process has Methanol soluble extractive 63.31%w/w, water soluble extractive 89.86 % w/w, loss on drying 9.64 % w/w and ash value 4.0 % w/w. 6. An improved process for the production of dry aqueous extract of Vijasar (pterocarpus marsupium), substantially as her described with reference to the examples and drawings accompanying this specification.

Full Text

The present invention relates to an improved process for the production of dry aqueous extract of vijaysar heartwood (Petrocarpus marsupium).
The present invention particularly relates to an economic process for the preparation of stable dry powder from aqueous extract of heartwood of Bijasar (Pterocarpus marsupium) by standardised extraction, concentration and spray drying techniques using minimum quantity of water and optimizing heat load and time of extraction of the said process.
Pterocarpus marsupium Roxb. (N.O. Leguminoseae) the Indian Kino tree, indigenously known as Vijaysar, Bija, Bijasar, Pitasal, Piyasal etc. is a large deciduous tree of central and South India and Srilanka, extending northwards as far as the hills of Bihar, Binda and Kumaon Terai. The tree yields the gum kina and its wood contains a dye soluble in water, having a blue flourescence.
It was a popular belief that watery extract of the wood is cure for diabetes. Some medical practitioners maintain that the sugar content of the urine is reduced by drinking water from vessels of vijaysar. Vessels made of vijaysar have a popular reputation for transferring to their contents anti diabetic qualities (Trotter - The common commercial Timber of India and their uses, 156, 1944).
Ojha, K.N et. al. [Ojha, K.N., Pabrai, Paramjit R. and Venkatachalam, K., Indian J. Pharmacology II, 188 (1949)] have reported that aqueous extract of Pterocarpus marsupium Roxb. given orally is effective in lowering blood sugar in rabbits as well as in diabetic patient, without any toxic symptoms.
Seshadri (Seshadri, T.R. Phytochemistry 11, 881 (1972)) has reported Pterocarpus marsupium to be rich source of Polyphenolic
compounds. Various researchers have isolated a number of compounds from extracts of Pterocarpus marsupium. Some of them are as follows: Stilbene, pterostilbene (Mathew, J., Subba Rao, A.V., and Subba Rao, N.V., Current Sci., 46, 337 (1997)); the sesquiterpene alcohols, (3-eudesmol, triterpene alcohol, erythrodiol-3-monoacetate [Adinarayana, D., Syamadunder, K.V., Phytochemistry, 21, 1083 (1982)]; catechin, epicatechin [Chakravarthy, B.K., Gupta, S., Gambir, S.S., and Gode, K.D., Life Sci, 29, 2043 (1981)]; the flavonoids, pseudobaptigenin liquiritigenin, garbanzol, 5-deoxykaempferol, chalcone, isoliquiritigenin, dihydrochalcone.pterosuprin and aromatic aldehyde, p-hydroxybenzaldehyde [Adinarayana, D., Syamasunder, K.V., Seliqmann, O., and Wagner, H, Z. Naturforsch 37C, 145 (1982)]; the isoflavonoid glycol, marsupol (4,4' dihydroxy-L-methylthydro benzoin) [ Subba Rao, A.V., and Mathew, J., Phytochemistry, 21, 1837 (1982)]; pterocarpols A and B [Bhargava, P.N. Proc. Ind. Acad. Sci. 24, 496 (1946)] and other phenolic compounds from extract of heart wood of P. marsupium (Maurya, R., Ray, A.B., J. of Natural Product Vol.-4 179-181 (1984).
The process for production of aqueous extract of vijaysar (Pterocarpus marsupium) known for centuries is still being used commercially.(Caraka Samhita of Agnivesa, 194 A.D.)
This process involves cutting of vijaysar heartwood, slicing the same and crushing it to 25-50 mm length with 5-10 mm width/height. The crushed wooden pieces are put in the open pan type steam extractor and 16 times water is added to these wooden chips. The mixture is heated by steam in the jacket or by direct fire and concentrated, until the volume of the mixture is reduced to % of its original volume. The concentrated mixture is filtered in ordinary filters and the filtrate is further concentrated in electrically heated vessels until, bone dry product is obtained. The total dry, water
soluble extract obtained is around 8% of the crushed mass of the wood. And it takes around 72 hours for a batch of 100 kg of crushed wood to produce 8 kg of the product.
Dry aqueous extract of vijaysar obtained from the above cited method, is only product known in Ayurveda. The time of extraction is very long and yield of the product thus obtained is low. The steam/electricity consumption is also very high.
Further following disadvantages have been observed in the process described in the prior art.
1. The process involves boiling wood and water in the ratio of 1:16
and then concentrating the same to % of its original volume,
making the process energy intensive with lot of wastage of
steam/vapour in open pan.
2. Drying/further concentration step in electrically heated vessels
is also energy intensive and the drying is not uniform. The final
texture of the product is also dark brown.
3. Some of the bioactive constituents are likely to be lost or
damaged with some loss of bioactiviety as a net result.
Whereas, in the present invention authors have used novel, extraction with refluxing, vacuum concentration, and spray drying method, thereby reducing time of processing to 18 hours and consequent reduction in steam consumption and increasing the yield from 8% to 10.5%.
The novelty of this invention resides in the use carrying out only two extractions of 5 hour each of the crushed heart wood with water, using wood:water ratio of 1:5 only, in each
extraction. The extraction system is fully closed with reflux
condenser.
There has been no improvement in the process described in the
literature ever since.
The main objective of the present invention is to provide a faster
and an economic process for the production of dried aqueous
extract of vijaysar heartwood.
The another objective is to concentrate the extract under vacuum, filtering and spray drying the material into a uniform powder.
Yet another objective is to get powder having uniform hue and is stable at ambient temperature. Still another objective is to make the process cost effective and easy to operate, while retaining the original bioactivity.
Accordingly the present invention provides an improved process for the production of dry aqueous extract of pterocarpus marsupium heartwood, consisting of the following steps:
a) crushing of the pterocarpus marsupium (vijaysar) heart wood
into wood chips,
b) extracting the wood chips twice successively with water under
refluxing conditions in the minimum ratio of 1:5, for a period of
about 5 hours each in a closed extractor with reflux condenser,
c) filtering each water extract.,
d) concentrating the filtrate in wiped film evaporator under
vacuum at temperature ranging from 35°C- 65°C under reduced
pressure ranging from 40-200 mg of Hg,
e) drying the concentrate by spray drying method to obtain the
aqueous extract in powder form and standardizing the product
by HPLC profile .
The total processing time for 5 kg batch is 11 hours and that for 100kg batch is 18 hours.
In an embodiment of the present invention the extraction may be carried in closed extractor with reflux condensers having wood to water ratio of 1:5 and time of each extraction as five hours.
In another embodiment the concentration of the filtrate may be carried out in vacuum operated wiped film evaporator.
In yet another embodiment the spray drying may be carried out in a spray dryer at chamber temperature of 160-170°C. The present invention provides an improved and economic process for the production of aqueous extract of vijaysar heartwood, which comprises of crushing the heart wood in chips, followed by two water extractions of wood chips in water in the ratio of 1:5 under re fluxing condition for 5 hours each, concentration of the filtrate from extraction in vacuum operated, wiped film evaporator and spray drying the concentrate to get dry powder of extract.
The process of the preparation of dry powder of aqueous extract of vijaysar heart wood (Pterocarpus marsupium) is described in detail as given below which is provided by way of examples for illustrations only and therefore should not be construed to limit the scope of the present invention.
Experiment-1 ( 5 kg scale )
5 kgs of crushed vijaysar heartwood is mixed with 25 litres of water in an extractor fitted with reflux condenser. The mixture is brought to the boiling temperature and refluxed for 5 hours. After this the water extract is (drained and filtered and sent to wiped film evaporator for concentration under vacuum. In the mean time 25 litres of fresh water are added to the already extracted vijaysar heartwood chips. The contents are once again boiled and refluxed for 5 hours. After draining and filtration the filtrate is taken to wiped film evaporator for vacuum concentration. In vacuum evaporator, concentration of filtrate is carried out at around 35°C and 40 mm of Hg (reduced pressure).
The total volume of filtrate from two water extractions is about 45 litres as 5 litres is hold-up in the crushed wood. This 45 litres contains about 0.5 kg ( i.e.about 1%) of water solubles. The concentration of this lean mixture is increased to about 25-30% i.e. out of 45 litres, approximately 43 litres of water are evaporated. The final 25% concentrate is dried in spray dryer to obtain dry powder of extract of vijaysar heartwood. The yield of the final dry product is 0.50 kgs.
Time cycle - Extraction - 10 hours
Concentration 45 minutes.
@ 1-1.5 litre/minute.
Spray drying 15 minutes
Total 11 hours
Experiment-2 ( 5 kg scale )
5 kgs of crushed vijaysar heartwood is mixed with 25 litres of water in an extractor fitted with reflux condenser. The mixture is brought to the boiling temperature and refluxed for 5 hours. After this the water extract is drained and filtered and sent to wiped film evaporator for concentration under vacuum. In the meantime 25 litres of fresh water are added to the already extracted vijaysar heartwood chips. The contents are once again boiled and refluxed for 5 hours. After draining and filtration the filtrate is taken to wiped film evaporator for vacuum concentration. In vacuum evaporator, concentration of filtrate is carried out at around 50°C and 100 mm of Hg (reduced pressure).
The total volume of filtrate from two water extractions is about 45 litres as 5 litres is hold-up in the crushed wood. This 45 litres contains about 0.5 kg (i.e.about 1%) of water solubles. The concentration of this lean mixture is increased to about 25-30% i.e. out of 45 litres, approximately 43 litres of water are evaporated. The final 25% concentrate is dried in spray dryer to obtain dry powder of extract of vijaysar heartwood. The yield of the final dry product is 0.52 kgs.
Time cycle - Extraction - 10 hours
Concentration 45 minutes.
@ 1-1.5 litre/minute.
Spray drying 15 minutes
Total 11 hours
Experiment-3 ( 5 kg scale )
5 kgs of crushed vijaysar heartwood is mixed with 25 litres of water in an extractor fitted with reflux condenser. The mixture is brought to the boiling temperature and refluxed for 5 hours.
After this the water extract is drained and filtered and sent to wiped film evaporator for concentration under vacuum. In the meantime 25 litres of fresh water are added to the already extracted vijaysar heartwood chips. The contents are once again boiled and refluxed for 5 hours. After draining and filtration the filtrate is taken to wiped film evaporator for vacuum concentration. In vacuum evaporator, concentration of filtrate is carried out at around 65°C and 200 mm of Hg (reduced pressure).
The total volume of filtrate from two water extractions is about 45 litres as 5 litres is hold-up in the crushed wood. This 45 litres contains about 0.5 kg (i.e.about 1%) of water solubles. The concentration of this lean mixture is increased to about 25-i.e. out of 45 litres, about 43 litres of water are evaporated. The final 25% concentrate is dried in spray dryer to obtain dry powder of extract of vijaysar heartwood. The yield of the final dry product is 0.51 kgs.
Time cycle - Extraction - 10 hours
Concentration 45 minutes.
@ 1-1.5 litre/minute.
Spray drying 15 minutes
Total 11 hours
Experiment - 4 (100 kg scale)
100 kg of crushed heartwood of vijaysar is taken in the extractor fitted with reflux condenser. 500 litres of water are thereafter added to it and extractor is bolted. The mixture is boiled and refluxing carried out for 5 hours. After 5 hour of extraction, the mixture is filtered and sent for vacuum concentration in wiped film evaporator. In the meantime 500 litres of water are once again added to the already extracted material and the mixture again boiled under refluxing conditions for 5 more hours.
The extract from the extractor is again filtered and sent for vacuum concentration in wiped film evaporator at 50°C and 100 mm of Hg (reduced pressure).
The total volume of the filtrate from two water extractions is about 900 litres and hold up is 1:1 i.e. about 100 litres. The filtrate contains about 1% solids as water solubles. The concentration of these water solubles is increased to 25% i.e. about 860 litres of the water is evaporated, leaving concentrated mixture of about 40 litres. The remaining concentrate is spray dried to yield dry powder of aqueous extract of vijaysar. The yield of the final dry product is 10.55 kgs. Time cycle -
Extraction =10 hours
Concentration @ 3 litre/minute = 5 hours
Spray drying @ 10 lit./Hr. = 3 hours
Total = 18 hours
Experiment - 5 (100 kg scale)
100 kg of crushed heartwood of vijaysar is taken in the extractor fitted with reflux condenser. Thereafter 600 litres of water are added to it and extractor is bolted. The mixture is boiled and refluxing carried out for 5 hours. After 5 hour of extraction, the mixture is filtered and sent for vacuum concentration in wiped film evaporator. In the meantime 600 litres of water are once again added to the already extracted material and similarly the mixture is again boiled under refluxing conditions for 5 more hours.
The second extract from the extractor is filtered and sent for vacuum concentration in wiped film evaporator at 65°C and 200 mm of Hg (reduced pressure).
The total volume of the filtrate from two water extractions is about 1100 litres and hold up is 1:1 i.e. about 100 litres. The filtrate contains about 1% solids as water solubles. The concentration of
these water solubles is increased to 25% i.e. about 1060 litres of the
water is evaporated, leaving concentrated mixture of about 40 litres.
The remaining concentrate is spray dried to yield dry powder of
aqueous extract of vijaysar. The yield of the final dry product is 10.50
kgs.
Time cycle -
Extraction =10 hours
Concentration @ 3 litre/minute = 6 hours
Spray drying @ 10 lit./Hr. = 3 hours
Total = 19 hours
The wood to water ratio of 1:5 and Extraction time of 5 hours were obtained after optimizing these two parameters on both 5 kg and 100 kg. scale with respect to total quantity of dry extract obtained. ADVANTAGES OF OUR PROCESS
1. The total time of Extraction, concentration under vacuum and
spray drying for 100 kg batch is 18 hours only.
2. For two Extractions, wood to water ratio of only 1:10 is used.
And there is practically no steam wastage, as all the processes
are carried out under closed conditions.
3. There is a lot of energy saving in this process.
4. Concentration under vacuum saves time and energy costs.
5. Spray drying makes final product uniform with pleasing brown
colour. It also saves time and therefore the cost.
6. The Quality and bioactivity of the final dry product as
determined by HPLC is at par with that obtained by the
conventional process. (,TABLE - I to 4, Figure- I & II.)
Quality Control Parameters of Spray Dried and Conventional extracts of Vjjaysnr Heart Wood

(Table Removed)

Table 1 & 2. Hypoglycaemic activity of Vijaysar extract prepared by conventional method and spray drying method II (525mg/kg P.o) in 18 hr fasted rats.
Absorption at 505 wavelength Vijaysar (525mg/kg wt.) conventional

(Table Removed-I)

Vijaysar Spray dryied sample II (525 rug/kg wt.)

(Table Removed-II)

Table 3 & 4. Hypoglycaemic activity of Vijaysar extract prepared by conventional method and spray drying method (525mg/kg P.o) in glucose loaded rats
Vijaysar (525mg/kg wt.) conventional

(Table Removed-III)

Vijaysar Spray dryied sample II (525 mg/kg wt. )

(Table Removed-IV)

We claim
1. An improved process for the production of dry aqueous extract
of pterocarpus marsupium heartwood, consisting of the
following steps:
a) crushing of the pterocarpus marsupium (vijaysar) heart wood
into wood chips,
b) extracting the wood chips twice successively with water under
refluxing conditions in the minimum ratio of 1:5, for a period of
5 hours each in a closed extractor with reflux condenser,
c) filtering each water extract.,
d) concentrating the filtrate in wiped film evaporator under
vacuum at temperature ranging from 35°C , 65°C, ,under
reduced pressure ranging from 40-200 mg of Hg,
e) drying the concentrate by spray drying method to obtain the
aqueous extract in powder form and standardizing the product
by HPLC profile .
2. A process as claimed in claim 1 of the present invention,
concentration of the filtrate from the extractor is carried out
under vacuum in wiped film evaporator at 50°C and 100 mm of
Hg (reduced pressure).
3. A process as claimed in claims 1-2, of the present invention,
spray diying is carried out in a spray dryer at chamber
temperature of 160-170°C.
4. A process as claimed in claims 1-3, of the present invention, the
total processing time for 5 kg batch is 11 hours and that for
100kg batch is 18 hours.
5. A process as claimed in claims 1-3 wherein the product
obtained by the process has Methanol soluble extractive
63.31%w/w, water soluble extractive 89.86 % w/w, loss on
drying 9.64 % w/w and ash value 4.0 % w/w.

6. An improved process for the production of dry aqueous extract
of Vijasar (pterocarpus marsupium), substantially as her described with reference to the examples and drawings accompanying this specification.

Documents:

200-del-2002-abstract.pdf

200-del-2002-claims.pdf

200-del-2002-correspondence-others.pdf

200-del-2002-correspondence-po.pdf

200-del-2002-description (complete).pdf

200-del-2002-drawings.pdf

200-del-2002-form-1.pdf

200-del-2002-form-18.pdf

200-del-2002-form-2.pdf

200-del-2002-form-3.pdf

« Previous Patent

Next Patent »

Patent Number

231018

Indian Patent Application Number

200/DEL/2002

PG Journal Number

13/2009

Publication Date

27-Mar-2009

Grant Date

28-Feb-2009

Date of Filing

07-Mar-2002

Name of Patentee

COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH.

Applicant Address

RAFI MARG, NEW DELHI-110001. INDIA.

Inventors:

#	Inventor's Name	Inventor's Address
1	GHULAM NABI QAZI	REGIONAL RESEARCH LABORATOUS, CANEL ROAD, JAMMU-TOUR, INDIA.
2	CHUNI LAL TIKOO	REGIONAL RESEARCH LABORATOUS, CANEL ROAD, JAMMU-TOUR, INDIA.
3	VIRENDER KUMAR KAUL	REGIONAL RESEARCH LABORATOUS, CANEL ROAD, JAMMU-TOUR, INDIA.
4	SUMAN KAUL	REGIONAL RESEARCH LABORATOUS, CANEL ROAD, JAMMU-TOUR, INDIA.
5	OM PRAKASH SURI	REGIONAL RESEARCH LABORATOUS, CANEL ROAD, JAMMU-TOUR, INDIA.
6	KASTURI LAL BEDI	REGIONAL RESEARCH LABORATOUS, CANEL ROAD, JAMMU-TOUR, INDIA.
7	RAVINDER KUMAR RAINA	REGIONAL RESEARCH LABORATOUS, CANEL ROAD, JAMMU-TOUR, INDIA.

PCT International Classification Number

A61Q 19/10

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA