CN105212010A - A kind of water extraction flocculence prepares the method for pine needle natural antiseptic agent - Google Patents
A kind of water extraction flocculence prepares the method for pine needle natural antiseptic agent Download PDFInfo
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- CN105212010A CN105212010A CN201410320914.6A CN201410320914A CN105212010A CN 105212010 A CN105212010 A CN 105212010A CN 201410320914 A CN201410320914 A CN 201410320914A CN 105212010 A CN105212010 A CN 105212010A
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Abstract
The present invention relates to a kind of preparation method of pine needle natural antiseptic agent, be mainly used in food fresh keeping.Be extracted by following technique by pine needle: pine needle clear water is cleaned, dry, add water after pulverizing, boiling waterbath, cross leaching filtrate, add Old Region after being evaporated to finite concentration, after leaving standstill, isolated by filtration or centrifugation, obtain refined liquid.Pine needle natural antiseptic agent i.e. this refined liquid or the pulvis that this refined liquid is made after drying.The extract from pine needles that the present invention obtains has stronger inhibitory action to gram-positive bacteria, Gram-negative bacteria, and extract has good heat endurance, under condition of different pH, all have good antibacterial effect.Compared with traditional aqueous extraction-alcohol precipitation technology, greatly can reduce costs, shorten the production cycle, and extract quality be more stable.The present invention take pine needle as raw material, and wide material sources are with low cost.
Description
Technical field
The extracting method of to be a kind of with pine needle be raw material the produces natural antiseptic agent that the present invention relates to, belongs to food additives field.
Background technology
Food industry has become one of large pillar industry of national economy three, and food is subject to microbial infection and causes corruption in processing, preservation, storage and transport process, not only makes it to lose nutritive value and loss and waste, food poisoning also can be caused to endanger the health of people.At present, the most convenient and economic technological means adds food preservative.
Use the most extensive with the Prof. Du Yucang anticorrisive agent of benzoic acid, sorbic acid and its esters and parabens in food processing at present, but through the discovery that studies for a long period of time, there is certain toxic and side effect and chronic injury to human body in excess and the Use overrun problem of these Prof. Du Yucang anticorrisive agents, such as Japan has completely forbidden the use of Sodium Benzoate at fruits and vegetables, food, medicine, feed and cosmetics.
Natural antiseptic agent, because of its has a broad antifungal spectrum, safety non-toxic, steady performance, becomes a focus of Recent study and exploitation food industry.Natural antiseptic agent is mainly derived from animal, plant and microorganism.The existing seed plant of China about 25700 kinds, pteridophyte more than 2400 is planted, and bryophyte is kind more than 2100, adds up to and has higher plant kind more than 30000, and these plants are that exploitation natural antiseptic agent provides valuable resource.
Pine needle is the needle of Pinaceae pine genus plant as black pine, Chinese pine, Korean pine, Huashan pine, pinus yunnanensis, masson pine etc., is the Main By product of pine tree.Functional components main in pine needle is mainly the materials such as volatile oil, flavone compound, lignanoid, shikimic acid, phenols, and they mostly have antibacterial and anti-inflammation functions.
At present water extraction and alcohol precipitation method mostly is to the method that Plant crude extract is refined, water extract-alcohol precipitation is that solvent decocts raw material with water, add ethanol after concentrated and carry out clarifying treatment to finite concentration, remove the materials such as protein, gelatinized starch, mucilaginous substance, polysaccharide, fat-soluble pigment, finally reclaim ethanol, obtain the extract clarified.But water extraction and alcohol precipitation method complex operation, elapsed time is longer, and finished product stability is poor, cost is higher.
Be used for the patent of food antiseptic about pine needle to have been reported, take pine needle as antiseptics for natural food of raw material and preparation method thereof as patent 200810219943.8 reports a kind of, this method utilizes organic solvent ethyl acetate to extract active component in pine needle; Patent 201210054069.3 reports a kind of extract from pine needles and preparation method thereof, and this method utilizes super-pressure to destroy cell membrane with alcohol extract; Patent 200810162531.5 reports a kind of wet-land pine tree extract from pine needles and for food fresh keeping, adopts extracting in boiling water, obtain light tan powder antistaling agent after vacuum drying.
Summary of the invention
The object of the present invention is to provide a kind of efficiently, the method for antibacterial material in the extraction pine needle of low cost, this extract from pine needles has water-soluble preferably.
For achieving the above object, there is provided following technical scheme: a kind of water extraction flocculence prepares the method for pine needle natural antiseptic agent, take pine needle as raw material, boiling after cleaning, dry, pulverizing, cross leaching filtrate, add Old Region after being evaporated to finite concentration, leave standstill and be separated the refined liquid obtained afterwards.
Its concrete steps comprise:
A) pine needle is cleaned, dries, is pulverized rear boiling, obtains hydrophily extract after filtration;
B) by steps A) described in hydrophily extract reduced pressure concentration, obtain concentrate;
C) step B) described in concentrate add Old Region, leave standstill after be separated to obtain refined liquid.
D) step C) in refined liquid obtain extract from pine needles pulvis after drying.
Further, refined liquid can also make pulvis after drying, and this refined liquid or aforementioned pulvis are pine needle natural antiseptic agent of the present invention.
Further, solid-liquid mass ratio is 1: 5 ~ 15, and decoct temperature 70 ~ 100 DEG C, the time is 30min ~ 1.5h.
Further, filtrate reduced in volume to 1: 1 ~ 1: 10 (ml:g), the temperature of reduced pressure concentration is 50 ~ 80 DEG C.
Further, Old Region comprises chitin, shitosan, ZTC1+1-II type natural clarifying agent, ZTC1+1-III type natural clarifying agent, ZTC1+1-IV type natural clarifying agent, ZTC plant at least one put forward in fining agent.
Further, drying means is the one in spraying dry or freeze drying.
Further, flocculation leave standstill after solid-liquid separating method be at least one in isolated by filtration and centrifugation.
Further, isolated by filtration adopts at least one in filtered through gauze, plate-frame filtering, bag type filtering; Centrifugation adopts at least one in tube centrifuge, horizontal centrifuge, desk centrifuge, butterfly centrifugal machine, and described centrifugal force scope is 10000 ~ 24700 × g.
Further, pine needle is at least one of masson pine, Korean pine, cdear or wet-land pine tree pine needle.
Beneficial effect of the present invention:
1) the present invention adopts water as antimicrobial component in solvent extraction pine needle, avoids the use of organic solvent, ensure that pure natural, and product has good water-soluble, and the scope of application is wider.
2) the present invention adopts the technical scheme of flocculate and clarify, cancels and uses water extraction and alcohol precipitation method, shorten operating procedure and settling time, solve extract viscosity large, the problem of Separation of Solid and Liquid difficulty, and finished product preparation is stablized, can withstand high temperatures sterilization and chilling treatment.Compared with traditional aqueous extraction-alcohol precipitation technology, safety non-pollution, technique is simple, can reduce operation, reduce costs (ethanol), and solve the safety problem of factory.
3) extract from pine needles that the present invention obtains has very strong inhibitory action to common gram positive bacteria, Gram-negative bacteria, heat treatment temperature and pH on its fungistatic effect without impact; Extract from pine needles can be dissolved into the aqueous solution of variable concentrations, be applied to the fresh-keeping of various food.
Detailed description of the invention
Embodiment 1: the preparation method 1 of extract from pine needles
1: get pine needle, after flushing, drain, 45 DEG C of oven dry.
Pine needle after above-mentioned oven dry is pulverized by 2, gets 100g pine needle, adds 1000ml water, at 70 DEG C, extract 1h.
3 cross leaching filtrate, are evaporated to 500ml at 60 DEG C.
4 add ZTC in 500ml concentrate plants and carries fining agent, and leave standstill 6 hours, centrifugal segregation precipitates.
5 get the rear liquid pressure-reducing of flocculation is concentrated into paste, and freeze drying obtains 9.4g extract from pine needles.
The extract from pine needles that the present invention obtains is pale yellow powder, good water solubility.
Embodiment 2: the preparation method 2 of extract from pine needles
1: get pine needle, after flushing, drain, 45 DEG C of oven dry.
Pine needle after above-mentioned oven dry is pulverized by 2, gets 100g pine needle, adds 500ml water, at 70 DEG C, extract 30min.
3 cross leaching filtrate, are evaporated to 100ml at 50 DEG C.
4 add ZTC in 100ml concentrate plants and carries fining agent, and leave standstill 6 hours, centrifugal segregation precipitates.
5 get the rear liquid pressure-reducing of flocculation is concentrated into paste, and freeze drying obtains 7.6g extract from pine needles.
The extract from pine needles that the present invention obtains is pale yellow powder, good water solubility.
Embodiment 3: the preparation method 3 of extract from pine needles
1: get pine needle, after flushing, drain, 45 DEG C of oven dry.
Pine needle after above-mentioned oven dry is pulverized by 2, gets 100g pine needle, adds 1500ml water, decocts to 100 DEG C of extraction 1.5h.
3 cross leaching filtrate, are evaporated to 1000ml at 80 DEG C.
4 add ZTC in 1000ml concentrate plants and carries fining agent, and leave standstill 6 hours, centrifugal segregation precipitates.
5 get the rear liquid pressure-reducing of flocculation is concentrated into paste, and freeze drying obtains 12.3g extract from pine needles.
The extract from pine needles that the present invention obtains is pale yellow powder, good water solubility.
Embodiment 4: the antibacterial activity of extract from pine needles
Escherichia coli are indicator bacterias of people and warm-blooded animal fecal pollution, and salmonella typhimurium is the main pathogenic fungi causing acute gastroenteritis, both belongs to gramnegative bacterium.The enterotoxin that staphylococcus aureus produces is worldwide health problem, a bacillus subtilis energy starch-splitting, and be the main bacterial strain causing rice fermentation, bread mucous modification, both are representatives of gram-positive bacteria.Four kinds of bacterium are common food pollutantbacteria.Mould is usually on citrus and other fruit, and aspergillus niger can cause that the grain that moisture is higher goes mouldy, and the two is the common contaminated mold of food.
As shown in Table 1, extract from pine needles all has inhibitory action in various degree to four kinds of bacteriums, and along with extract concentrations increases, inhibitory action strengthens.As shown in Table 2, extract from pine needles is substantially suitable with chemical preservative Sodium Benzoate to the antibacterial effect of bacterium, and poor to mould inhibitory action.
Table 1 variable concentrations extract from pine needles is to the inhibition zone size (mm) of four kinds of food pollutantbacteria
Table 2 extract from pine needles is to the minimum bactericidal concentration (mg/ml) of food pollutant bacteria
| For examination bacterial classification | Extract from pine needles | Sodium Benzoate |
| Escherichia coli | 3.125 | 4 |
| Bacillus subtilis | 3.125 | 2 |
| Staphylococcus aureus | 3.125 | 4 |
| Salmonella typhimurium | 1.560 | 1 |
| Aspergillus niger (spore) | 60 | 12.5 |
| Mould (spore) | 40 | 12.5 |
Embodiment 5:pH is on the impact of extract from pine needles antibacterial activity
Regulate extract from pine needles pH to be 4.5,5.5,6.5,7.5,8.5, carry out bacteriostatic experiment.Result is as shown in table 3, in the scope of pH4.5 ~ 8.5, finds that the antibacterial activity of extract from pine needles is without significant change.Illustrate that extract from pine needles all can play antibacterial action under condition of different pH.
Under the different pH of table 3, extract from pine needles is to the comparison of Escherichia coli inhibition zone size (mm)
| pH | 4.5 | 5.5 | 6.5 | 7.5 | 8.5 |
| Extract from pine needles | 15.2 | 14.9 | 15.1 | 14.9 | 15 |
| Sterilized water | 0 | 0 | 0 | 0 | 0 |
Embodiment 6: temperature is on the impact of extract from pine needles antibacterial activity
As shown in Table 4, extract from pine needles through 121 DEG C, after the high-temperature process of 15min, still can keep antibacterial activity, illustrate that the antibacterial effect of high temperature on extract from pine needles is without impact, has good heat endurance.
Table 4 temperature is on the impact of extract from pine needles antibacterial (Escherichia coli) activity
| Temperature | Inhibition zone size | Sterilized water contrasts |
| Untreated | 15.6 | 0 |
| 121℃、15min | 15.3 | 0 |
Embodiment 7: the extract from pine needles that the inventive method obtains is to the preservative challenge test of cider
Get fresh apple, clean, peeling, be sub-packed in after squeezing the juice in the blue lid bottle of sterilizing, add extract from pine needles 0.5ml and 2ml respectively; Not add pine needle extract for blank, ambient temperatare is put, and evaluates fruit juice quality, smell, total plate count every 12h.Result is as shown in table 5, and the cider not adding extract from pine needles at 24h is existing obviously rotten, and adds a certain amount of extract from pine needles and have certain fresh-keeping effect, and along with adding increasing of extract amount, corrosion-resistanting fresh-keeping effect is more obvious.
Table 5 extract from pine needles is to the antiseptic effect of cider
Above content is in conjunction with concrete optimal technical scheme further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (10)
1. a water extraction flocculence prepares the method for pine needle natural antiseptic agent, it is characterized in that: take pine needle as raw material, boiling after cleaning, dry, pulverizing, crosses leaching filtrate, add Old Region after being evaporated to finite concentration, leave standstill and be separated the refined liquid obtained afterwards.
2. water extraction flocculence according to claim 1 prepares the method for pine needle natural antiseptic agent, it is characterized in that comprising the steps:
A) pine needle is cleaned, dries, is pulverized rear boiling, obtains hydrophily extract after filtration;
B) by steps A) described in hydrophily extract reduced pressure concentration, obtain concentrate;
C) in step B) add Old Region in described concentrate, be separated to obtain refined liquid after leaving standstill.
D) step C) in refined liquid obtain extract from pine needles pulvis after drying.
3. water extraction flocculence according to claim 1 prepares the method for pine needle natural antiseptic agent, it is characterized in that: described refined liquid can also make pulvis after drying, and this refined liquid or aforementioned pulvis are pine needle natural antiseptic agent of the present invention.
4. water extraction flocculence according to claim 1 prepares the method for pine needle natural antiseptic agent, it is characterized in that: solid-liquid mass ratio is 1: 5 ~ 15, and decoct temperature 70 ~ 100 DEG C, the time is 30min1.5h.
5. water extraction flocculence according to claim 1 prepares the method for pine needle natural antiseptic agent, it is characterized in that: filtrate reduced in volume to 1: 1 ~ 1: 10 (ml:g), and the temperature of reduced pressure concentration is 50 ~ 80 DEG C.
6. method according to claim 1, is characterized in that described Old Region comprises chitin, shitosan, ZTC1+1-II type natural clarifying agent, ZTC1+1-III type natural clarifying agent, ZTC1+1-IV type natural clarifying agent, ZTC plant at least one put forward in fining agent.
7. method according to claim 3, is characterized in that: drying means is the one in spraying dry or freeze drying.
8. method according to claim 1, is characterized in that: the solid-liquid separating method after flocculation leaves standstill is at least one in isolated by filtration or centrifugation.
9. method according to claim 8, it is characterized in that: described isolated by filtration adopts at least one in filtered through gauze, plate-frame filtering, bag type filtering, described centrifugation adopts at least one in tube centrifuge, horizontal centrifuge, desk centrifuge, butterfly centrifugal machine, and centrifugal force scope is 10000 ~ 24700 × g.
10. a kind of pine needle natural antiseptic agent according to claim 1, is characterized in that: described pine needle is masson pine, Korean pine, cdear or wet-land pine tree pine needle.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107198085A (en) * | 2017-05-23 | 2017-09-26 | 合肥师范学院 | A kind of preparation method of lotus leaf natural antiseptic agent |
| CN108378731A (en) * | 2016-08-21 | 2018-08-10 | 王琪 | A kind of walnut opener with preservation |
-
2014
- 2014-07-03 CN CN201410320914.6A patent/CN105212010A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108378731A (en) * | 2016-08-21 | 2018-08-10 | 王琪 | A kind of walnut opener with preservation |
| CN107198085A (en) * | 2017-05-23 | 2017-09-26 | 合肥师范学院 | A kind of preparation method of lotus leaf natural antiseptic agent |
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