CN102585033B - Hu shaddock pectin with anti-tumor efficacy and preparation method of hu shaddock pectin - Google Patents
Hu shaddock pectin with anti-tumor efficacy and preparation method of hu shaddock pectin Download PDFInfo
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- CN102585033B CN102585033B CN201110435500.4A CN201110435500A CN102585033B CN 102585033 B CN102585033 B CN 102585033B CN 201110435500 A CN201110435500 A CN 201110435500A CN 102585033 B CN102585033 B CN 102585033B
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Abstract
The invention discloses hu shaddock pectin with anti-tumor efficacy and a preparation method of the hu shaddock pectin, and belongs to the technical field of health product preparation. The preparation method comprises the steps as follows: (1) collection and treatment of raw materials; (2) extraction, filtration and concentration of pectin substances; (3) high-temperature high-pressure treatment; (4) precipitation treatment; (5) washing; and (6) drying, crushing and other steps. The hu shaddock peel pectin that is extracted primarily is treated through high temperature and high pressure, and then the average molecular weight (Mn) of the hu shaddock peel pectin is decreased from 30505 to 17816, so that the hu shaddock peel pectin can be absorbed by human bodies more easily, can adhere to tumor cells and inhibit the proliferation of the tumor cells, and achieves a good anti-tumor effect; the hu shaddock pectin is obtained from natural fruits, thereby being safer; and the hu shaddock pectin and the preparation method can greatly improve the economical utilization value of hu shaddock and can be popularized and applied to hu shaddock production places and enterprises.
Description
Technical field
The present invention relates to the preparing technical field of healthcare products, be specifically related to a kind ofly take Hu shaddock ped or slag and as Raw material processing, there is pectin of antitumor efficacy and preparation method thereof.
Background technology
Recklessly shaddock is shaddock and other citrus natural hybrid species, originates in Changshan County, Zhejiang Province, and because its fruit appearance is similar to little shaddock, therefore named Hu shaddock, has over one hundred year history, for Changshan County, Zhejiang Province exclusive.The correlative study of Zhejiang medical courses in general institute thinks that recklessly shaddock is cool in nature, has relieving cough and reducing sputum, clearing heat and detoxicating, the cough-relieving of promoting the production of body fluid, the restoring consciouness of relieving the effect of alcohol, the easypro stomach that helps digestion, defaecation diuresis, strong kidney moistening lung, the effect of promoting longevity, and is the protective foods of pure natural.
Pectin is one group of polygalacturonic acid, it be generally white to pale yellow powder, be slightly with tart flavour, have water-soluble, its molecular weight approximately 5～300,000 Da, its solution can form gel under optimum conditions.On food, make jelling agent, thickening material, stablizer, suspension agent, emulsifying agent, flavouring synergistic agent, and can be used for makeup, and to protection skin, preventing ultraviolet radiation, wound, all certain effects of tool of beautifying face and moistering lotion are treated in smelting.Though shaddock fruit is rich in pectin substance recklessly, because molecular weight is low, in molecule, free carboxy legibility, from producing negative charge, causes intermolecular mutual repulsion, causes the gelling of pectin product poor, cannot meet practical application request.Meanwhile, because Hu shaddock pectin molecule amount is low, molecular structure is simple, easy Adhesion To Tumor Cells, and suppress the propagation of cell, therefore can be used as good antitumor product application.
Summary of the invention
The present invention seeks to, for the poor characteristic of Hu shaddock pectin gelling, propose a kind ofly to take Hu shaddock ped or slag and become the Hu shaddock pectin of tool antitumor efficacy as Raw material processing, to improve the preparation method of the Hu shaddock pectin of shaddock ped slag for comprehensive utility value recklessly.
The object of the invention is achieved by following technical solution:
Have an antitumor efficacy preparation method for shaddock pectin recklessly, the method is carried out according to the following steps:
(1) collection of raw material and processing: get shaddock ped recklessly or squeeze the juice after Hu shaddock slag be raw material, Hu shaddock ped wherein first carries out fragmentation, then through clear water soak, clear water washing while being colourless to elutant for several times only; Shaddock slag is with after clear water washing 4 times, standby recklessly;
(2) lixiviate of pectin substance, filtration and concentrated: by extremely complete submergence in the hydrochloric acid soln of the Hu shaddock ped after break process or Hu shaddock slag immersion pH2.0～2.5, under 85～98 ℃ of conditions of liquid temperature, lixiviate is 1～3 hour; After lixiviate, filter, collect extracting solution; Adopt vacuum concentration to 40～50% of original volume extracting solution; (3) high temperature high pressure process: concentrated extracting solution is put in high-pressure steam sterilizing pan, processed 10～60 minutes under 115～125 ℃, 0.169～0.232MPa condition;
(4) precipitation process: to adding long-pending 2～6 times of this liquid in high temperature high pressure process liquid, the ethanolic soln of concentration 95%, standing after stirring, until pectin substance, fully precipitate and filter during supernatant liquid clarification, collect filter residue, and break up;
(5) washing: wash after filter residue after breaing up 1～2 time with 95% ethanolic soln, then repeat to filter and break up 1 time according to step (4) technique;
(6) dry, pulverize: the filter residue after step (5) is broken up is put in loft drier, dry to water content for 65 ℃ and reach 8%, after pulverizing shaddock pectin product recklessly.
A kind of Hu shaddock pectin product with antitumor efficacy being made by aforesaid method.
The invention has the beneficial effects as follows:
One, the present invention utilizes the feature that shaddock pectin molecule amount is low recklessly, coagulative power is low, pectin after tentatively extracting is prepared into the pectin product that molecule amount is lower after high temperature high pressure process, and (molecular weight distribution of pomelo-pectin and Hu shaddock slag pectin is shown in respectively accompanying drawing 1 and accompanying drawing 2 recklessly, before and after pyroprocessing, molecular weight contrast is as shown in table 1), easily be absorbed by the body, Adhesion To Tumor Cells, thereby suppress the increment of cell, present good antitumous effect.
Table 1 is shaddock pectin pyroprocessing front and back molecular weight contrast (unit: Da) recklessly
Two, the low molecule pectin of selling is in the market used as cancer therapy drug as the GCS-100 of the PectaSol of the MCP of Centrax Int. company, EcoNugenics company, GlycoGenesys company.Several pectin adopts the chemical processes such as acid-base method, enzyme process to be prepared into low molecule pectin above, and all belongs to external import pectin, expensive, and domestic also some unit is at development low molecule pectin, but quality is unsatisfactory.Therefore produce the active demand that the high-quality pectin with antitumour activity has become domestic market.The pectin product purity that the present invention produces surpasses 75%, and solvability is good, is easily absorbed by the body, anti-tumor activity is high, product extracts from natural phant, and obtains through the modification of physics pyroprocess, and the low molecule pectin making than external chemical method and general chemistry antitumor drug have more security.
Three, to utilize recklessly the processing refuses such as shaddock ped and slag be raw material in the present invention, extracts, is prepared into the Hu shaddock pectin (seeing embodiment 4) with antitumor efficacy, greatly improved economy and the utility value of Hu shaddock.
Accompanying drawing explanation
Fig. 1 is the curve distribution schematic diagram of pomelo-pectin high temperature high pressure process front and back different molecular weight recklessly
Fig. 2 is the curve distribution schematic diagram of shaddock slag pectin high temperature high pressure process front and back different molecular weight recklessly
Embodiment
By following examples, the present invention is described in further detail, but be never that the present invention is imposed any restrictions.
Beet slicer: TW-802 type, Guangzhou Tian Ye Food Machinery Co., Ltd.;
Rotatory evaporator: R1002B type, Shensheng Science & Tech. Co., Ltd., Shanghai;
High-pressure steam sterilizing pan: D-1 type, Beijing Fa En scientific & trading Co., Ltd.;
Electric heating constant-temperature blowing drying box: DHG-9146A type, the grand experimental installation of upper Nereid company limited;
Pulverizer: QE～200 type, the Wuyi County Tools Co., ltd that stands erect.
Embodiment 1:(is pomelo-pectin working method 1 recklessly)
The method is carried out according to the following steps:
(1) collection of raw material and processing: getting shaddock ped is recklessly raw material, is cut into the strip of approximately 5 mm wides with beet slicer, soak, wash when several is colourless to elutant through clear water and stop, standby;
(2) lixiviate of pectin substance, filtration and concentrated: by extremely complete submergence in the hydrochloric acid soln of the Hu shaddock ped bar immersion pH2.0 after processing, under 85 ℃ of conditions of liquid temperature, lixiviate is 2 hours; After lixiviate, filter, collect extracting solution; Adopt rotatory evaporator vacuum concentration to 50% of original volume extracting solution;
(3) high temperature high pressure process: concentrated extracting solution is put in high-pressure steam sterilizing pan, processed 10 minutes under 125 ℃, 0.232MPa condition;
(4) precipitation process: to adding long-pending 6 times of this liquid in high temperature high pressure process liquid, the ethanolic soln of concentration 95%, standing after stirring, until pectin substance, fully precipitate and filter during supernatant liquid clarification, collect filter residue, and break up;
(5) washing: the filter residue after breaing up with 95% ethanolic soln washing 1 time, then filter and break up according to step (4) technique;
(6) dry, pulverize: the filter residue after step (5) is broken up is put in loft drier, dry to water content for 65 ℃ and reach 8%, after pulverizing with pulverizer pomelo-pectin product recklessly.
Embodiment 2:(is pomelo-pectin working method 2 recklessly)
In this example, the lixiviate of step (2) pectin substance, filtration and concentrated: shaddock ped bar immerses in the hydrochloric acid soln of pH2.2 recklessly, and under 98 ℃ of conditions of liquid temperature, lixiviate is 1 hour, and extracting solution is concentrated into 40% of original volume; Step (3) high temperature high pressure process: concentrated extracting solution is processed 60 minutes under 115 ℃, 0.169MPa condition; Step (4) precipitation process: add this liquid to amass the ethanolic soln of the concentration 95% of 2 times in high temperature high pressure process liquid; Step (5)) washing: the filter residue after breaing up with 95% ethanolic soln washing 2 times; All the other process are with embodiment 1.
Embodiment 3:(is shaddock slag pectin working method 3 recklessly)
In this example, collection and the processing of step (1) raw material: the Hu shaddock slag of getting after squeezing the juice is raw material, use clear water washing by soaking 4 times; The lixiviate of step (2) pectin substance, filtration and concentrated: shaddock slag immerses in the hydrochloric acid soln of pH2.5 recklessly, and under 90 ℃ of conditions of liquid temperature, lixiviate is 3 hours, and extracting solution is concentrated into 45% of original volume; Step (3) high temperature high pressure process: concentrated extracting solution is processed 30 minutes under 120 ℃, 0.199MPa condition; Step (4) precipitation process: add this liquid to amass the ethanolic soln of the concentration 95% of 4 times in high temperature high pressure process liquid; Step (5) washing: the filter residue after breaing up with 95% ethanolic soln washing 2 times; All the other process are with embodiment 1.
Embodiment 4:(is the anti tumor activity in vitro test of shaddock pectin recklessly)
(1) cell strain and culture condition:
Human prostata cancer PC 3 cells are purchased from Chinese Academy of Sciences's Shanghai cell bank, with the DMEM nutrient solution containing 10% foetal calf serum, 100U/L penicillin and 100mg/L Streptomycin sulphate, in 37 ℃, 5%CO
2and the cultivation of going down to posterity in the incubator of saturated humidity, take the logarithm vegetative period cell for experiment;
(2) tumor cell in vitro propagation inhibition test:
The Hu shaddock pectin (natural product) that embodiment 1,2 or 3 makes is diluted to desired concn with serum-free DMEM before administration, 0.22 μ m membrane filtration degerming.Positive control medicine (synthetic product) is cisplatin injections (DDP), and Jiangsu Haosen Pharmaceutical Co., Ltd produces.
PC 3 cells in vegetative period of taking the logarithm, adjusting concentration of cell suspension is 4 * 10
4/ ml, every hole 100 μ l cell suspension inoculations are in 96 porocyte culture plates, and administration (100 μ l/ hole) after inoculation 24h, establishes respectively blank group, cell control group and 5 concentration Hu shaddock pectin treatment group.After continuing to cultivate 72h, every hole adds 100 μ l MTT (1mg/ml, with DMEM nutrient solution, dissolve), cultivate 4h for 37 ℃, discard and in each hole, after liquid, add 150 μ l acidifying Virahols (containing 0.04mol/L HCl), lucifuge is placed 30min, microplate reader is measured 570nm place absorbancy, calculate the proliferation inhibition rate of shaddock pectin to PC 3 cells recklessly, and the NDST writing with professor Sun Ruiyuan (New Drug Statistical Treatment) computer program calculates the half-inhibition concentration (IC of tested material to tumor cell proliferation (72h)
50).
(3) experimental result:
Shaddock pectin suppresses active IC to PC 3 cells in vitro recklessly
50value (half-inhibition concentration of tested material to tumor cell proliferation (72h)) is as shown in table 2.From this table, the anti-knurl effect of gained pectin of the present invention is better, considers that this product is whole food composition, and safe without toxic side effect, is developed as anti-cancer agent or protective foods is with a wide range of applications.
Table 2 recklessly shaddock pectin suppresses active to PC 3 cells in vitro
Claims (2)
1. there is a recklessly preparation method for shaddock pectin of antitumor efficacy, it is characterized in that the method carries out according to the following steps:
(1) collection of raw material and processing: get shaddock ped recklessly or squeeze the juice after Hu shaddock slag be raw material, Hu shaddock ped wherein first carries out fragmentation, then through clear water soak, clear water washing while being colourless to elutant for several times only; Shaddock slag is with after clear water washing 4 times, standby recklessly;
(2) lixiviate of pectin substance, filtration and concentrated: by extremely complete submergence in the hydrochloric acid soln of the Hu shaddock ped after break process or Hu shaddock slag immersion pH2.0～2.5, under 85～98 ℃ of conditions of liquid temperature, lixiviate is 1～3 hour; After lixiviate, filter, collect extracting solution; Adopt vacuum concentration to 40～50% of original volume extracting solution;
(3) high temperature high pressure process: concentrated extracting solution is put in high-pressure steam sterilizing pan, processed 10～60 minutes under 115～125 ℃, 0.169～0.232MPa condition;
(4) precipitation process: to adding long-pending 2～6 times of this liquid in high temperature high pressure process liquid, the ethanolic soln of concentration 95%, standing after stirring, until pectin substance, fully precipitate and filter during supernatant liquid clarification, collect filter residue, and break up;
(5) washing: wash after filter residue after breaing up 1～2 time with 95% ethanolic soln, then repeat to filter and break up 1 time according to step (4) technique;
(6) dry, pulverize: the filter residue after step (5) is broken up is put in loft drier, dry to water content for 65 ℃ and reach 8%, after pulverizing shaddock pectin product recklessly.
2. the Hu shaddock pectin product with antitumor efficacy being made by claim 1 method.
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