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Method for extracting paralytic shellfish toxins from shell raw materials

A shellfish toxin and shellfish technology, applied in the direction of organic chemistry, can solve the problems of geographical restrictions, low toxin content, and difficulty in extracting pure samples, etc., and achieve the effects of easy acquisition, improved extraction rate, and low processing temperature

Inactive Publication Date: 2015-09-02
INST OF AGRO FOOD SCI & TECH CHINESE ACADEMY OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For the extraction of paralytic shellfish toxins, the method of cultivating toxin-producing algae in seawater is generally adopted, but this has certain geographical restrictions.
However, the toxins extracted from shellfish tissue, due to the low content of such toxins, are easily affected by shellfish substrate substances such as protein, fat, sugar and other substances during the extraction and concentration process, and it is difficult to extract to a relatively high purity. of samples for toxin-related studies

Method used

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  • Method for extracting paralytic shellfish toxins from shell raw materials
  • Method for extracting paralytic shellfish toxins from shell raw materials

Examples

Experimental program
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Embodiment 1

[0034] 1) Thaw the frozen Ezo scallop under running water, take the gonad and drain it, and weigh 1 kg. Homogenize with a homogenizer, put it into a beaker with a volume of 3 liters, add 1 liter of 0.1M acetic acid aqueous solution, stir well until the pH value of the mixture is 3, and use an ultrasonic breaker to crush for 10 minutes under the condition of 600W power , then heated in boiling water for 5 minutes, filtered with four layers of medical gauze after cooling, and collected the filtrate;

[0035] 2) Concentrate the filtrate obtained in step 1) under reduced pressure with a vacuum rotary evaporator until it reaches 0.3 liters, then refrigerate and centrifuge at 4°C for 10 minutes at 4000 rpm and a centrifugal radius of 5 cm, take the supernatant and put it in a separatory funnel. 150mLCHCl3 extracted twice to remove some fatty substances. Take the upper layer extract and mix it with 300mL ethanol, stir at room temperature for 24 hours, then perform a second centrifug...

Embodiment 2

[0041] 1) Remove the shell of the luxurious Chlamys farreri and take its gonads, drain and weigh 1 kg. Homogenize with a homogenizer, put it into a beaker with a volume of 3 liters, add 1 liter of 0.1M acetic acid aqueous solution, stir well until the pH value of the mixture is 2, and use an ultrasonic breaker to crush for 8 minutes under the condition of 600W power , then heated in boiling water for 10 minutes, filtered with four layers of medical gauze after cooling, and collected the filtrate;

[0042] 2) Concentrate the filtrate obtained in step 1) under reduced pressure with a vacuum rotary evaporator until it reaches 0.3 liters, then refrigerate and centrifuge at 4°C for 10 minutes at 5000 rpm and a centrifugal radius of 5 cm, take the supernatant and put it in a separatory funnel. Extract twice with 150mLCHCl3 to remove some fatty substances. Take the upper layer extract and mix it with 300mL ethanol and stir it at room temperature for 24 hours, then perform a second c...

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Abstract

The invention discloses a method for extracting paralytic shellfish toxins from shell tissues. The method comprises the following steps: 1, mixing shell raw materials with acetic acid until the pH value of the obtained mixture is 2-4, carrying out ultrasonic crushing, heating the crushed mixture in boiling water for 5-10min, cooling, filtering, and collecting the obtained filtrate; 2, carrying out reduced pressure concentration on the filtrate, freezing, centrifuging, taking the obtained supernatant, extracting the supernatant by using trichloromethane, uniformly mixing the obtained upper layer extract liquid with ethanol, stirring at room temperature for 20-24h, carrying out secondary centrifuge, collecting the obtained new supernatant, carrying out reduced pressure concentration, drying, dissolving the obtained dried material in acidic methanol, filtering, collecting the obtained new filtrate, drying, dissolving the dried new filtrate in an aqueous acetic acid solution with the pH value of 2-4, adding the obtained sample to a gel column, carrying out column chromatography, and collecting the fraction with the retention time of 160-250min. The method maximally improves the extraction rate of the paralytic shellfish toxins, can effectively remove fats, proteins, carbohydrates and other impurities in the tissues, and maximally reduces the bioactive loss of the toxins.

Description

technical field [0001] The invention belongs to the field of organic compound extraction, in particular to a method for extracting paralytic shellfish toxin from shellfish raw materials. Background technique [0002] Paralytic shellfish poisoning toxins (PSP) are a type of marine biotoxins that can paralyze the human nervous system. They are mainly produced by toxic dinoflagellates and can pass through the food chain in shellfish, such as: emerald mussels, ctenophores Bioaccumulation and amplification of scallop, scallop, meretrix meretrix, green clam, near river oyster and snail. When people accidentally eat these poisoned seafood, poisoning or death will occur. The distribution of paralytic shellfish toxin is more and more widespread in the world, and the frequency is getting higher and higher. There are 2000 poisoning incidents every year, and the mortality rate reaches 15%. PSP toxin is a class of tetrahydropurine derivatives derived from saxitoxin (STX) as the skeleto...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/20
Inventor 张松山哈益明靳静李庆鹏杨宝路李咏富李珍耿乙文
Owner INST OF AGRO FOOD SCI & TECH CHINESE ACADEMY OF AGRI SCI
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