Unlock instant, AI-driven research and patent intelligence for your innovation.

Method of preparing high-purity Chlorin e6 from spirulina platensis

A technology of Spirulina platensis and chlorophyllin, applied in organic chemistry and other fields, can solve the problems of low yield and purity of chlorophyllin Chlorine6

Active Publication Date: 2015-12-23
CHINA UNIV OF PETROLEUM (EAST CHINA)
View PDF1 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims at the problem of low yield and purity of commercialized Chlorine6, and proposes a method for preparing Chlorine6 with high efficiency and high purity

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method of preparing high-purity Chlorin e6 from spirulina platensis
  • Method of preparing high-purity Chlorin e6 from spirulina platensis
  • Method of preparing high-purity Chlorin e6 from spirulina platensis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The concrete steps of the preparation method of high-purity chlorophyll acid Chlorine6 of the present invention are as follows:

[0028] Take 1 L of Spirulina platensis algae liquid grown to the late logarithmic growth phase, centrifuge and separate the algae, discard the supernatant, enrich the precipitate in a centrifuge tube, and then extract it with 50 mL of ethanol three times, and combine the extracts.

[0029] Add 20mL of petroleum ether (boiling range 60-90°C) to the extract and mix well, then add 1 / 3 volume of water to the extract, swirl and perform back extraction, repeat the extraction twice with petroleum ether, and use petroleum ether with pigment Wash twice with 20mL water-ethanol solution (volume ratio 1:1).

[0030] Add 10 mL of 1 mol / L NaOH in 95% ethanol to the petroleum ether extract, and stir for 0.5 h.

[0031] Add 10 mL of water to the above mixed solution, vortex and stand to separate. The upper petroleum ether phase contains carotenoids and turn...

Embodiment 2

[0035] The concrete steps of the preparation method of high-purity chlorophyll acid Chlorine6 of the present invention are as follows:

[0036] Take 1 L of Spirulina platensis algal liquid grown to the late logarithmic growth phase, centrifuge and separate the algae, discard the supernatant, enrich the precipitate in a centrifuge tube, and then extract three times with 40 mL of ethanol, and combine the extracts.

[0037] Add 15mL of petroleum ether (boiling range 60-90°C) to the extract and mix well, then add 1 / 3 volume of water to the extract, swirl and perform back extraction, repeat the extraction twice with petroleum ether, and use petroleum ether with pigment 0.5mol / L NaOH water-ethanol solution (volume ratio 1:1) 15mL quick wash twice.

[0038] Add 10 mL of 1 mol / L NaOH in 95% ethanol to the petroleum ether extract, and stir for 2 h.

[0039] Add 10 mL of water to the above mixed solution, vortex and stand to separate. The upper petroleum ether phase contains carotenoid...

Embodiment 3

[0043] The concrete steps of the preparation method of high-purity chlorophyll acid Chlorine6 of the present invention are as follows:

[0044] Take 1 L of Spirulina platensis algae liquid grown to the late logarithmic growth phase, centrifuge and separate the algae, discard the supernatant, enrich the precipitate in a centrifuge tube, and then extract it with 50 mL of ethanol three times, and combine the extracts.

[0045] Add 20mL of petroleum ether (boiling range 60-90°C) to the extract and mix well, then add 1 / 3 volume of water to the extract, swirl and perform back extraction, repeat the extraction twice with petroleum ether, and use petroleum ether with pigment Wash twice with 20mL water-ethanol solution (volume ratio 1:1).

[0046] Add 10 mL of 1 mol / L NaOH in 95% ethanol to the petroleum ether extract, and stir for 3 h.

[0047] Add 10 mL of water to the above mixed solution, vortex and stand to separate. The upper petroleum ether phase contains carotenoids and turns ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a method of preparing high-purity Chlorin e6 from fresh spirulina platensis. The method comprises the steps that firstly, pigments are extracted from the spirulina platensis with ethanol as the solvent, a proper amount of petroleum ether is added into the extract liquor and evenly mixed with the extract liquor, water is added for phase splitting, reextraction is conducted after the extract liquor is shaken, and then extraction is repeated several times with petroleum ether; secondly, petroleum ether phases are washed several times with water-ethanol solution; thirdly, 95% ethanol solution of NaOH is added into extract liquor of petroleum ether and stirred for reaction; fourthly, water is added into the mixed liquor, the mixed liquor stands for separation after being shaken, and the water-ethanol solution at the lower layer is washed several times with petroleum ether; fifthly, hydrochloric acid is dripped into the mixed liquor to neutralize the mixed liquor into subacidity, the mixed liquor is subjected to centrifugal separation and sedimentation or extraction with dichloromethane, the sediment is frozen and dried after being dispersed and suspended with a small amount of deionized water, or the dichloromethane solution is rotated for evaporation to recover the solvent, and then high-purity Chlorin e6 solids can be acquired. The Chlorin e6 prepared through the method does not contain other chlorophyllin, and the HPLC purity is higher than 99.5%.

Description

technical field [0001] The invention relates to the technical field of natural photosensitizers for photodynamic therapy, in particular to a method for preparing the second-generation photosensitizer Chlorine6 with high efficiency and high purity. Background technique [0002] Chlorine 6 and its derivatives belong to the second generation photosensitizer of photodynamic therapy. Chlorine6 is a natural molecule derived from chlorophyll. It has a long lifetime of photoexcited triplet states, and has a high molar absorptivity in the red region of visible light. Compared with other porphyrin photosensitizers, it is cheap. Its research and application are in the clinical trial stage. [0003] Chlorine6 is generally obtained by alkaline hydrolysis of chlorophyll a. The preparation method of commercial Chlorine6 involves the separation and purification of chlorophyll by column chromatography. The yield of chlorophyll a is relatively low, and the purity of Chlorine6 obtained is gene...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/22
CPCC07D487/22
Inventor 于道永李泉李富强吴晨露张宏玉葛保胜黄方
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)