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Extraction and purification method of pyrrolo[1,2-a]pyrazine-1,4-dione, hexahydro-3-(2-methylpropyl) from euphausia superba and detection method

An Antarctic krill and purification method technology, applied in the direction of measuring devices, organic chemistry, instruments, etc., can solve the problems of finding Cyclo, etc., and achieve the effect of simple extraction and purification steps and cheap and easy-to-obtain reagents

Inactive Publication Date: 2017-01-04
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no research report on finding Cyclo(Pro-Leu) from Antarctic krill

Method used

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  • Extraction and purification method of pyrrolo[1,2-a]pyrazine-1,4-dione, hexahydro-3-(2-methylpropyl) from euphausia superba and detection method
  • Extraction and purification method of pyrrolo[1,2-a]pyrazine-1,4-dione, hexahydro-3-(2-methylpropyl) from euphausia superba and detection method
  • Extraction and purification method of pyrrolo[1,2-a]pyrazine-1,4-dione, hexahydro-3-(2-methylpropyl) from euphausia superba and detection method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Weigh 100 g of freeze-dried Antarctic krill, add 800 ml of methanol, and extract under reflux at 70° C. for 7 times, each time for 1 hour, until the extract is colorless. After filtration, the filtrate was rotary evaporated to obtain a methanol paste. Add diethyl ether to the methanol paste for leaching 4 times, 1 hour each time, and filter to obtain the ether extract; the ether extract is concentrated by rotary evaporation to obtain the ether extract. Diethyl ether extract is dissolved in an appropriate amount of ether to obtain ether extract, and the mass volume ratio of said ether extract to ether is 1g:10ml; then add 10 times the volume fraction of ether extract and be 2% H 2 SO 4 The aqueous solution was stirred and extracted, and the layers were separated to obtain an acidic aqueous layer. Add an equal volume of chloroform to the acidic aqueous layer, magnetically stir and extract 3 times, each time for 1 h, and stand still for liquid separation to obtain the ch...

Embodiment 2

[0038] Weigh 100 g of freeze-dried Antarctic krill, add 1000 ml of methanol, and extract under reflux at 85° C. for 8 times, each time for 1 hour, until the extract is colorless. After filtration, the filtrate was rotary evaporated to obtain a methanol paste. Add diethyl ether to the methanol extract and extract 5 times, 1 hour each time, and filter to obtain ether extract; the ether extract is concentrated by rotary evaporation to obtain ether extract. Diethyl ether extract is dissolved in an appropriate amount of ether to obtain ether extract, and the mass volume ratio of said ether extract to ether is 1g:10ml; then add 30 times the volume fraction of ether extract and be 1% H 2 SO 4 The aqueous solution was stirred and extracted, and the liquid was separated to obtain an acidic aqueous layer. Add an equal volume of chloroform to the acidic aqueous layer, magnetically stir and extract 4 times, each time for 1 h, and stand still for liquid separation to obtain the chlorofor...

Embodiment 3

[0041] Weigh 100 g of freeze-dried Antarctic krill, add 600 ml of methanol, and extract under reflux at 80° C. for 9 times, each time for 1 hour, until the extract is colorless. After filtration, the filtrate was rotary evaporated to obtain a methanol paste. Add diethyl ether to the methanol paste for leaching 6 times, 1 hour each time, and filter to obtain the ether extract; the ether extract is concentrated by rotary evaporation to obtain the ether extract. Diethyl ether extract is added with ether to dissolve to obtain ether extract, the mass volume ratio of said ether extract to ether is 1g:10ml; add 30 times the volume fraction of ether extract and be 3% H 2 SO 4 The aqueous solution was stirred and extracted, and the layers were separated to obtain an acidic aqueous layer. Add an equal volume of chloroform to the acidic aqueous layer, magnetically stir and extract 3 times, each time for 1 h, and stand still for liquid separation to obtain the chloroform layer A. Add a...

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Abstract

The invention discloses an extraction and purification method of pyrrolo[1,2-a]pyrazine-1,4-dione, hexahydro-3-(2-methylpropyl) (Cyclo(Pro-Leu)) from euphausia superba and a detection method. The extraction method comprises: adding methanol into euphausia superba for reflux extraction and performing filtration to obtain a filtrate; evaporating and concentrating the filtrate to obtain a methanol extract; adding methanol paste into ether for extraction and performing filtration to obtain an ether liquid; evaporating the ether liquid to obtain an ether extract; dissolving the ether extract in a proper amount of ether to obtain an ether extract liquid, adding a sulfuric acid aqueous solution for stirring and extraction to obtain an acid water layer; adding chloroform to the acid water layer for extraction, and performing standing and liquid separation to obtain a chloroform layer A; adding a sodium hydroxide aqueous solution to the chloroform layer A for extraction, and performing standing and liquid separation to obtain an alkaline water layer and a chloroform layer B; adding NH4Cl to the alkaline water layer, adding chloroform with the same volume for extraction, and performing standing and liquid separation to obtain a chloroform layer C; and evaporating and concentrating the chloroform layer C to obtain a Cyclo(Pro-Leu) sample. Euphausia superba is taken as a raw material and is purified and extracted to obtain Cyclo(Pro-Leu) for detection for the first time. The method has significance to development of euphausia superba.

Description

technical field [0001] The invention relates to an extraction, purification and detection method of pyrrolo[1,2-a]pyrazine-1,4-dione, hexahydro-3-(2-methylpropyl) in Antarctic krill, which belongs to food , pharmaceuticals and chemical industry. Background technique [0002] Antarctic krill (Euphausia superba Dana), belonging to the phylum Arthropoda, Crustacea, and Order Krill, is small in size, generally about 5.5-6.0cm in length, and about 2g in weight. There are few species of Antarctic organisms, but the number is huge, and the food chain is relatively simple. Antarctic krill, which feeds on phytoplankton, is the main food of whales, seals, penguins and other carnivores, and is also the basis of the Antarctic food chain. Antarctic krill is one of the largest and most successful single species of biological resources on the earth, with a biological reserve of about 6.5×10 8 ~10×10 8 tons, the latest estimate is 3.79×10 8 Ton. Antarctic krill is nutritious and rich ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/04G01N30/02
CPCC07D487/04G01N30/02
Inventor 王翩翩刘代成
Owner SHANDONG NORMAL UNIV
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