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A method for extraction, purification and detection of pyrrolo[1,2-a]pyrazine-1,4-dione, hexahydro-3-(phenylmethyl) in Antarctic krill

An Antarctic krill and purification method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of cheap and easy-to-obtain reagents and simple extraction and purification steps

Active Publication Date: 2018-08-28
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-Phe) from Antarctic krill. Therefore, to study whether Antarctic krill contains Cyclo (Pro-Phe) and its extraction, purification and detection methods will further improve Antarctic krill resources. It is very important to develop and utilize

Method used

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  • A method for extraction, purification and detection of pyrrolo[1,2-a]pyrazine-1,4-dione, hexahydro-3-(phenylmethyl) in Antarctic krill
  • A method for extraction, purification and detection of pyrrolo[1,2-a]pyrazine-1,4-dione, hexahydro-3-(phenylmethyl) in Antarctic krill
  • A method for extraction, purification and detection of pyrrolo[1,2-a]pyrazine-1,4-dione, hexahydro-3-(phenylmethyl) in Antarctic krill

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 100 g of freeze-dried Antarctic krill, add 800 ml of methanol, and extract under reflux at 85° 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 with ether to obtain ether extract, 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 and stir for extraction 6 times, stirring for 1 h each time. After standing still, separate the layers to obtain the chloroform layer A. Ad...

Embodiment 2

[0036]Weigh 100 g of freeze-dried Antarctic krill, add 1000 ml of methanol, and extract under reflux at 70° C. for 8 times, each time for 1.5 h, 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, each time for 1h, and filter to obtain ether extract; the ether extract is concentrated by rotary evaporation to obtain ether extract. Diethyl ether extract is dissolved in ether to obtain ether extract, the mass volume ratio of said ether extract to ether is 1g:10ml; add 10 times the volume fraction of ether extract and then add 1% 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 and stir for extraction 6 times, stirring for 1 h each time. After standing still, separate the layers to obtain the chloroform layer A. Add an equa...

Embodiment 3

[0039] 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 2 hours, 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, each time for 0.5h, and filter to obtain ether extract; diethyl ether extract is concentrated by rotary evaporation to obtain diethyl ether extract. Diethyl ether extract is dissolved in ether to obtain ether extract, the mass volume ratio of said ether extract to ether is 1g:10ml; add 10 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 and stir for extraction 7 times, stirring for 1 h each time. After standing still, separate the layers to obtain the chloroform layer A. Ad...

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Abstract

The invention discloses an extraction purification method and a detection method for pyrrolo[1,2-a]pyrazine-1,4-dione,hexahydro-3-(phenylmethyl) in euphausia superb. The extraction purification method comprises: adding methanol to euphausia superba, carrying out reflux extraction, and filtering to obtain a filtrate; carrying out evaporation concentration on the filtrate to obtain a methanol extract; adding diethyl ether to the methanol extract, leaching, and filtering to obtain a diethyl ether liquid; evaporating the diethyl ether liquid to obtain a diethyl ether extract; adding a proper amount of diethyl ether to the diethyl ether extract, dissolving to obtain a diethyl ether extract liquid, adding a sulfuric acid aqueous solution, and carrying out stirring extraction to obtain an acid water layer; adding chloroform to the acid water layer, extracting, and carrying out standing liquid separation to obtain a chloroform layer A; adding a sodium hydroxide aqueous solution to the obtained chloroform layer A, extracting, and carrying out standing liquid separation to obtain an alkali water layer and a chloroform layer B; and evaporating the obtained chloroform layer B to remove the solvent so as to obtain Cyclo(Pro-Phe), wherein the obtained Cyclo(Pro-Phe) is analyzed and detected by using gas chromatography-mass spectrometry (GC-MS). According to the present invention, the euphausia superba is adopted as the raw material, the Cyclo(Pro-Phe) is firstly extracted and purified from the euphausia superba, and the detection is performed, such that the important significance is provided for the development of the 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-(phenylmethyl) in Antarctic krill, belonging to food and medicine 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 in active s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 王翩翩刘代成
Owner SHANDONG NORMAL UNIV
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