CN101462779B - Preparation of Gymnodinium breve inhibitor - Google Patents

Preparation of Gymnodinium breve inhibitor Download PDF

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Publication number
CN101462779B
CN101462779B CN2009100138364A CN200910013836A CN101462779B CN 101462779 B CN101462779 B CN 101462779B CN 2009100138364 A CN2009100138364 A CN 2009100138364A CN 200910013836 A CN200910013836 A CN 200910013836A CN 101462779 B CN101462779 B CN 101462779B
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China
Prior art keywords
inhibitor
preparation
gymnodinium breve
ethyl acetate
gymnodinium
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Expired - Fee Related
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CN2009100138364A
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Chinese (zh)
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CN101462779A (en
Inventor
王震宇
田志佳
李锋民
别聪聪
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Ocean University of China
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Ocean University of China
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Abstract

The invention relates to a method for preparing a Gymnodinium breve inhibitor and belongs to the field of treatment of marine red tide. The method comprises the following preparation steps: firstly, a large-scale alga ulva pertusa material is pulverized and leached through anhydrous ethanol, usually, each kilogram of the ulva pertusa material uses 2 to 5 liters of the anhydrous ethanol to obtain an extract; secondly, cream obtained through condensation of the extract is dissolved in water; a supernatant fluid is taken out, is extracted through petroleum ether and is delaminated to obtain a water phase substance; and the water phase substance is extracted with n-butyl alcohol and is delaminated to obtain a water phase substance; and finally, the water phase substance is extracted with acetic ether; and the obtained acetic ether phase is the Gymnodinium breve inhibitor. The inhibitor with the concentration of between 8 and 10 milligram/litre has optimal inhibition ratio on Gymnodinium breve. The preparation method has a simple process, low preparation cost and no organic pollution; and the used reagent has low price and lower toxicity.

Description

A kind of preparation method of Gymnodinium breve inhibitor
Technical field
The invention belongs to the marine red tide process field, particularly a kind of preparation method of Gymnodinium breve inhibitor.
Background technology
The method of administering marine red tide is a lot, mainly is divided into physics method, chemical method and biological process.Wherein the physics method mainly is to adopt the method for machinery, and it is by the planktonic algae of excessive multiplication in machine or the artificial filtering seawater, and these class methods are time-consuming, effort, expense is higher and very difficult big area is used.Chemical method is mainly by adding inhibitor (cupric ion Cu commonly used in water body 2+Or weedicide), but this class inhibitor can cause secondary pollution, and other hydrobiological existence is constituted a threat to, and destroys the Marine ecosystems balance.The most requirement of the extracting method that the allelochemical that suppresses the algae effect is arranged of report used expensive reagent, separator column etc. at present, and its cost height.
Summary of the invention
The purpose of this invention is to provide a kind of from kelp extraction separation be the method for the red tide alga inhibitor of main component---the preparation method of Gymnodinium breve inhibitor with the allelochemical, to remedy the deficiencies in the prior art.
It is characterized in that this method comprises the steps:
1) kelp hole sea lettuce material is pulverized the back with dehydrated alcohol lixiviate 1-8 hour, filtered, obtain extracting solution;
2) said extracted liquid is carried out concentrating under reduced pressure and obtain paste, use the dissolved in distilled water paste again, get its supernatant liquor;
3) described supernatant liquor is extracted with sherwood oil after, get aqueous-phase material;
4) described aqueous-phase material is used n-butanol extraction again, get aqueous-phase material;
5) with 4) described in the aqueous-phase material ethyl acetate extraction, get the ethyl acetate phase, the gained ethyl acetate is the algae-inhibiting agent that can suppress Gymnodinium breve growth mutually.
Per kilogram hole sea lettuce is with 2~5 liters of dehydrated alcohol lixiviates in step 1).
In step 2) described in obtain supernatant liquor and the two-part method of precipitation is with the dissolved in distilled water paste: with behind the dissolved in distilled water paste, adopt centrifugal method that supernatant liquor is separated with throw out.
Should adopt boiling range at the supernatant liquor described in the step 3) is that 30~60 ℃ sherwood oil extracts.
Using inhibitor concentration of the present invention is 8~10 mg/litre, to inhibiting rate the best of Gymnodinium breve.
It is simple that the method for the invention has technology, and expense is low, advantages such as agents useful for same cheapness and low toxicity.
Embodiment
The present invention at first pulverizes hole sea lettuce material the back and use the dehydrated alcohol lixiviate, obtains extracting solution, and common per kilogram hole sea lettuce material is with 2~5 liters of dehydrated alcohols;
Again extracting solution is adopted methods such as reduction vaporization, drying to concentrate, obtain paste.Use the dissolved in distilled water paste again,, obtain supernatant liquor and precipitation two portions with whizzer under 5000 rev/mins of conditions centrifugal 10 minutes;
With the supernatant liquor boiling range is that 30~60 ℃ sherwood oil extracts, the water intaking phase;
Again with the above-mentioned water n-butanol extraction that obtains, the water intaking phase;
With the above-mentioned water ethyl acetate extraction that obtains, obtaining ethyl acetate promptly is the inhibitor that suppresses the Gymnodinium breve growth mutually again.
Embodiment 1
After at first will pulverizing 500 gram hole sea lettuce is with 1 premium on currency extraction using alcohol, back dissolved in distilled water again contracts its extracting solution, supernatant liquor is respectively 30~60 ℃ sherwood oil, propyl carbinol and ethyl acetate extraction successively with boiling range, and the ethyl acetate that obtains contains the algae-inhibiting agent that can suppress the Gymnodinium breve growth in mutually.Algae-inhibiting agent added containing in the water body of Gymnodinium breve, when algae-inhibiting agent concentration is 8 mg/litre, is 90% to the inhibiting rate of Gymnodinium breve.
Embodiment 2
With 1 kilogram of hole sea lettuce after pulverizing with 5 liters of dehydrated alcohol extraction, again its extracting solution is concentrated the back dissolved in distilled water, supernatant liquor is respectively 30~60 ℃ sherwood oil, propyl carbinol and ethyl acetate extraction successively with boiling range, and the ethyl acetate that obtains contains the inhibitor that can suppress the Gymnodinium breve growth in mutually.Utilizing this algae-inhibiting agent to suppress the growth of Gymnodinium breve in seawater, when algae-inhibiting agent concentration is 10 mg/litre, is 98% to the inhibiting rate of Gymnodinium breve.
Sherwood oil is the series product with different boiling ranges temperature range, and employed sherwood oil is to select boiling range minimum among the present invention, is the product of 30~60 ℃ temperature range, to save time, cuts down the consumption of energy.

Claims (6)

1. the preparation method of a Gymnodinium breve inhibitor is characterized in that this method comprises the steps:
1) kelp hole sea lettuce material is pulverized the back with dehydrated alcohol lixiviate 1-8 hour, filtered and obtain extracting solution;
2) extracting solution is concentrated obtain paste, and use the dissolved in distilled water paste again, obtain supernatant liquor and precipitation two portions;
3) with described supernatant liquor petroleum ether extraction, get aqueous-phase material;
4) with described aqueous-phase material n-butanol extraction, get aqueous-phase material;
5) with 4) described in the aqueous-phase material ethyl acetate extraction, get the ethyl acetate phase, the gained ethyl acetate is Gymnodinium breve inhibitor mutually.
2. preparation method according to claim 1 is characterized in that: per kilogram hole sea lettuce material is with 2~5 liters of dehydrated alcohol lixiviates in step 1).
3. preparation method according to claim 1 is characterized in that: it is that 30~60 ℃ sherwood oil extracts that the supernatant liquor described in the step 3) should adopt boiling range.
4. preparation method according to claim 1 is characterized in that propyl carbinol described in the step 4) and water volume ratio are 1: 1~1: 20.
5. preparation method according to claim 1 is characterized in that ethyl acetate described in the step 5) and water volume ratio are 1: 1~1: 5.
6. the application of the Gymnodinium breve inhibitor of claim 1 preparation, using this inhibitor concentration is 8~10 mg/litre, to inhibiting rate the best of Gymnodinium breve.
CN2009100138364A 2009-01-09 2009-01-09 Preparation of Gymnodinium breve inhibitor Expired - Fee Related CN101462779B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2009100138364A CN101462779B (en) 2009-01-09 2009-01-09 Preparation of Gymnodinium breve inhibitor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2009100138364A CN101462779B (en) 2009-01-09 2009-01-09 Preparation of Gymnodinium breve inhibitor

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CN101462779A CN101462779A (en) 2009-06-24
CN101462779B true CN101462779B (en) 2011-01-12

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Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103690571B (en) * 2013-12-06 2016-04-13 淮海工学院 From U. pertusa, phenolic acid and alkaloidal method and purposes are prepared in separation and purification
CN105243250A (en) * 2015-11-20 2016-01-13 深圳职业技术学院 Auto-control water source layering water taking method and system based on three-dimensional algae ecology model
CN110063430B (en) * 2019-05-14 2022-09-09 宁波大学 Brown algae extract and application of brown algae extract in inhibiting proliferation of virulent Carlo algae in bait microalgae propagation

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