CN104839230A - Preparation method of plant-source algicide - Google Patents

Preparation method of plant-source algicide Download PDF

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Publication number
CN104839230A
CN104839230A CN201510188039.5A CN201510188039A CN104839230A CN 104839230 A CN104839230 A CN 104839230A CN 201510188039 A CN201510188039 A CN 201510188039A CN 104839230 A CN104839230 A CN 104839230A
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China
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algicide
macleaya
absolute
ethyl alcohol
fruit pod
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CN201510188039.5A
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Chinese (zh)
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邵继海
李锦龙
陈安伟
彭亮
吴根义
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Hunan Agricultural University
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Hunan Agricultural University
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Abstract

The invention relates to a method for extracting a biological-source algaecidal substance from plant macleaya cordata or/and macleaya microcarpa fruit pods. The method comprises the following steps: firstly crushing macleaya cordata or/and macleaya microcarpa fruit pods by a pulverizer, extracting by the use of absolute methanol or anhydrous ethanol, and carrying out rotary evaporation on an organic solvent in the extract liquid to obtain a dry extract; and finally dissolving the extract in dimethylsulfoxide to obtain the plant-source algicide. Less than millesimal volume of the plant-source algicide is added into a water-blooming cyanobacteria culture system, thus effectively inhibiting growth of water-blooming cyanobacteria. It shows through field algae removal tests that the biological-source algicide can effectively remove water-blooming cyanobacteria so as to obviously improve water quality. The algaecidal substance comes from traditional Chinese herbal plants and has good biosecurity, environment-friendliness and good application value.

Description

A kind of preparation method of plant resource algicide
Technical field
The present invention relates to the preparation of plant resource algicide, particularly one utilizes macleaya cordata (Macleaya cordata) or/and the plant resource algicide preparation method of macleaya microcarpa Fedde (Macleaya microcarpa) fruit pod, and this algicide is for suppressing water body blue algae growth and removing water body blue algae water bloom.
Background technology
China's poisons in freshwater eutrophication is on the rise, and some large-size lake, aquaculture system and city appearance water body have successively broken out serious blue-green alga bloom.In water body, blue-green algae amount reproduction, accumulation and aerobic decomposition can reduce Dissolved Oxygen in Water, cause the aquatic animals such as fishes and shrimps dead, reduce aqueous bio diversity, and many bloom blue algaes can discharge cyanophycean toxin to water body, final aquatic products animal safety and the human health of giving brings great harm.
The minimizing technology of current blue-green alga bloom is mainly divided into physical method, chemical method and biological method.In actual applications, because of their difference such as accommodation, condition, respective advantages and disadvantages is all shown.Physics algae-removing method has the methods such as direct filtration process, mechanical removal method, By Bubble-floating Method, ultrasonic removal method, and the advantage of these methods can not bring secondary pollution to environment, and its shortcoming is that power consumption is large except algae effect is bad.Chemical algae removing mainly by adding algicide, algae-inhibiting agent, flocculant etc. to water body, removes the wawter bloom algae in water body.Chemical algae removing is the main method that current small water blue-green algae is removed, although the method has except algae is effective, the advantage of instant effect, but most chemical algae removing agent can bring secondary pollution to environment, and these chemical algae removing agent do not have selectivity to aquatic toxicity effect, often cause the collapse of this water ecosystem after using this kind of algicide.Although biological except algae be a kind of comparatively safe except/control algae mode.But at present the biological shortcoming except/control algae be except/control algae theory is immature, large by such environmental effects, does not have versatility, except algae effect and except in algae speed all not as good as chemical algae removing.So current urgent need is a kind of efficiently, the blue-green alga bloom minimizing technology of environmental protection.
Macleaya cordata is as a kind of traditional Chinese medicine, and existing very long applicating history, has good biological safety.Macleaya cordata fruit pod derives from plant macleaya cordata, belongs to botanical components, has good degradation property in the environment, belong to environmentally friendly botanical material.Lixiviate Algicidal substances from macleaya cordata fruit pod, the biogenic algicide of preparation is a kind of safety and eco-friendly algicide, has good using value.
Summary of the invention
Technical problem to be solved by this invention is, not enough for prior art, provides a kind of safety, and the preparation method of environment amenable plant resource algicide.
For solving the problems of the technologies described above, the technical solution used in the present invention is, with absolute methanol or absolute ethyl alcohol as digestion agent from macleaya cordata or/and extract biogenic algicide macleaya microcarpa Fedde fruit pod powder.
Preparation method's Trace bio-element scheme of a kind of plant resource algicide of the present invention is, first with cracker by macleaya cordata or/and macleaya microcarpa Fedde fruit pod pulverize, the standard adding 50mL absolute methanol or absolute ethyl alcohol according to 5g fruit pod powder again adds absolute methanol or absolute ethyl alcohol in fruit pod powder, then ultrasonic extraction, after ultrasonic extraction terminates, suction filtration on core filter, residue 10mL absolute methanol or absolute ethanol washing, merging filtrate and cleaning solution, rotary evaporation removes absolute methanol or absolute ethyl alcohol on the rotary evaporator, finally extract is dissolved in methyl-sulfoxide, its final concentration is made to be greater than 10mg/mL, namely plant resource algicide is obtained.Wherein, ultrasonic extraction conditions is: each ultrasonic 10min, work interval 1min, all times 60min.
A large amount of extraction schemes of the preparation method of a kind of plant resource of the present invention algicide are, first with cracker by macleaya cordata or/and macleaya microcarpa Fedde fruit pod pulverize, the standard adding 50mL absolute methanol or absolute ethyl alcohol according to 5g fruit pod powder again adds absolute methanol or absolute ethyl alcohol in fruit pod powder, then dark surrounds lixiviate 12 hours, mechanical agitation is aided with during lixiviate, after extraction terminates, leaching liquor first uses filtered through gauze, obtain just filtrate, first filtrate is filtered with glass fibre cotton again, obtain smart filtrate, the method of essence filtrate rotary evaporation in vacuo removes organic solvent, finally extract is dissolved in methyl-sulfoxide, its final concentration is made to be greater than 10mg/mL, namely plant resource algicide is obtained, the absolute methanol distilled or absolute ethyl alcohol recycle and reuse.
In such scheme, described cracker adopts 8 order crackers.
Compared with prior art, the advantage of the invention is:
What 1, the present invention relates to removes algae material for deriving from the extract of Chinese herbal medicine (macleaya cordata is or/and macleaya microcarpa Fedde fruit pod), has good biological safety.
2, the plant resource algicide prepared of the inventive method, is easy to degraded in the environment, belongs to environmentally friendly algicide.
Accompanying drawing explanation
Fig. 1 is that absolute ethyl alcohol extracts the algicide prepared of macleaya cordata fruit pod to the inhibition of blue algae growth.
Fig. 2 is that absolute methanol extracts the algicide prepared of macleaya cordata fruit pod to the inhibition of blue algae growth.
Fig. 3 is that absolute methanol extracts the algicide prepared of macleaya cordata fruit pod to the removal effect of blue-green alga bloom.
Fig. 4 is that absolute methanol extracts the situation of change of the algicide prepared of macleaya cordata fruit pod except water transparency after algae.
Fig. 5 is that absolute methanol extracts the situation of change of the algicide prepared of macleaya cordata fruit pod except water body ammonium nitrogen content after algae.
Fig. 6 is that absolute methanol extracts the situation of change of the algicide prepared of macleaya cordata fruit pod except water body total phosphorus content after algae.
Fig. 7 is that absolute methanol extracts the situation of change of the algicide prepared of macleaya cordata fruit pod except chemical oxygen demand of water body (COD) content after algae.
Embodiment
Embodiment 1:
With cracker (8 order) by macleaya cordata (Macleaya cordata) or/and macleaya microcarpa Fedde (Macleaya microcarpa) fruit pod pulverize, take 5g fruit pod powder in 250mL wide-mouth triangular flask, add 50mL absolute methanol wherein, put into KQ2200E type supersonic wave cleaning machine, ultrasonic extraction, ultrasonic extraction conditions is: each ultrasonic 10min, work interval 1min, all times 60min.After extraction terminates, suction filtration on core filter, residue 10mL absolute methanol washs, merging filtrate and cleaning solution, on rotary evaporator RE-3000, rotary evaporation removes absolute methanol, again extract is dissolved in methyl-sulfoxide, makes its final concentration be greater than 10mg/mL (mass/volume), namely obtain the plant resource algicide that methyl alcohol extracts preparation.
Embodiment 2:
With cracker (8 order) by macleaya cordata (Macleaya cordata) or/and macleaya microcarpa Fedde (Macleaya microcarpa) fruit pod pulverize, take 5g fruit pod powder in 250mL wide-mouth triangular flask, add 50mL absolute ethyl alcohol wherein, put into KQ2200E type supersonic wave cleaning machine, ultrasonic extraction, ultrasonic extraction conditions is: each ultrasonic 10min, work interval 1min, all times 60min.After extraction terminates, suction filtration on core filter, residue 10mL absolute ethanol washing, merging filtrate and cleaning solution, on rotary evaporator RE-3000, rotary evaporation removes absolute ethyl alcohol, again extract is dissolved in methyl-sulfoxide, makes its final concentration be greater than 10mg/mL (mass/volume), namely obtain plant resource algicide prepared by alcohol extract.
Laboratory algal control test: for preparing by embodiment 1 and embodiment 2 derives from macleaya cordata or/and the algicide of macleaya microcarpa Fedde fruit pod suppresses the growth of microcystic aeruginosa.
Produce malicious bloom blue algae kind: microcystic aeruginosa (Microcystis aeruginosa PCC7806)
Algae culture medium: CT medium
Algal control test method: test and carry out in the triangular flask of 250mL, getting the algicide of variable concentrations that 100 μ L derive from macleaya cordata fruit pod joins in aseptic CT medium, separately get 100 μ L methyl-sulfoxides and do blank, again respectively to wherein adding the microcystic aeruginosa M.aeruginosa PCC7806 being in exponential phase cultivated with CT, final volume is 100mL, the ultimate density of algicide deriving from macleaya cordata fruit pod is 0,1,2.5,4,5.5mg/L (be as the criterion with extract dry weight and calculate), the initial OD of M.aeruginosa PCC7806 680value is 0.196.All process are all placed in light intensity 30 μm of olprotons/ (m 2s 1), temperature 25 ± 1 DEG C, cultivates under photoperiod 12h:12h (L:D) condition, in sampling in the 2nd, 4,6 day of experiment.Frustule chlorophyll 80% acetone extraction measures.The growing state of this algae of different disposal group is reflected with the situation of change of culture chlorophyll content.
Algal control result of the test: as shown in Fig. 1 (absolute ethyl alcohol extracting method) and Fig. 2 (absolute methanol extracting method), after adding to microcystic aeruginosa M.aeruginosa PCC7806 cultivating system the algicide deriving from macleaya cordata fruit pod, when algicide additive capacity is 1mg/L, the biomass of M.aeruginosa PCC7806 and remarkable in contrast, along with the passing of incubation time, the depression effect of this algicide to M.aeruginosa PCC7806 is also more and more obvious, and along with the increase of additive capacity, the depression effect of this algicide to M.aeruginosa PCC7806 is also more and more stronger.
Embodiment 3:
By macleaya cordata or/and macleaya microcarpa Fedde fruit pod cracker (8 order) is pulverized, take 5Kg fruit pod powder in 100L Plastic Drum, add 50L absolute methanol wherein, dark lixiviate 12 hours, is aided with mechanical agitation during lixiviate.After extraction terminates, leaching liquor first uses filtered through gauze, obtain just filtrate, first filtrate is filtered with glass fibre cotton again, obtains smart filtrate, and the method for smart filtrate rotary evaporation in vacuo removes methyl alcohol, again extract is dissolved in methyl-sulfoxide, make its final concentration be greater than 10mg/mL (mass/volume), namely obtain plant resource algicide, the methyl alcohol distilled recycles and reuses.
Field is except algae test: the field water chosen just breaks out blue-green alga bloom, and main blue-green algae kind is wherein Microcystis aeruginosa.2 × 2 × 2m is built at this water body 3enclose lattice, enclosure material is that food plastic level processes.Add the algicide deriving from macleaya cordata fruit pod of embodiment 3 wherein, make the final concentration of algicide be 8mg/L (be as the criterion with extract dry weight and calculate), and contrast is set.Monitoring water body chlorophyll alpha, ammonium nitrogen, total phosphorus and chemical oxygen demand (COD) content, continue 31 days.
Except algae result of the test: find by continuing to monitor algae and water Chlorophyll-a Content, add derive from macleaya cordata fruit pod algicide enclosure in water body Chlorophyll-a Content significantly lower than contrast (see Fig. 3), illustrate that this algicide has good removal effect to blue-green alga bloom.And within the experimental period of 1 month, the blue alga biomass adding the processed group of the algicide deriving from macleaya cordata fruit pod is all extremely remarkable in control group (T test Analysis, P<0.01).Continue to monitor the transparency of water body, the enclosure water transparency finding to add this algicide within the experimental period of 1 month is significantly higher than contrast (see Fig. 4).Although to the monitoring result of water body ammonia nitrogen content find the processed group of adding this algicide in 1-3 days of test higher than contrast, and to after the 5th day, add the processed group ammonia nitrogen content of this algicide all lower than control group (see Fig. 5).The monitoring result of water body total phosphorus content is found, in the processed group of adding this algicide the 3rd day of test higher than contrast, and at the 24-31 days of experimental period, add the processed group total phosphorus content of this algicide all lower than control group (see Fig. 6).The variation tendency of water body COD content is similar with the variation tendency of total phosphorus, at the 3rd day of test, add the processed group water body COD content of this algicide higher than contrast, and the 10th day and 24-31 days testing, add the processed group total phosphorus content of algicide all lower than control group (see Fig. 7).

Claims (6)

1. a preparation method for plant resource algicide, is characterized in that, with absolute methanol or absolute ethyl alcohol as digestion agent from macleaya cordata or/and extract biogenic algicide macleaya microcarpa Fedde fruit pod powder.
2. the preparation method of a kind of plant resource algicide according to claim 1, it is characterized in that, first with cracker by macleaya cordata or/and macleaya microcarpa Fedde fruit pod pulverize, the standard adding 50mL absolute methanol or absolute ethyl alcohol according to 5g fruit pod powder again adds absolute methanol or absolute ethyl alcohol in fruit pod powder, then ultrasonic extraction, after ultrasonic extraction terminates, suction filtration on core filter, residue 10mL absolute methanol or absolute ethanol washing, merging filtrate and cleaning solution, by the absolute methanol in leaching liquor or absolute ethyl alcohol rotary evaporation, obtain lixiviate dry matter, finally extract is dissolved in methyl-sulfoxide, its final concentration is made to be greater than 10mg/mL, namely plant resource algicide is obtained.
3. the preparation method of a kind of plant resource algicide according to claim 2, it is characterized in that, ultrasonic extraction conditions is: each ultrasonic 10min, work interval 1min, all times 60min.
4. the preparation method of a kind of plant resource algicide according to claim 2, is characterized in that, described cracker adopts 8 order crackers.
5. the preparation method of a kind of plant resource algicide according to claim 1, it is characterized in that, first with cracker by macleaya cordata or/and macleaya microcarpa Fedde fruit pod pulverize, the standard adding 50mL absolute methanol or absolute ethyl alcohol according to 5g fruit pod powder again adds absolute methanol or absolute ethyl alcohol in fruit pod powder, then dark surrounds lixiviate 12 hours, mechanical agitation is aided with during lixiviate, after extraction terminates, leaching liquor first uses filtered through gauze, obtain just filtrate, first filtrate is filtered with glass fibre cotton again, obtain smart filtrate, the method of essence filtrate rotary evaporation in vacuo removes absolute methanol or absolute ethyl alcohol, finally extract is dissolved in methyl-sulfoxide, its final concentration is made to be greater than 10mg/mL, namely plant resource algicide is obtained, the absolute methanol distilled or absolute ethyl alcohol recycle and reuse.
6. the preparation method of a kind of plant resource algicide according to claim 5, is characterized in that, described cracker adopts 8 order crackers.
CN201510188039.5A 2014-11-28 2015-04-20 Preparation method of plant-source algicide Pending CN104839230A (en)

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CN109179563A (en) * 2018-10-16 2019-01-11 天津科技大学 A kind of light intensity chemical algae removing agent

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CN1740175A (en) * 2005-08-29 2006-03-01 长沙世唯科技有限公司 Plumepoppy total alkaloid salt and its prepn and application

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刘秀斌: "博落回属植物中生物碱代谢累积研究", 《中国优秀硕士学位论文全文数据库 农业科技辑》 *
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Application publication date: 20150819