Title of Invention

PROCESS FOR CONVERSION OF CRUDE LIQUID LECITHIN INTO AN ANTI-FREEZE STANDARDIZED LIQUID LECITHIN

Abstract A process for producing Phosphatidyl Choline - 70 % from liquid lecithin comprising following steps: a) subjecting liquid (crude) lecithin with organic solvent in a cylindrical mixer at room temperature with revolution per minute ranging from 150 - 300; . Add aqueous solution of Magnesium Sulfate ( 8 -15 % ) in alcohol soluble material b) decanting the mixture of solvent and Phosphatidyl Choline rich fraction. c) draining reffinate material containing Phosphatidyl ethanolamine and Phosphatidyl inositol rich fraction and subjecting to multiple chilled acetone extraction to get powdered lecithin; d) filtering methanol - Phosphatidyl Choline Rich fraction in a multiple filter to remove . fine particles; e) distilling the mixture of solvent and Phosphatidyl Choline Rich fraction at 65 to 70°C at a vacuum of 70 to 750 millimeter of mercury to recover the solvent from mixture; f) cooling at room temperature Phosphatidyl Choline, the product obtained after distillation under vacuum of 750 millimeter of mercury: g) packing the powdered Phosphatidyl Choline under asceptic conditions.
Full Text FORM 2
THE PATENTS ACT, 1970
COMPLETE SPECIFICATION (SECTION 10)
THE PROCESS OF MANUFACTURE OF PHOSPHATIDYL CHOLINE 70 % FROM CRUDE LIQUID LECITHIN
SONIC BIOCHEM EXTRACTIONS LTD., A Limited Company registered under the Companiec Act, 1956, having its office at 38, Patel Nagar, Indore, Madhya Pradesh, India, PIN 452 001.
The following specifications particularly describe the nature of this invention and the manner in which it is to be performed:-
Characteristic: Deoiled, wax like, Solid plastic, yellowish brown
Composition : Mixture of Phospho & glycolipids
Acid Value: 1 KOH/g max
Moisture : 1 % max
Peroxide Value : 1 meq max
Phosphatidyl Choline : Min 70 %
Phosphorus : 3 - 4 %



589/MUM/2006
13/4/2006


This invention relates to a process of extraction of Phosphatidyl Choline 70 % from Crude Liquid Lecithin, more particularly the extraction of Phosphatidyl choline 70 % rich fraction from Crude Liquid Lecithin which is derived from vegetable oil sources like Soyabean, Cotton seed, Rapseed, Corn, Rice Bran, Sunflower seeds, Peanuts etc. Soyabean is a natural crop having multipurpose uses for human beings, It had its origin in China and was developed in India around 1965. Soyabean was primarily developed and grown in India for its high oil content and its uses in improving nitrogen content of land. The crops had a fast growth and the major portion is grown in M.P. accounting for 70% of India's production and rest developed in Rajasthan and Vidharbh area of Maharashtra. The size of the crop is around 70 lacs tons per year, which yields around 13 lacs tons of Soyabean oil.
Soyabean is a natural boon to humanity, it contains oil, proteins, phospholipids, Vitamin E (Tocopherol) and polyunsaturated fatty acids. Till now conventionally in India, Soyabeans are being used mainly for oil extraction and deoiled cake production. Gums and sludge produced during oil refining are not used for any value addition although these contain valuable fractions like Lecithin, Phospholipids.
Our R&D unit has developed the process and the technology of extraction of Phosphatidyf Choline from liquid lecithin derived for Soyabean oil gums.

Lecithin is a group of naturally occurring phospholipids that's found in nearly every living cell. Though the word lecithin is derived from the Greek term lekkithos meaning "yolk of an egg", the primary commercial source of lecithin is Soyabean.
Lecithin is widely used in manufactured food, feed and pharmaceutical, cosmetic and industrial applications such as crystal formation and antidusting, modifying, emulsilying, dispersing, wetting, penetrating & antioxidising properties.
Lecithin is a naturally occurring group of phospholipids, which are important constituents of cell membrane and polyunsaturated fatty acids.
The typical composition of phospholipids and fatty acids in lecithin is as under: -
A) Phospholipids:
1) Phosphatidyl Choline (PC) -23%
2) Phosphatidyl Ethenolamine (PE) - 20%
3) Phosphatidyl Inositol (PI) -14%
4) Phosphotidic Acid (PA) -5%
5) Phosphatidyl Serine (PS) -0.2%
B) Fatty Acid in Soyabean Lecithin:
1) MyristicAcid - 1.5%
2) Palmitic Acid - 18.9%
3) Palmito Oleic Acid - 8.6%-
4) Stearic Acid - 3.9%
5) Oleic Acid - 9.8%
6) LinoleicAcid - 20%
7) Linolenic Acid - 2.5%
8) Arachidic Acid - 2.1%
The constitutional formula of Phosphatidyl Choline is as under:-



Lecithin also contains natural antioxidant as Tocopherol and hence acts as a good antioxidant particularly because of its ability to complex heavy metals.
Phosphatidyl Choline is an important constituent of all human cells. As such it plays an important role in the pathophysiology of human disease. The adult human ingests 300 - 1000 mgs. of choline per day.
In adult tissue choline levels are significantly increased following ingestion of a choline or lecithin supplemented meal. Choline deficiency has major consequences for many species of animals. It is associated with fatty infiltration liver in the baboon, rat dog, hamster, pig & chicken. Renal function may also be impaired due to membrane lecithin deficiency; Choline deficient animals have abnormal memory, free water absorption, renal plasma flow and gross renal hemorrhaging. Choline deficiency in animals has also been associated with infertility, growth retardation and body abnormalities.
Malnourished humans have very low choline concentration in plasma. Supplemental choline can also influence organ function by increasing availability of Choline above normal levels. Choline is a acetyl choline precursor. It is involved in lipid metabolism and acts as methyl doner in various other metabolic processes. Choline has traditionally been considered to be a Vitamin B substance. Acetylcholine is essential for proper brain function. In the brain, choline stimulates the production of Acetylcholine, a neurotransmitter. Neurotransmitters are the chemical messengers that conduct information through the nervous systems bridging the gap between individual neurons and muscle cell. Neurons, tiny nerve cells, control every aspect of behaviour including mood, memory, thought, speech sensation and movement. It is not clear what area acetylcholine targets, but the nervous systems cannot function properly without a sufficient amount of it. Choline obtained from lecithin source enhances operation of the brain and stimulates the brain cells to produce more acetylcholine.

Fledging research indicates that the choline from lecithin source may be able to boost memory and counter act depression and dementia traced to deficiency of acetylcholine. Starting results were achieved using choline rich lecithin to treat Tardive Dyskinesia, a disabling brain disorder caused by failure of the brain cells to release acetylcholine.
In addition, a study sponsored by Food & Drug Administration (FDA), USA found that taking large dosage of choline chloride or Bitartarate (synthetic product) can lead to nausea, vomiting, salivation, sweating and anorexia and the straight choline was only effective for a short time. Phosphatidyl choline had none of these side effects and proved to be longer acting resistant to bacterial attach and easier to tolerate. Choline deficiency for prolonged periods also lead to hepato carcinomas, a cancer. "FDA authorize claim for Phosphatidyl Choline as Newest Vitamin"
Phosphatidyl choline can be used to treat fatty liver and cirrhosis. It can also be used in the treatment of dementia & in various extra pyramidal disorders
According to this invention the process of producing Phosphatidyl choline - 70 % from crude liquid lecithin comprises following steps.
1) Subjecting liquid (crude) lecithin to requisite amount of solvent in a specially designed
mixer in presence of metallic salts like Magnesium. Calcium, Aluminium & Cadmium etc. The
solvent is aliphatic alcohols having 1 to 4 carbon atoms The preferred solvent is methanol. The
methanol needs to be dry enough to achieve maximum extraction of Phosphatidyl choline
fraction from lecithin. The moisture content or solvent ranges from 0-4%. The moisture content
below 1 % is preferable.
2) Solvent and liquid lecithin ratio plays important role in extraction. The ratio of solvent to lecithin can be 5:1. The preferred ratio being 3:1 and 4:1
3) The extraction is carried out in cylindrical mixer having rpm ranging from 200 to 1000 rpm. The preferred rpm being 150 - 300 rpm. The extraction can be carried out at room temperature or 30 - 35°C per hour. For better extraction elevated temperature upto 45°C also proves helpful. Add aqueous solution of Magnesium Sulfate ( 8 -15 % ) in alcohol soluble material ( 0.35 - 0.40 gm MgS04 ) per gram Phosphatide. Chemical Stirring is done for an hour and is then settled for three hours and then separated.

4) Extracted solvit & Phosphatidyl choline rich fraction ( top layer ) is decanted into distillation vessel- The reffinate material, which contains Phosphatidyl Ethanolamine & Phosphatidyl inositol rich fraction is then drained and subjected to multiple chilled acetone extraction to get powdered lecithin.
5) The extracted solvent mixture is then distilled at a temperature of 65 - 70°C at a vacuum of 700 - 750 mm of mercury to recover methanol from the extracts. The methanol choline extract is filtered through a special sparkler filter prior to distillation to remove particulate, if any-
6) Distilled material is then washed with water and acetone in the ratio of 1 ;0.5 : 0.5

7) Emulsion of precipitated top layer is then washed with acetone till it becomes oil free. Usually 2-3 washes are needed. Bottom layer contains acetone and water is also distilled to recover acetone.
8) Having washed with acetone, the top layer obtained, contains acetone and oil and is subjected to regular distillation.
9) Precipitate at the bottom is vacuum dried, to obtain the final product.
10) Phosphatidyl choline so obtained is then cooled and packed in HDPE drums under
asceptic conditions.
The Phosphatidyl choline - 70 % thus obtained meets the following specifications:-
Characteristic: Deoiled, wax like, Solid plastic, yellowish brown
Add Value : 1 KOH / q max
Moisture : 1 % max
Peroxide Value : 1 meq max
Phosphatidyl Choline : Min 70 %
Phosphorus : 3 - 4 %

Prior Art. IN 180994 states :
The invention will now be described in greater details giving the various steps of process of the lecithin from the crude lecithin. The crude liquid lecithin from Soyabean oil refineries is fed to a cylindrical mixer, which contains solvent. The proper solvent to lecithin ratio is maintained to achieve maximum extractions of Phosphatidyl choline from lecithin without extracting other phospholipids, like Phosphatidyl ethanolamine and Phosphatidyl inositol. The speed of the rotation of mixing blade is critical. The more the speed more will be the extraction of undesirable phospholipids. The rpm of rotating blades of 550-600 rpm was found to be optimum. The blades were specially designed having perforation in the vanes, to achieve intimate mixing and optimum extraction. The mixing impeller has four blades welded at right angles, each having holes in it.
The moisture content of solvent is also important factor here. The moisture content below 1% is preferable. Methanol solvent is therefore dried through anhydrous sodium sulphate column to achieve desirable dryness. The ratio of solvent to lecithin is maintained at 3:1. Lower solvent ratio leads to lesser extraction of Phosphatidyl choline and longer extraction time The raised temperature extraction upto at 45°C reduces the extraction time. Extraction at a temperature of 30-35°C for 1 hour give optimum recovery of Phosphatidyl choline.
The solvent and Phosphatidyl choline rich lecithin mixture is then siphoed out in a distillation vessel. The raffinate material, which is rich in Phosphatidyl inositol and Phosphatidyl ethanolamine is then drained and converted into powder by multiple extraction with chilled acetone.
The excluded solvent mixture is distilled at 65-70 C at vacuum of 700-750 mm of mercury to recover methanol without damaging colour and flavour of the Phosphatidyl choline. It is important to filter to methanol extract in a sparkler filter having multiple filters of 100 mesh to remove the fine particles. The product obtained after distillation is cooled to room temperature under vacuum of 750mm of mercury and packed under asceptic conditions.
Example:
Process for enriching the Phosphatidyl Choline from mixture of Phosphatides
Phosphatides mixture mainly have Phosphatidyl Choline,Phosphatidyl
Ethanolamine,Phosphatidyl Inositol and Phosphatidic acid with 40 % oil admixing with solvent

-The soluble part of the product have Phosphatidyl Choline, Phosphatidyl Ethanolamine,Phosphatidyl Inositol and oil. The insoluble part have Phosphatidyl.Ethanolamine Phosphatic acid, and oil.
The separation of soluble & insoluble is depends on proper time of setting & solvent taken like Methanol Isopropanol Ethanol etc.The influence can be clearly seen of the water content in the solvent on the distribution of the accompanying triglycerides between soluble and insoluble fractions.
Experiment 01.
1. Take 100gm. Of alcohol soluble material in 500 ml methanol & stirr it. ( 50-100 RPM).
2. Add aq. Solution of magnesium sulfate ( 8 %) in alcohol soluble materiaf ( 0.35 gm Mg So4 Per gram phosphatides )
3. Stirr for one hour and separate the precipitate by centrifuge.
4. Filtered material is distilled under vacuum.
5. Wash tine acetone, precipitate are separated out, Dry it under vacuum.
6. Check yield & % of Phosphatidyl Choline on HPLC.
Initial Phosphatidyl Choline After treatment with Methanol /
] MgSo4= Phosphatidyl Choline%
35% : 67% I
Experiment 02.
1. Take 100gm. Of alcohol soluble material in 300 ml methanol & stirr it. (150-300 RPM) 1 Hr
2. Add aq. Solution of magnesium sulfate (15%) in alcohol soluble material { 0.40 gm Mg So4 Per gram phosphatides)
3. Settle material tor 3 hours and separate.
4. Take top layer and distill under vacuum.
5. Distilled material is washed with acetone & water (1:1)
6. Emulsion is formed on top layer of solution.
7. In bottom layer, acetone and water are separated out.
8. Emulsion is washed with pure acetone 2-3 times.
9. Bottom precipitate are separated out and dried under vacuum.
10. Check yield & % of Phosphatidyl Choline on HPLC.
Initial Phosphatidyl Choline After treatment with Methanol &
MgSQ4= Phosphatidyl Choline%
35% I 72% I

CONCLUSION :-
1. Temp, is not playing important role.
2. Water contents enrich the phosphatidyl choline % but yield is effected.
3. Distillation is done under vacuum.
4. Material separations is an important step.
5. phosphatidyl choline % is higher with 95 % Ethanol. Methanol and Isopropanol solvent are not so effective.
In this process, high efficiency chillers and efficient solar heating system is used to maintain operating parameters.

WE CLAIM
1. A process for producing Phosphatidyl Choline - 70 % from liquid lecithin comprising
following steps:
a) subjecting liquid (crude) lecithin with organic solvent in a cylindrical mixer at room temperature with revolution per minute ranging from 150 - 300; . Add aqueous solution of Magnesium Sulfate ( 8 -15 % ) in alcohol soluble material
b) decanting the mixture of solvent and Phosphatidyl Choline rich fraction.
c) draining reffinate material containing Phosphatidyl ethanolamine and Phosphatidyl
inositol rich fraction and subjecting to multiple chilled acetone extraction to get
powdered lecithin;
d) filtering methanol - Phosphatidyl Choline Rich fraction in a multiple filter to remove
. fine particles;
e) distilling the mixture of solvent and Phosphatidyl Choline Rich fraction at 65 to 70°C
at a vacuum of 70 to 750 millimeter of mercury to recover the solvent from mixture;
f) cooling at room temperature Phosphatidyl Choline, the product obtained after distillation under vacuum of 750 millimeter of mercury:
g) packing the powdered Phosphatidyl Choline under asceptic conditions.
2. A process of producing Phosphatidyl Choline - 70 % as claimed in claim (1), wherein the
organic solvent is selected from aliphatic alcohol having 1 to 4 carbon atoms; preferably
methanol.
3. A process of producing Phosphatidyl choline as claimed in claim (1), wherein moisture
content of the solvent is from 0 to 4% preferably below 1 %.
4. A process of producing Phosphatidyl Choline as claimed in claim (1), wherein the ratio of
solvent to liquid lecithin is 5:1 to 2:1, preferably 3:1.
5. A process of producing Phosphatidyl Choline as claimed in claim (1), wherein the
revolution per minute of cylindrical mixture is preferably from 150 - 300.
6. A process of producing Phosphatidyl Choline as claimed in claim (1), wherein the
extraction temperature is room temperature preferably below 45°C.
7. A process of producing Phosphatidyl Choline - 70 % as herein before described in this
complete specification.

11

Documents:

589-mum-2006-cancelled pages(30-12-2010).pdf

589-mum-2006-claims(13-4-2006).doc

589-mum-2006-claims(13-4-2006).pdf

589-MUM-2006-CLAIMS(AMENDED)-(30-12-2010).pdf

589-MUM-2006-CLAIMS(AMENDED)-(4-6-2010).pdf

589-mum-2006-claims(granted)-(13-1-2011).pdf

589-mum-2006-claims.pdf

589-mum-2006-correspondence(11-1-2008).pdf

589-MUM-2006-CORRESPONDENCE(4-6-2010).pdf

589-mum-2006-correspondence(ipo)-(14-1-2011).pdf

589-mum-2006-correspondence-received.pdf

589-mum-2006-description (complete).pdf

589-mum-2006-description(complete)-(13-4-2006).pdf

589-mum-2006-description(granted)-(13-1-2011).pdf

589-mum-2006-form 1(13-4-2006).pdf

589-MUM-2006-FORM 1(25-3-2010).pdf

589-mum-2006-form 18(11-1-2008).pdf

589-mum-2006-form 2(13-4-2006).doc

589-mum-2006-form 2(13-4-2006).pdf

589-mum-2006-form 2(complete)-(13-4-2006).pdf

589-mum-2006-form 2(granted)-(13-1-2011).pdf

589-mum-2006-form 2(title page)-(13-4-2006).pdf

589-MUM-2006-FORM 2(TITLE PAGE)-(30-12-2010).pdf

589-mum-2006-form 2(title page)-(complete)-(13-4-2006).pdf

589-mum-2006-form 2(title page)-(granted)-(13-1-2011).pdf

589-MUM-2006-FORM 3(25-3-2010).pdf

589-mum-2006-form-1.pdf

589-mum-2006-form-2.doc

589-mum-2006-form-2.pdf

589-MUM-2006-OTHER DOCUMENT(4-6-2010).pdf

589-MUM-2006-REPLY TO EXAMINATION REPORT(25-3-2010).pdf

589-MUM-2006-REPLY TO EXAMINATION REPORT(30-12-2010).pdf

589-MUM-2006-SPECIFICATION(AMENDED)-(30-12-2010).pdf


Patent Number 245341
Indian Patent Application Number 589/MUM/2006
PG Journal Number 03/2011
Publication Date 21-Jan-2011
Grant Date 13-Jan-2011
Date of Filing 13-Apr-2006
Name of Patentee SONIC BIOCHEM EXTRACTIONS LTD.
Applicant Address 38, Patel Nagar, Indore, Madhya Pradesh - 452 001 India. An Indian National.
Inventors:
# Inventor's Name Inventor's Address
1 SHRIKISHAN CHOITHRAM MATLANI 38, Patel Nagar, Indore, Madhya Pradesh, Pin - 452 01, India.
2 GIRISH MATLANI 38, Patel Nagar, Indore, Madhya Pradesh, Pin - 452 01, India.
PCT International Classification Number A23L1/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA