CN105010721A - Multi-step coupling method to prepare concentrated phospholipids with a high transparency - Google Patents

Multi-step coupling method to prepare concentrated phospholipids with a high transparency Download PDF

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CN105010721A
CN105010721A CN201510431196.4A CN201510431196A CN105010721A CN 105010721 A CN105010721 A CN 105010721A CN 201510431196 A CN201510431196 A CN 201510431196A CN 105010721 A CN105010721 A CN 105010721A
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concentrated
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centrifugal
grade
food
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刘元法
吴楠
李进伟
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Jiangnan University
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Jiangnan University
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Abstract

The present invention discloses a multi-step coupling method to prepare concentrated phospholipids with a high transparency, which belongs to the technical field of soybean phospholipid production. The feed-grade concentrated phospholipids are used as raw materials, and the raw materials are dissolved in normal hexane or other non-polar solvents, are subjected to pre-impurity removing by centrifugation, precisely filtrated, bleached by food-grade hydrogen peroxide, are subjected to adsorption treatment and other multi-step coupling processes to obtain soybean concentrated phospholipids which contain normal hexane insoluble substances less than 0.05%, and are high in transparency and light in color and luster. By using precisely filtration and other technology, a new technology condition which uses feed-grade phospholipids as raw materials to produce food-grade soybean concentrated phospholipids is established, and the concentrated phospholipids can be industrially produced in a large scale. The preparation method solves the technical problems that the soybean concentrated phospholipids are high in impurity content and poor in transparency in our country, and each indicator of the prepared soybean transparent concentrated phospholipid product reaches or is above the national standards.

Description

The method of high grade of transparency concentrated phosphatide is prepared in a kind of multistep coupling
Technical field
The present invention relates to the method that high grade of transparency concentrated phosphatide is prepared in the coupling of a kind of multistep, belong to soybean lecithin production technical field.
Background technology
Phosphatide is mainly derived from the vegetalitas oil plants such as soybean, and soybean lecithin is the product that the accessory substance in crude oil of soybean hydration degum production process obtains after processed.Phosphatide mainly comprises: phosphatid ylcholine (PC), phosphatidyl-ethanolamine (PE), phosphorus phosphatidylinositols (PI) and neutral wet goods.Phospholipid prod all has important Function and operation in body-care, diet nutritional and disease prevention and cure etc.In addition, phosphatide, due to its good emulsibility, wetability and surface-active, can be used as surfactant, emulsifying agent and lubricant etc. and is widely used in and cures, in candy, the food industry of vegetable milk wet goods.
China's scale reaches 279250 ton per days with the factory's soybean squeezing aggregated capacity that oils, and oil foot production scale is big well imagines.But, the scouring processes that China's fats and oils processing is produced generally only is focused on degumming effect and ignores the quality of oil foot, cause the problems such as the soybean lecithin ubiquity n-hexane insolubles content of domestic production is high, color and luster dark, transparency difference, the concentrated soybean phospholipid produced is caused mostly to be added in feed as nutrition fortifier, or abroad, range of application is very limited for low-price export.Therefore, if the soybean lecithin resource of China's abundant can be made full use of, Development and Production goes out the concentrated soybean phospholipid that n-hexane insolubles content is low, the transparency is good, color and luster is more shallow, not only can improve the added value of concentrated soybean phospholipid, and for follow-up phospholipid prod seriation, become more meticulous, customizations establishes application foundation.
At present, the existing method using inorganic membrane filtration to prepare food-grade concentrated phosphatide, but easily cause film blocking, flux depression in filter process, the cleaning difficulty of film, and equipment investment is costly; In addition, the method for existing employing centrifugal segregation n-hexane insoluble matter, too high to the requirement of centrifugal rotational speed (6000 ~ 20000rpm), be difficult to reach, energy consumption is high.
Summary of the invention
The object of the invention is to adopt multistep coupling processing to prepare food-level concentrated soybean phospholipid, realize the transformation of feed grade soybean lecithin raw material to food level soybean phosphatide.
Technical solution of the present invention comprises following steps:
(1) centrifugal pretreatment: feed grade soybean lecithin mixes with the ratio of n-hexane according to mass ratio 1:2 ~ 1:8, under centrifugal rotational speed is 3000 ~ 4500rpm condition, within centrifugal 10 ~ 30 minutes, carry out centrifugal pretreatment, be separated and remove most of n-hexane insoluble matter;
(2) filter: centrifugal pretreated supernatant is squeezed into ultra-filtration system, described ultra-filtration system is titanium rod candle filter, filtering accuracy is 0.1 ~ 5 μm, filter pressure is 0.1 ~ 0.6MPa, discharge velocity is 20ml/min ~ 30ml/min, feeding temperature is 30 ~ 60 DEG C, and filtering times is 1 ~ 4 time;
(3) decolour: the feed liquid after ultra-filtration system filters carries out desolventing technology, decolorizer to be mass fraction be 30% edible hydrogen peroxide, decolorizer addition is 1% ~ 5% of feed grade concentrated phosphatide quality, and bleaching time is 20 ~ 60 minutes, and bleaching temperature is 30 ~ 80 DEG C;
(4) adsorption treatment: the feed liquid after desolventing technology carries out adsorption treatment, adsorbent is diatomite, active carbon or atlapulgite, adsorbent addition is 1% ~ 5% of feed grade concentrated phosphatide quality, and adsorption time is 30 minutes ~ 60 minutes, and adsorption temp is 30 ~ 80 DEG C;
(5) secondary centrifuging: the feed liquid after adsorption treatment, under centrifugal rotational speed is 3000 ~ 4500rpm condition, carries out secondary centrifuging process in centrifugal 10 ~ 30 minutes;
(6) evaporation and concentration: the feed liquid after secondary centrifuging process carries out Vacuum film evaporation, evaporating temperature is 80 ~ 95 DEG C, and residual voltage is less than 0.09Mpa, and evaporation time is 60 ~ 180 minutes, remove solvent and excessive moisture, obtain high-quality food-level concentrated soybean phospholipid.
In one embodiment of the invention, the mass ratio of step (1) feed grade soybean lecithin and n-hexane is 1:4, and centrifugal pretreatment condition is 4500rpm, centrifugal 20 minutes.
In one embodiment of the invention, the filtering accuracy of step (2) ultra-filtration system is 0.4 μm, and discharge velocity is 25ml/min, and feeding temperature is 40 DEG C, and filtering times is 2 times.
In one embodiment of the invention, step (3) hydrogen peroxide addition is 2% of concentrated phosphatide quality, decolours 40 minutes at 50 DEG C.
In one embodiment of the invention, step (6) 90 DEG C, under residual voltage is less than 0.09MPa condition, Vacuum film evaporation obtains the high food-grade phosphatide of transparency for 2 hours.
The techniques such as centrifugal pretreatment, secondary filter process, desolventing technology, adsorption treatment, evaporation and concentration process combine by the present invention effectively, make that originally color and luster is comparatively dark, higher, the opaque feed concentrated soybean phospholipid of n-hexane insolubles content is refined as color and luster is more shallow, n-hexane insolubles content extremely low (being less than 0.03%), transparent food soybean lecithin, for the industrialization realizing food soybean lecithin lays the foundation.Accurate filter used not easily blocks, easy to clean, and residue can be removed by " blowback ", and gained food-grade concentrated phosphatide indices all reaches or higher than national standard.
Detailed description of the invention
Acetone insoluble matter: assay method imports and exports the phosphatide acetone insoluble matter method of inspection with reference to SNT 0802.2-1999.
N-hexane insoluble matter: assay method is with reference to GB28401-2012 national food safety standard food additives phosphatide.
Gartner color and luster: assay method is with reference to AOCS Official Method Ja 9-87Gardner Color.
Product light transmittance: found by the length scanning in 400 ~ 800nm visible-range, with n-hexane compound concentration be the membrane filtration sample of 1g/ml, feed grade concentrated soybean phospholipid sample, self-control food-grade concentrated phosphatide sample have obvious difference at 440nm place absworption peak, therefore select the light transmittance T of the different sample of 440nm place mensuration.
Embodiment 1
With feed grade concentrated soybean phospholipid for raw material, be that 1:4 mixed dissolution is abundant by itself and n-hexane solvent according to optimum quality ratio, under low speed desk centrifuge 4500rpm condition, centrifugal 20 minutes, secondary filter adopts 0.4 micron of titanium rod, discharge velocity is 25ml/min, and feeding temperature is 40 DEG C, and filtering times is 2 times; In decolorization, hydrogen peroxide addition is 2% of concentrated phosphatide quality, decolours 50 minutes at 50 DEG C; Adsorption treatment 40 minutes at temperature is 50 DEG C, secondary centrifuging 10 minutes under 4500rpm; Get supernatant and carry out Vacuum film evaporation, evaporating temperature is 90 DEG C, and residual voltage is less than 0.09Mpa, removes solvent and excessive moisture, obtains high-quality food-level concentrated soybean phospholipid.The n-hexane insolubles content of feed grade concentrated soybean phospholipid raw material is 0.6%, and acetone insoluble matter content is 62.5%, Gartner color and luster 14+, and light transmittance is less than 10%; Food-level concentrated soybean phospholipid n-hexane insolubles content prepared by existing membrane filtration is less than 0.04%, and acetone insoluble matter content is greater than 60%, Gartner color and luster 11+, light transmittance about 85%.The product acetone insoluble matter obtained is greater than 62%, and n-hexane insoluble matter is less than 0.03%, and Gartner color and luster 10+, product light transmittance can reach 90%.
Embodiment 2
With feed grade concentrated soybean phospholipid for raw material, be that 1:2 mixed dissolution is abundant by itself and n-hexane solvent according to optimum quality ratio, under low speed desk centrifuge 4000rpm condition, centrifugal 20 minutes, secondary filter adopts 0.8 micron of titanium rod, discharge velocity is 20ml/min, and feeding temperature is 30 DEG C, and filtering times is 1 time; In decolorization, hydrogen peroxide addition is 1% of concentrated phosphatide quality, decolours 60 minutes at 40 DEG C; Adsorption treatment 30 minutes at temperature is 40 DEG C, secondary centrifuging 10 minutes under 4500rpm; Get supernatant and carry out Vacuum film evaporation, evaporating temperature is 80 DEG C, and residual voltage is less than 0.09Mpa, removes solvent and excessive moisture, obtains high-quality food-level concentrated soybean phospholipid.The n-hexane insolubles content of feed grade concentrated soybean phospholipid raw material is 0.6%, and acetone insoluble matter content is 62.5%, Gartner color and luster 14+, and light transmittance is less than 10%; Food-level concentrated soybean phospholipid n-hexane insolubles content prepared by existing membrane filtration is less than 0.04%, and acetone insoluble matter content is greater than 60%, Gartner color and luster 11+, light transmittance about 85%.The product acetone insoluble matter obtained is greater than 62%, and n-hexane insoluble matter is less than 0.03%, and Gartner color and luster 11+, product light transmittance can reach 85%.
Embodiment 3
With feed grade concentrated soybean phospholipid for raw material, be that 1:8 mixed dissolution is abundant by itself and n-hexane solvent according to optimum quality ratio, under low speed desk centrifuge 4500rpm condition, centrifugal 20 minutes, secondary filter adopts 1 micron of titanium rod, discharge velocity is 30ml/min, and feeding temperature is 60 DEG C, and filtering times is 3 times; In decolorization, hydrogen peroxide addition is 4% of concentrated phosphatide quality, decolours 40 minutes at 60 DEG C; Adsorption treatment 50 minutes at temperature is 60 DEG C, secondary centrifuging 10 minutes under 4500rpm; Get supernatant and carry out Vacuum film evaporation, evaporating temperature is 75 DEG C, and residual voltage is less than 0.09Mpa, removes solvent and excessive moisture, obtains high-quality food-level concentrated soybean phospholipid.The n-hexane insolubles content of feed grade concentrated soybean phospholipid raw material is 0.6%, and acetone insoluble matter content is 62.5%, Gartner color and luster 14+, and light transmittance is less than 10%; Food-level concentrated soybean phospholipid n-hexane insolubles content prepared by existing membrane filtration is less than 0.04%, and acetone insoluble matter content is greater than 60%, Gartner color and luster 11+, light transmittance about 85%.The product acetone insoluble matter obtained is greater than 62%, and n-hexane insoluble matter is less than 0.03%, and Gartner color and luster 11+, product light transmittance can reach 85%.
Although the present invention with preferred embodiment openly as above; but it is also not used to limit the present invention, any person skilled in the art, without departing from the spirit and scope of the present invention; all can do various changes and modification, what therefore protection scope of the present invention should define with claims is as the criterion.

Claims (6)

1. prepare a method for food-level concentrated soybean phospholipid, it is characterized in that, comprise following steps:
(1) centrifugal pretreatment: feed grade soybean lecithin mixes with the ratio of n-hexane according to mass ratio 1:2 ~ 1:8, under centrifugal rotational speed is 3000 ~ 4500rpm condition, within centrifugal 10 ~ 30 minutes, carry out centrifugal pretreatment, be separated and remove most of n-hexane insoluble matter;
(2) filter: centrifugal pretreated supernatant is squeezed into ultra-filtration system, described ultra-filtration system is titanium rod candle filter, filtering accuracy is 0.1 ~ 5 μm, filter pressure is 0.1 ~ 0.6MPa, discharge velocity is 20ml/min ~ 30ml/min, feeding temperature is 30 ~ 60 DEG C, and filtering times is 1 ~ 4 time;
(3) decolour: the feed liquid after ultra-filtration system filters carries out desolventing technology, decolorizer to be mass fraction be 30% edible hydrogen peroxide, decolorizer addition is 1% ~ 5% of feed grade concentrated phosphatide quality, and bleaching time is 20 ~ 60 minutes, and bleaching temperature is 30 ~ 80 DEG C;
(4) adsorption treatment: the feed liquid after desolventing technology carries out adsorption treatment, adsorbent is diatomite, active carbon or atlapulgite, adsorbent addition is 1% ~ 5% of feed grade concentrated phosphatide quality, and adsorption time is 30 minutes ~ 60 minutes, and adsorption temp is 30 ~ 80 DEG C;
(5) secondary centrifuging: the feed liquid after adsorption treatment, under centrifugal rotational speed is 3000 ~ 4500rpm condition, carries out secondary centrifuging process in centrifugal 10 ~ 30 minutes;
(6) evaporation and concentration: the feed liquid after secondary centrifuging process carries out Vacuum film evaporation, evaporating temperature is 80 ~ 95 DEG C, and residual voltage is less than 0.09Mpa, and evaporation time is 60 ~ 180 minutes, remove solvent and excessive moisture, obtain high-quality food-level concentrated soybean phospholipid.
2. method according to claim 1, is characterized in that, the mass ratio of step (1) feed grade soybean lecithin and n-hexane is 1:4, and centrifugal pretreatment condition is 4500rpm, centrifugal 20 minutes.
3. method according to claim 1, is characterized in that, the filtering accuracy of step (2) ultra-filtration system is 0.4 μm, and discharge velocity is 25ml/min, and feeding temperature is 40 DEG C, and filtering times is 2 times.
4. method according to claim 1, is characterized in that, step (3) hydrogen peroxide addition is 2% of concentrated phosphatide quality, decolours 40 minutes at 50 DEG C.
5. method according to claim 1, is characterized in that, step (6) 90 DEG C, under residual voltage is less than 0.09MPa condition, Vacuum film evaporation obtains the high food-grade phosphatide of transparency for 2 hours.
6. according to the food-level concentrated soybean phospholipid that the arbitrary described method of claim 1-5 prepares.
CN201510431196.4A 2015-07-21 2015-07-21 Multi-step coupling method to prepare concentrated phospholipids with a high transparency Pending CN105010721A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108003187A (en) * 2016-11-01 2018-05-08 中粮集团有限公司 A kind of method for preparing transparent concentrating soya lecithin
CN112851707A (en) * 2021-01-22 2021-05-28 浙江省粮食科学研究所有限责任公司 Method for preparing high-quality soybean concentrated phospholipid by combined progressive filtration

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108003187A (en) * 2016-11-01 2018-05-08 中粮集团有限公司 A kind of method for preparing transparent concentrating soya lecithin
CN112851707A (en) * 2021-01-22 2021-05-28 浙江省粮食科学研究所有限责任公司 Method for preparing high-quality soybean concentrated phospholipid by combined progressive filtration

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Application publication date: 20151104