WO2014042509A1

WO2014042509A1 - Extracting lecithin from palm agro-waste

Info

Publication number: WO2014042509A1
Application number: PCT/MY2013/000067
Authority: WO
Inventors: Thang Yin MEE; Zairey Bin Mohd Zain Mohd; David Ross APPLETON; Jaril Asis Ahmad; Kulaveerasingam HARIKRISHNA A/L; Yusof@Hassan HIRZUN BIN MOHD; Bee Keat Neoh; Amiron Bin Ersad Mohd; Bin Aminuddin Junaidi
Original assignee: Sime Darby Malaysia Berhad
Priority date: 2012-09-12
Filing date: 2013-04-01
Publication date: 2014-03-20
Also published as: BR112015005292A2; CO7350650A2; IN2015DN01922A; MY161428A; CR20150157A

Abstract

The invention relates to a method of extracting lecithin from palm agro-waste produced in a palm oil mill. The method comprises the steps of introducing a palm agro-waste selected from a group consisting of separator sludge and decanter cake as a starting material; subjecting the starting material to a pre-treatment step, followed by extraction using a solvent to give an extracted meal and a solvent extract; separating the solvent extract from the extracted meal; and removing the solvent followed by precipitation to give a residue fraction comprising lecithin having a phospholipids content of not less than 20%, more preferably, not less than 35%.

Description

EXTRACTING LECITHIN FROM PALM AGRO-WASTE

FIELD OF THE INVENTION

The present invention relates to a method of extracting lecithin from palm agro-waste. More particularly, the present invention relates to a method of extracting lecithin from palm agro-waste from palm oil mill, and a composition containing the extracted lecithin. BACKGROUND

Lecithin is a yellow-brownish fatty substance found in practically any animal and plant tissues. Lecithin generally comprises of phosphoric acid, choline, fatty acids, glycerol, glycolipids, triglycerides, and phospholipids. Lecithin is sold as a food supplement and for medical uses. Commercial lecithin, as used by food manufacturers, is a mixture of phospholipids in oil.

There are different types of phospholipids and the main phospholipids in lecithin include phosphatidyl choline (PC), phosphatidyl ethanolamine (PE), phosphatidyl inositol (PI) and phosphatidic acid (PA).

Lecithin can be extracted from oil seed materials by means of solvent extraction, water degumming, and enzymatic degumming. Lecithin is currently produced commercially from soybeans and egg yolks. The amphiphilic character and endogenous nature of phospholipids in lecithin have proven to be an important raw material in food, pharmaceutical and cosmetic products.

Lecithin has emulsification and lubricant properties, and is a surfactant. Lecithin has been recognized as being one of the major classes of food emulsifier. Phospholipids in lecithin have also been used as release agents, through their role as surfactants.

There are many known methods for extracting lecithin from various oil seed materials.

US Patent no. 4,515,726, US Patent no. 4,221 ,731 and WO 2004/014144 disclose methods of extracting lecithin from soybeans. US Patent no. 5,833,858 describes a method of obtaining acidic phospholipids from an oil seed selected from the group consisting of soybean, rapeseed, corn, sunflower and palm. US Publication no. US2005/01 12735A1 and WO 2005/035693 each describes a process for extracting lipids and lecithin from sludge generated during biological treatment.

US Patent no. 7,550,616 discloses a process for recovering polar lipid from native biomaterials, such as egg, fish, crustaceans, microbes, brain tissue, milk, meat and plant material, including oilseeds. WO 91/03946 discloses a process for recovering an egg lecithin from egg yolk. US Patent no. 6,355,693 discloses a method for producing polar lipids from plant material such as cereal or grains. US Patent no. 5,597,602 describes a process for recovering lecithin from soy-beans, rapeseed, sunflower seed, corn, hemp and linseed.

Other patents which relate to extraction of lecithin from various materials include US Patent no. 5,783,210 which describes a lecithin extracted from egg yolk, soy lecithin and other commercially available sources of lecithin. US Patent no. 4,927,544 discloses a process of recovering lecithin from soy bean oil, sunflower seed oil, rape seed oil, palm oil and other vegetable oils as well as lard, tallow, and fish oil by centrifugal separation for continuous removal of a gum phase. US Patent no. 7,494,679 describes a process of recovering lecithin from soy bean oil, corn oil, ground nut oil, olive oil, linseed oil, rapeseed oil, sunflower seed oil, safflower seed oil, cottonseed oil, and grape seed oil using membrane separation technology.

WO 2005/77485 A1 discloses a method for recovering lecithin from palm oil mill effluent using membrane filtration. There are several publications that discuss methods of extracting lecithin from crude palm oil, palm pressed fiber and palm oil mill sludge. For example, Goh et al., "Total Phospholipids in Crude Palm Oil: Quantitative Analysis and Correlations with Oil Quality Parameters", JAOCS, Vol. 61 : 1597-1600 (1984) discloses a method of using methanol-acetic acid to extract phospholipids from crude palm oil. Chua et a)., Optimization of Ultrasound Extraction of Phospholipids from Palm-Pressed Fiber", Journal of Food Engineering Vol. 92:403-409 (2009) discloses a method of using chloroform-methanol solvent to extract phospholipids from palm pressed fiber. The extraction was assisted by an ultrasound device.

Chow M C et al., "Chemical Composition of Oil Droplets from Palm Oil Mill Sludge", Journal of Oil Palm Research Vol. 14, no. 1 :25-34 (2002) discloses a method of using choloroform-methanol solvent to extract lecithin from palm oil mill sludge. The method involves a two-stage centrifugation process and only droplets obtained after centrifugation are used for extraction. The composition obtained by this method contains about 10 wt% of phospholipids.

Yuen May Choo et al., "Phospholipids from Palm-Pressed Fiber", JAOCS, Vol. 81 , no.5:471 -475 (2004) discloses a method of using hexane-ethanol solvent in a ratio of 1 :1 to extract phospholipids from palm-pressed fiber collected from a palm oil mill. The extract yielded about 4.68% of phospholipids, consisting predominantly phosphatidyl choline (PC), phosphatidyl ethanolamine (PE), phosphatidylglycerol (PG) and phosphatidic acid (PA). The methods disclosed in the above studies are only able to produce less than 10% of phospholipids in the extract.

With the increase in use and demand of lecithin in food, pharmaceutical and cosmetic industries, there is a need to look for a new source of lecithin to meet the demand and to address at least one of the above problems, or at least to provide an alternative.

SUMMARY OF THE INVENTION

The above and other problems are solved and an advance in the art is made by providing a method for extracting lecithin from palm agro-waste in accordance with this invention. It is an advantage of a method in accordance with this invention that the method is capable of yielding lecithin containing phospholipids in a higher concentration from palm agro-waste. A second advantage of this invention is that the method is easily scalable for commercial production of lecithin. A third advantage of this invention is that a composition containing lecithin having a phospholipids content of not less than 20%, more preferably, not less than 35% extracted from palm agro-waste is obtained. A fourth advantage of this invention is that the method yields more than 0.5% dry wt/wt of the palm agro-waste.

In accordance with an embodiment of the invention, the method is performed in the following manner. The method comprises the steps of introducing a palm agro-waste as a starting material selected from a group consisting of a separator sludge or a decanter cake; subjecting the starting material to extraction using a solvent to give an extracted meal and a solvent extract; separating the solvent extract from the extracted meal; and drying the solvent extract to give a residue fraction comprising lecithin having a phospholipids content of not less than 20%, with a yield of more than 0.5% dry wt/wt of the starting material.

In accordance with an embodiment of the invention, the residue fraction comprises lecithin having a phospholipids content of not less than 35%.

In accordance with an embodiment of the invention, the yield is more than 1.5% dry wt/wt of the starting material.

In accordance with some embodiments of the invention, the method further comprises pre-treating the starting material prior to the step of subjecting the starting material to extraction. In accordance with some of these embodiments, the pre-treating step comprises the step of drying the separator sludge to obtain a dried sludge as the starting material. In accordance with some other embodiments of the invention, the pre-treating step comprises the step of centrifuging the separator sludge to obtain a solid and a supernatant. In accordance with some of these embodiments, the pre- treating step further comprises washing the solid of palm agro-waste to obtain a pre- washed solid of palm agro-waste as the starting material.

In accordance with another embodiment of this invention, the pre-treating step comprises washing the decanter cake with water to obtain a pre-washed decanter cake as the starting material.

In accordance with some of these embodiments, the extraction solvent is a mixture of hexane and ethanol. In accordance with some of these embodiments, the solvent is a mixture of ethanol and water.

In accordance with the embodiment of the invention, the weight ratio of the starting material to the solvent is from 1 : 1 to 1 :20.

In accordance with another embodiment of the invention, there is provided a composition comprising lecithin extracted from palm agro-waste selected from a group consisting of a separator sludge or a decanter cake, having a phospholipids content of not less than 20%.

In accordance with an embodiment of the invention, the composition having a phospholipids content of not less than 35%. In accordance with an embodiment of the invention, the lecithin comprises phosphatidylethanolamine (PE), phosphatidylcholine (PC), phosphatidylinositol (PI), phosphatidylserine (PS), phosphatidylglycerol (PG), phasphatidic acid (PA), and lyso- derivatives. In accordance with some embodiments of the invention, the lecithin comprises a phosphotidylcholine (PC) concentration of more than 30% wt wt of total phospholipids. The phosphotidylcholine (PC) to the phosphatidylethanolamine (PE) is in a weight ratio of more than 4. DETAILED DESCRIPTION OF THE INVENTION

Definitions

The following words and terms have the meanings given below, unless indicated otherwise. These are intended as general definitions and should in no way limit the scope of the present invention to those terms alone, but are put forth for better understanding of the following description.

The term "palm agro-wastes" refers to wastes produced in a palm oil mill. The wastes can be in the form of sludge, effluent or a mixture thereof. The term "raw sludge" refers to sludge or effluent obtained directly from a centrifuging decanter, a centrifuging separator and/or a 3-phase decanter of a palm oil mill without undergoing any pretreatment or solid-liquid separation. The term "supernatant" refers to a liquid obtained from centrifuging the raw sludge as defined above.

The term "dried supernatant" refers to a supernatant that is obtained from centrifuging a raw sludge and dried by any method known in the art including, but is not limited to, freeze-dried, vacuum dried, evaporation or desiccant dried.

The term "solid" refers to a solid obtained from centrifuging the raw sludge as defined above. The term "dried sludge" refers to a raw sludge that has been dried.

The term "cake" refers to a solid or cake obtained from a 3-phase decanter of a palm oil mill. The term "pre-washed solid" refers to a solid or cake that has been washed with water.

Malaysian crude palm oil (CPO) contains relatively low levels of polar constituents, such as phosphatides (5-130 ppm). These minor components are present in extracts that are obtained from palm agro-waste, such as decanter cake, sludge and effluents from palm oil mills in a much higher concentration. In view of the abundance of palm agro-wastes produced in palm oil mills, there is a growing interest in recovering these polar constituents, for example, lecithin from the palm agro-wastes produced in palm oil mills, as the process can add value to existing palm oil industry. Therefore, exploration on palm agro-wastes, such as separator sludge or decanter cake is the focus of the present invention.

Separator sludge is one of the waste streams that contributed to be part of palm oil mill effluent (POME). Approximately 1.5m³ of POME will be generated from the sludge separator for each tonne of crude palm oil processed. It is a colloidal suspension containing more than 80% of water, about 15% to 19% of total solids, consisting mainly of debris from palm fruit mesocarp, and small amount of oil. Another palm agro-waste that generates interest is the decanter cake which is basically the solid material that remains after sludge is decanted from the clarifier using a three phase decanter from palm oil mill. About 3% to 4% of decanter cake is generated with every tonne of fresh fruit bunch processed. It contains relatively lower water content as compared to those agro-wastes from the separator sludge and effluent.

The design and year of operation of the palm oil mill is not particularly restricted for the purpose of the invention, as long as the palm oil mill uses a decanter or a separator type of apparatus for processing the crude palm oil. The palm oil mill can include a horizontal, vertical or continuous sterilizer.

The present invention relates to a method of extracting lecithin from palm agro-waste produced in a palm oil mill. The method comprises introducing a palm agro-waste selected from a group consisting of a separator sludge and a decanter cake as a starting material and subjecting the starting material to extraction using a solvent to give an extracted meal and a solvent extract.

In one embodiment of the invention, the solvent used in the extraction step is a hexane- ethanol solvent. The volume ratio of hexane to ethanol present in the solvent preferably ranges from 100:0 to 0:100, more preferably 25:75 to 0:100, and most preferably 25:75 to 75:25. The ethanol in the solvent may contain about 5% to 6% water. In another embodiment of the invention, an ethanol-water solvent is used in the extraction step. The volume ratio of ethanol to water present in the solvent preferably ranges from 80:20 to 99.9:0.1 , and more preferably in a ratio of 80:20 to 95:5.

The extraction step is carried out at a stirring speed of about 400 rpm to 800 rpm, and preferably more than 800 rpm. The stirring speed is not particularly restricted for the purpose of the invention. The stirring can be done by means of mixing or by any means known in the art to enhance the recovery of the phospholipids. In one embodiment of the invention, the duration in which the extraction is carried out is about one hour. The duration of the extraction can be prolonged if necessary to obtain maximum recovery of the phospholipids. The ratio of the starting material to solvent used in the method ranges from about 1 : 1 to 1 :20, and more preferably 1 :10. The extraction step is preferably carried out at a temperature in the range of 30°C to 60°C, and more preferably at 30°C or at ambient temperature.

The extraction step can be carried out over a pH range from about 5 to 9. It is preferable that the extraction step is carried out without adjusting the pH value of the mixture during the extraction.

After the extraction is completed, the solvent extract is separated from the extracted meal. This can be carried out by means of filtration or by other means known in the art.

The separated solvent extract is then dried to remove most of the solvent, followed by precipitation or crystallization. The precipitate obtained thereto is then recovered by filtration to give a residue fraction comprising lecithin having a phospholipids content of not less than 20%, more preferably, not less than 35%. This is achieved with a yield of more than 0.5% dry wt/wt of the palm agro-waste. The solvent extract may be dried under reduced pressure to remove the solvent. Any suitable method known in the art can be employed to dry the solvent extract. In an exemplary embodiment of the invention, the solvent extract is dried by distilling the solvent off the extract.

In another exemplary embodiment of the invention where ethanol-water solvent is used in the extraction step, the separated solvent extract is dried at a temperature below 40°C and at a pressure of less than 150 mbar (or 1.5 x 10⁴ Pa). The solution containing the extract is kept at temperature below 8°C for more than 12 hours. The precipitate formed is then centrifuged and separated from the solution. Any suitable method known in the art can be used to separate the precipitate from the solution.

The separator sludge (or raw sludge) and the decanter cake which are used as the starting material in the method of the present invention may be pre-treated to obtain other forms of palm agro-waste as the starting material prior to subjecting the starting material to extraction by solvent. These other forms of palm agro-waste include, but are not limited to, dried supernatant of palm agro-waste, solid of palm agro-waste, dried sludge, pre-washed solid of palm agro-waste and pre-washed solid of decanter cake. In one embodiment of the invention, the separator sludge or raw sludge is pre-treated by drying to obtain a dried sludge as the starting matter. It is understood that any suitable method known in the art may be employed for drying the raw sludge.

In another embodiment of the invention, the separator sludge is pre-treated by centrifuging the separator sludge to obtain a supernatant and a solid. The supernatant may be further treated by drying to obtain a dried supernatant. The supernatant can be dried by any suitable method known in the art including, but is not limited to, freeze- dried, vacuum dried, evaporation or desiccant dried. The dried supernatant and the solid (or solid of palm agro-waste) can separately be used as the starting material.

In yet another embodiment of the invention, the solid of palm agro-waste obtained through centrifuging the separator sludge is further treated by washing the solid with water to obtain a pre-washed solid of palm agro-waste as the starting material.

In other embodiment of the invention, the decanter cake is pre-treated by washing the decanter cake with water to obtain a pre-washed solid of decanter cake as the starting material.

The water pre-treatment step as described hereinabove can be carried out by any means known in the art. The ratio of palm agro-waste to water used preferably ranges from 1 :1 to 1 :20, and more preferably from 1 :4 to 1 :6.

The lecithin extracted by the method of the present invention contains phospholipids with content not less than 20%, more preferably, not less than 35%, with a yield of more than 0.5% dry wt/wt of the palm agro-waste. The lecithin comprises particularly of phosphatidylethanolamine (PE), phosphatidylcholine (PC), phosphatidylinositol (PI), phosphatidylserine (PS), phosphatidylglycerol (PG), phasphatidic acid (PA), and lyso- derivatives thereof relative to the lecithin in palm oil found in naturally occurring oil palm ago-wastes. Neutral lipids such triglycerides, diglycerides, and monoglycerides, fatty acids, glycolipids, sugars, and other minor components at arbitrary ratios may also be present.

In one preferred embodiment of the present invention where the starting material is decanter cake, the lecithin comprises PC concentration of more than 30% wt/wt of total phospholipids and a ratio of PC:PE of greater than 4, The solvent extract prepared by the method of the present invention is suitable for use as a starting material for purification/preparation of high purity phospholipids for use as standards, pharmaceutical additives, nutraceuticals, etc. Purification could be done using known methods, for example, simulated moving bed (SMB) method, countercurrent chromatography (CCC) method, acetone precipitation method, etc.

The method in accordance with this invention is easily scalable for commercial production of lecithin as the method involves a multi-stage extraction process.

The present invention also relates a composition comprising lecithin extracted from palm agro-waste selected from the group consisting of a separator sludge and a decanter cake and the lecithin having a phospholipids content of not less than 20%, more preferably, not less than 35%. The lecithin comprises phosphatidylethanolamine (PE), phosphotidylcholine (PC), phosphatidylinositol (PI), phosphatidylserine (PS), phosphatidylglycerol (PG), phasphatidic acid (PA), and lyso-derivatives. In a preferred embodiment where the starting material is the decanter cake, the lecithin comprises PC concentration of more than 30% wt/wt of total phospholipids and a ratio of PC:PE of greater than 4.

Having now generally described the invention, the same will be more readily understood through reference to the following examples, which are provided by way of illustration, and are in no way to be construed to limit the invention to specific procedures, conditions or compositions described therein, unless so specified.

EXAMPLES

Preparation of starting materials 100g of raw sludge was centrifuged at 8,000 rpm for one hour, to obtain a supernatant (about 82g) and a solid (about 18g). The supernatant was freeze-dried to obtain a dried supernatant (about 3.1g).

100g of raw sludge was freeze-dried to obtain a dried sludge (about 5.7g). About 10Og of decanter cake was washed with water to obtain more than 85g of pre- washed solid of decanter cake.

About 100g of solid obtained through centrifuging the raw sludge was washed with water to obtain a pre-washed solid of palm agro-waste.

Example 1

The phospholipids compositions (a) to (h) as illustrated in Table 2 were produced by extracting lecithin from the solid of palm agro-waste obtained through centrifuging raw sludge of palm agro-waste using the parameters set forth in (8), (10), (5), (1 ), (7), (6), (3) and (4) of Table 1 respectively. Solvent was removed from the respective extracts under reduced pressure to obtain the respective phospholipids extracts. Example 2

The phospholipids compositions (i) to (I) as illustrated in Table 2 were produced by extracting lecithin from the raw sludge using the parameters set forth in (1 1 ), (8), (2) and (9) of Table 1 respectively. Solvent was removed from the respective extracts under reduced pressure to obtain the respective phospholipids extracts.

TABLE 1

No °C Rpm Hex:EtOH PH

(1) 30 400 75:25 5

(2) 30 400 25:75 9

(3) 30 400 25:75 5

(4) 30 800 25:75 5

(5) 45 600 100:0 -

(6) 45 600 0:100 5

(7) 60 800 75:25 9

(8) 60 400 25:75 9

(9) 60 400 25:75 5

(10) 60 800 25:75 5

(11 ) 60 400 75:25 5

(12) 60 400 75:25 9 Example 3

72g of raw sludge was added to a 2L container. 1 ,440 mL of solvent containing a mixture of hexane-ethanol in a ratio of 25:75 was added to the same container. Extraction was performed at a stirring speed of 800 rpm at 30°C for 1 hour. The mixture was then filtered to obtain the extract solution. Solvent was distilled off from the extract under reduced pressure to give a desired phospholipids composition having composition as shown in (m) of Table 2. The phospholipids composition (m) was prepared using the parameters set forth in (4) of Table 1.

Example 4

100mg of dried sludge was added to a 2mL tube. 1ml_ of solvent containing a mixture of hexane-ethanol in a ratio of 75:25 was then added to the same tube. The pH of ethanol was adjusted to pH 9 by adding triethylamine before adding the ethanol to the tube containing the dried sludge. The tube was placed within a heating block and extraction was performed at a speed of 400 rpm at 60°C for 1 hour. The heating block was used to help control the temperature and the stirring speed of the mixture. After the extraction was completed, the solvent containing the extract was then filtered to remove the extracted cake. The extract solution was then freeze-dried to give a desired phospholipids composition having composition as shown in (n) of Table 2. The phospholipids composition (n) was prepared using the parameters set forth in (12) of Table 1.

Example 5

100mg of dried supernatant was added to a 2ml_ tube. 1ml_ of solvent containing a mixture of hexane-ethanol in a ratio of 75:25 was then added to the same tube. The tube was placed within a heating block and extraction was performed at a speed of 400 rpm at 60°C for 1 hour. After the extraction was completed, the solvent containing the extract was then filtered to remove the extracted cake. The extract solution was then freeze-dried to give a desired phospholipids composition having composition as shown in (o) of Table 2. The phospholipids composition (o) was prepared using the parameters set forth in (1 1 ) of Table 1. Example 6

500g of cake was added to a 10L stainless steel extraction vessel. 5,000 mL of solvent containing a mixture of hexane-ethanol in a ratio of 25:75 was then added to the same vessel. Extraction was performed at a speed of 800 rpm at room temperature for 1 hour. An IKA stirrer was used in stirring the mixture. After the extraction was completed, the solvent containing the extract was then filtered. The solvent was distilled off from the extract under reduced pressure to give a desired phospholipids composition having composition as shown in (p) of Table 3. The amount of extract obtained was about 6.34 ± 0.31% wt/wt of the cake.

Example 7

5g of cake was added to a 50 mL tube. 25mL of solvent containing a mixture of hexane-ethanol in a ratio of 25:75 was then added to the same tube. The heating block was used to help control the temperature and the stirring speed of the mixture. Extraction was performed at a speed of 800 rpm at room temperature for 2 hours. After the extraction was completed, the solvent containing the extract was then filtered. The extract solution was then freeze-dried to give a desired phospholipids composition having composition as shown in (q) of Table 3.

Example 8

5g of cake was added to a 50 mL tube. 15mL of solvent containing a mixture of hexane-ethanol in a ratio of 25:75 was then added to the same tube. Extraction was performed at a speed of 800 rpm at room temperature for 3 hours. After the extraction was completed, the solvent containing the extract was then filtered to discard from the extracted cake. The extract solution was then freeze-dried to give a desired phospholipids composition having composition as shown in (r) of Table 3.

Example 9

5g of cake was added to a 50 mL tube. 10mL of a solvent containing a mixture of hexane-ethanol in a ratio of 25:75 was then added to the same tube. Extraction was performed at a speed of 800 rpm at room temperature for 4 hours. After the extraction was completed, the solvent containing the extract was then filtered. The extract solution was then freeze-dried to give a desired phospholipids composition having composition as shown in (s) of Table 3.

Example 10

2g of cake was added to a 50 mL tube. 2mL of a solvent containing a mixture of hexane-ethanol in a ratio of 25:75 was then added to the same tube. Extraction was performed at a speed of 800 rpm at room temperature for 5 hours. After the extraction was completed, the solvent containing the extract was then filtered. The extract solution was then freeze-dried to give a desired phospholipids composition having composition as shown in (t) of Table 3.

Example 11

500g of cake was added to a 10L stainless steel extraction vessel. 5,000 mL of solvent containing a mixture of hexane-ethanol in a ratio of 25:75 was then added to the same vessel. The ethanol may contain about 5% to 6% water. Extraction was performed at a speed of 800 rpm at ambient temperature for 1 hour. An IKA stirrer was used to stir the mixture. After the extraction was completed, the solvent containing the extract was then filtered. The hexane fraction was separated from the ethanol fraction through solvent partition. The ethanol was distilled off from the extract under reduced pressure to obtain a desired phospholipids composition having composition as shown in (u) of Table 4. The amount of extract obtained was about 3.33 ± 0.04% wt/wt of the cake.

Example 12

500g of pre-washed solid of palm agro-waste was added to a 10L stainless steel extraction vessel. 5,000 mL of ethanol was then added to the same vessel. The ethanol may contain about 5% to 6% water. Extraction was performed at a speed of 800 rpm at room temperature for 1 hour. An IKA stirrer was used to stir the mixture. After the extraction was completed, the solvent containing the extract was then filtered. The solvent was distilled off from the extract under reduced pressure to give a desired phospholipids composition having composition as shown in (v) of Table 4. The amount of extract obtained was about 2.15% wt/wt of the cake. Example 13

Pre-washed solid obtained through washing the decanter cake with water (704.74 g) was added to a 10 L stainless steel extraction vessel. 7,000 ml. of solvent containing a mixture of hexane-ethanol in a ratio of 25:75 was then added to the same vessel. The ethanol may contain about 5% to 6% water. Extraction was performed at a speed of 800 rpm at room temperature for 1 hour. An IKA stirrer was used to stir the mixture. After the extraction was completed, the solvent containing the extract was then filtered. The hexane fraction was separated from the ethanol fraction through solvent partition. The ethanol was distilled off from the extract under reduced pressure to give a desired phospholipids composition having composition as shown in (w) of Table 4. The amount of extract obtained was about 1.93% wt/wt of the cake.

Example 14

707 g of decanter cake were washed with 3500 mL water to obtain a pre-washed solid. The pre-washed solid obtained thereto was added to a 10 L stainless steel extraction vessel. 7,000 mL of ethanol was then added to the same vessel. The ethanol may contain about 5% to 6% water. Extraction was performed at a speed of 800 rpm at ambient temperature for 1 hour. After the extraction was completed, the solvent containing the extract was then filtered. The solvent was distilled off from the extract at temperature below 40°C at pressure less than 150 mbar until about 500 ml of solution remained in the container. The solution containing the extract was kept at temperature below 8°C overnight. The precipitate formed was removed from the solution by centrifuging at 8000 rpm for 1 hour at 4°C. The precipitate was separated from the supernatant to give a desired phospholipids composition having composition as shown in (x) of Table 5. The amount of extract obtained was about 1.75 ± 0.52% wt/wt of the cake.

Example 15

The phospholipids compositions (y) to (bi) as illustrated in Table 6 were produced by extracting lecithin from the pre-washed solid of palm agro-waste using the parameters set forth in Example 12 with different solvent ratios of ethanol-water. Solvent was removed from the respective extracts under reduced pressure to obtain the respective phospholipids extracts. The phospholipids compositions obtained in the above Examples were subjected to HPLC analysis using an Evaporative Light Scattering Detector (ELSD). The results of the analysis and the phospholipids compositions (expressed in mg/g by weight in lipid mixture) are as shown in Tables 2, 3, 4 and 5 below.

TABLE 2

mg/g

Total of

Sample:

No Samples phospholipids PA &

solvent PE PI PS PC LPC

(mg/g) PG

(a) Solid (8) 1 :20 214.42 0.00 94.98 21.49 34.72 52.55 10.68

(b) Solid (10) 1 :20 194.52 0.00 79.02 14.47 42.42 50.33 8.28

(c) Solid (5) 1 :10 29.40 0.00 12.88 0.00 0.00 16.52 0.00

(d) Solid (1) 1 :20 256.78 0.00 111.28 21.87 67.99 44.08 11.56

(e) Solid (7) 1 :20 142.06 0.00 80.38 16.14 0.00 37.23 8.31

(0 Solid (6) 1 :10 168.49 0.00 61.04 24.67 18.11 53.30 11.37

(g) Solid (3) 1 :20 160.38 9.85 77.74 9.56 3.28 50.92 9.03

(h) Solid (4) 1 :10 177.37 0.00 62.48 27.44 16.15 58.00 13.30

(i) Raw sludge (11 ) 1 :20 20.83 0.00 0.00 0.00 0.00 20.57 0.26

(i) Raw sludge (8) 1 :20 326.06 0.00 173.13 16.22 94.33 29.48 12.90

(k) Raw sludge (2) 1 :20 167.66 0.00 129.35 8.28 0.00 22.74 7.28

(1) Raw sludge (9) 1 :20 87.99 0.00 23.71 7.41 44.06 12.81 0.00

(m) Raw sludge (4) 1 :20 147.09 0.00 35.56 16.96 54.18 28.95 11.44

(n) Dried sludge (12) 1 :10 89.90 0.00 56.72 7.08 6.40 18.09 1.62

(o) Dried supernatant ( 1) 1 :10 30.64 . 0.00 12.97 0.00 0.00 17.67 0.00

TABLE 3

mg/g

Total of

Samples ^S s^ao^mlv Jent ^' p _*"hos_*p»holiγpid™s> _{pA & pQ pE p| ps pc Lpc}

(mg/g)

(P) Cake (4) 1 :10 172.60 35.06 10.78 31.74 0 84.38 10.64

(q) Cake (4) 1 :5 124.36 21.85 37.50 11.63 17.36 30.82 5.21

(r) Cake (4) 1 :3 103.75 18.58 31.58 7.14 14.58 24.74 7.13

(s) Cake (4) 1 :2 42.65 9.29 10,83 3.62 7.00 9.81 2.10

(t) Cake (4) 1 :1 34.52 6.70 7.40 3.44 6.48 7.41 3.09 TABLE 4

Total of mg/g

Samples phospholipids

PA & PG PE PI PS PC

(mg/g) LPC

(u) Cake 244.06 50.62 6.87 39.88 0 125.18 21.51

M pre-washed solid 295.19 64.55 5.74 45.75 0 163.02 16.13

(w) pre-washed solid 240.52 45.08 30.21 26.69 0 125.79 12.75

TABLE 5

Total of mg/g

Samples phospholipids

PG PA PE PI/PS/LPS PC/LPS LPC

(mg/g)

M pre-washed solid 508.39128.89 64.06±3.44 6 63±0.44 168.76±7.77 227.63±18.84 26.74±1.45

TABLE 6

Total mg/g

Phospholipids

Sample

(mg/g) ^PG PA+PE PI+PS+LPA PC+LPS LPC

(y) 95% ETOH 280.45 27.96 53.25 83.47 98.67 17.10

(z) 90% EtOH 247.45 25.68 46.35 72.82 87.47 15.13

(ai) 80% ETOH 129.49 8.05 26.31 40.26 44.23 10.64 commercial food

(bi) 138.96 8.67 29.69 43.41 45.47 11.73 grade ethanol

The above is a description of the subject matter the inventors regard as the invention and is believed that others can and will design alternative methods and compositions that include this invention based on the above disclosure.

Claims

Claims:

1. A method of extracting lecithin from palm agro-waste, the method comprising: introducing a palm agro-waste as a starting material selected from a group consisting of a separator sludge and a decanter cake;

subjecting the starting material to extraction using a solvent to give an extracted meal and a solvent extract;

separating the solvent extract from the extracted meal; and

drying the solvent extract to give a residue fraction comprising lecithin having a phospholipids content of not less than 20%, with a yield of more than 0.5% dry wt/wt of the starting material.

2. The method according to claim 1 , wherein the residue fraction comprises lecithin having a phospholipids content of not less than 35%.

3. The method according to claim 1 , wherein the yield is more than 1.5% dry wt/wt of the starting material.

4. The method according to claim 1, wherein the lecithin comprises phosphatidylethanolamine (PE), phosphotidylcholine (PC), phosphatidylinositol (PI), phosphatidylserine (PS), phosphatidylglycerol (PG), phasphatidic acid (PA), and lyso- derivatives.

5. The method according to claim 1 , further comprising:

pre-treating the starting material prior to the step of subjecting the starting material to extraction.

6. The method according to claim 5, wherein the step of pre-treating comprises: washing the decanter cake with water to obtain a pre-washed decanter cake as the starting material.

7. The method according to claim 5, wherein the step of pre-treating comprises: centrifuging the separator sludge to obtain a solid of palm agro-waste and a supernatant.

8. The method according to claim 7, wherein the solid of palm agro-waste is used as the starting material.

9. The method according to claim 7, further comprising:

washing the solid of palm agro-waste with water to obtain a pre-washed solid of palm agro-waste as the starting material.

10. The method according to claim 5, wherein the step of pre-treating comprises: drying the separator sludge to obtain a dried sludge as the starting material.

11. The method according to claim 1 , wherein the solvent is a mixture of hexane and ethanol.

12. The method according to claim 1 1 , wherein the solvent of hexane-ethanol is in a weight ratio of 25:75 to 75:25.

13. The method according to claim 1 , wherein the solvent is a mixture of ethanol and water.

14. The method according to claim 13, wherein the solvent of ethanol-water is in a weight ratio of 80:20 to 99.9:0.1.

15. The method according to claim 1 , wherein extraction of the starting material is performed at a temperature from 30°C to 60°C.

16. The method according to claim 1 , wherein extraction of the starting material is performed at a stirring speed of 400 rpm to 800 rpm.

17. The method according to claim 1 , wherein weight ratio of the starting material to the solvent is from 1 : 1 to 1 :20.

18. A composition comprising lecithin extracted from palm agro-waste selected from a group consisting of a separator sludge and a decanter cake, having a phospholipids content of not less than 20%.

19. A composition according to claim 18, wherein the composition having a phospholipids content of not less than 35%.

20. The composition according to claim 18, wherein the lecithin comprises phosphatidylethanolamine (PE), phosphotidylcholine (PC), phosphatidylinositol (PI), phosphatidylserine (PS), phosphatidylglycerol (PG), phasphatidic acid (PA), and lyso- derivatives.

21. The composition according to claim 18, wherein the palm agro-waste is decanter cake.

22. The composition according to claim 21 , wherein the lecithin comprises a phosphotidylcholine (PC) concentration of more than 30% wt/wt of total phospholipids.

23. The composition according to claim 22, wherein the phosphotidylcholine (PC) to the phosphatidylethanolamine (PE) is in a weight ratio of more than 4.