CN107805215A - A kind of extracting method of astaxanthin - Google Patents
A kind of extracting method of astaxanthin Download PDFInfo
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- CN107805215A CN107805215A CN201710972211.5A CN201710972211A CN107805215A CN 107805215 A CN107805215 A CN 107805215A CN 201710972211 A CN201710972211 A CN 201710972211A CN 107805215 A CN107805215 A CN 107805215A
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- astaxanthin
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- broken wall
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- JEBFVOLFMLUKLF-IFPLVEIFSA-N Astaxanthin Natural products CC(=C/C=C/C(=C/C=C/C1=C(C)C(=O)C(O)CC1(C)C)/C)C=CC=C(/C)C=CC=C(/C)C=CC2=C(C)C(=O)C(O)CC2(C)C JEBFVOLFMLUKLF-IFPLVEIFSA-N 0.000 title claims abstract description 46
- 235000013793 astaxanthin Nutrition 0.000 title claims abstract description 46
- MQZIGYBFDRPAKN-ZWAPEEGVSA-N astaxanthin Chemical compound C([C@H](O)C(=O)C=1C)C(C)(C)C=1/C=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(C)C=CC=C(C)C=CC1=C(C)C(=O)[C@@H](O)CC1(C)C MQZIGYBFDRPAKN-ZWAPEEGVSA-N 0.000 title claims abstract description 46
- 229940022405 astaxanthin Drugs 0.000 title claims abstract description 46
- 239000001168 astaxanthin Substances 0.000 title claims abstract description 46
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000011347 resin Substances 0.000 claims abstract description 31
- 229920005989 resin Polymers 0.000 claims abstract description 31
- 241000168517 Haematococcus lacustris Species 0.000 claims abstract description 16
- 108010059892 Cellulase Proteins 0.000 claims abstract description 10
- 229940106157 cellulase Drugs 0.000 claims abstract description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 33
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical class [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 23
- 239000000463 material Substances 0.000 claims description 18
- 238000001556 precipitation Methods 0.000 claims description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000000926 separation method Methods 0.000 claims description 11
- 241000195493 Cryptophyta Species 0.000 claims description 10
- NIQQIJXGUZVEBB-UHFFFAOYSA-N methanol;propan-2-one Chemical compound OC.CC(C)=O NIQQIJXGUZVEBB-UHFFFAOYSA-N 0.000 claims description 10
- 238000004108 freeze drying Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 9
- 239000006228 supernatant Substances 0.000 claims description 9
- 238000006911 enzymatic reaction Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims 1
- 239000008157 edible vegetable oil Substances 0.000 claims 1
- 238000002481 ethanol extraction Methods 0.000 claims 1
- 108090000790 Enzymes Proteins 0.000 abstract description 5
- 102000004190 Enzymes Human genes 0.000 abstract description 5
- 229940088598 enzyme Drugs 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000006378 damage Effects 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000004480 active ingredient Substances 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 8
- 238000005119 centrifugation Methods 0.000 description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 230000008859 change Effects 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 241000238557 Decapoda Species 0.000 description 2
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 2
- RASZIXQTZOARSV-BDPUVYQTSA-N astacin Chemical compound CC=1C(=O)C(=O)CC(C)(C)C=1/C=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(C)C=CC=C(C)C=CC1=C(C)C(=O)C(=O)CC1(C)C RASZIXQTZOARSV-BDPUVYQTSA-N 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 102000034498 Astacin Human genes 0.000 description 1
- 108090000658 Astacin Proteins 0.000 description 1
- FMKGDHLSXFDSOU-BDPUVYQTSA-N Dienon-Astacin Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)C(=O)C(=CC1(C)C)O)C=CC=C(/C)C=CC2=C(C)C(=O)C(=CC2(C)C)O FMKGDHLSXFDSOU-BDPUVYQTSA-N 0.000 description 1
- 241000168525 Haematococcus Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 235000003676 astacin Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical group 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- -1 light Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C403/00—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone
- C07C403/24—Derivatives of cyclohexane or of a cyclohexene or of cyclohexadiene, having a side-chain containing an acyclic unsaturated part of at least four carbon atoms, this part being directly attached to the cyclohexane or cyclohexene or cyclohexadiene rings, e.g. vitamin A, beta-carotene, beta-ionone having side-chains substituted by six-membered non-aromatic rings, e.g. beta-carotene
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The present invention provides a kind of extracting method of astaxanthin, this method mainly includes cryogrinding, enzyme process low temperature broken wall, the technological means such as the multistage extraction of organic solvent and combined macroporous resin purification, primary broken wall is carried out to haematococcus pluvialis first with the method for cryogrinding, secondary broken wall is carried out then in conjunction with cellulase and pectase, and temperature during secondary broken wall is 0~4 DEG C, breach conventional broken wall temperature selection thinking, avoid destruction of the high temperature to haematococcus pluvialis active ingredient, so as to realize the abundant broken wall of cell, good basis is provided for follow-up Astaxanthin extraction.By way of multistage is extracted, mild condition, destruction will not be produced to astaxanthin, simultaneously combined macroreticular resin is employed to be purified, substantially increase the recovery rate and purity of astaxanthin, so as to improve the value of haematococcus pluvialis, increase economic benefit, solid foundation is established for industrialized production.
Description
Technical field
The present invention relates to the extractive technique field of natural products, and in particular to a kind of extracting method of astaxanthin.
Background technology
Astaxanthin, also known as astaxanthin or astacin, it is a Carotenoids, is a kind of stronger antioxidant,
Exist in shrimp, crab, algae, yeast, the natural astaxanthin content being currently known it is higher be haematococcus pluvialis and farad yeast, rain
The astaxanthin for the mainly esterification that raw haematococcus contains, the astaxanthin of esterification are stored in internal more stable not oxidized
The astaxanthin crossed, therefore be acknowledged as producing the best biology of astaxanthin in nature.
Astaxanthin is long-chain unsaturated double-bond structural system, and therefore, property is unstable, easy isomerization and degraded, to heat,
Oxygen, light, acid, alkali etc. are more sensitive.The recovery rate of astaxanthin, purity are relatively low at present, and production cost is high, it is therefore desirable to more complete
The exploitation extracting method in face, the recovery rate and purity of astaxanthin are improved, increases its economic benefit.
The content of the invention
For in place of above the deficiencies in the prior art, the present invention provides a kind of extracting method of astaxanthin.
The technical scheme that the present invention takes is as follows：
A kind of extracting method of astaxanthin, comprises the following steps：
S1：Take haematococcus pluvialis algae 3~5g of powder, carry out cryogrinding, add 0.3~0.6mg/mL cellulase and
Totally 200~300mL carries out broken wall, 0~4 DEG C of broken wall temperature, 45~60min of broken time, enzyme to 0.1~0.3mg/mL pectase
PH 3.5~5.0 is reacted, adds 0.5~2g/mL sodium chloride solution, mixes 5~10min, separation supernatant precipitation；
S2：The precipitation in step S1 is taken, by solid-liquid ratio 1：2~3, the methanol solution containing 2~3% sodium hydroxides is added, instead
1~2h is answered, edible oil-acetone and ethyl acetate is added and is extracted, separate, obtain extract solution a and filter residue X；Filter residue X is taken to distinguish
With different volumes than acetone-methanol solution extracted successively, separate, filter residue Y and extract solution b are obtained after merging；Take filter residue Y
Extracted with ethanol, separate, obtain extract solution c；
S3：Extract solution a, extract solution b and extract solution c are mixed, freeze-drying, selection is mixed with three kinds of macroreticular resin materials
The combined macroreticular resin formed is purified, and obtains astaxanthin of the present invention.
Preferably, the addition of sodium chloride is 20~50ml in the step S1, and parameter of noncentricity is：2000~3000rpm
Centrifuge 5~10min.
Preferably, in the step S2 volume ratio of edible oil-acetone and ethyl acetate for 50~52: 25~29: 19~
25, the volume ratio of acetone-methanol is respectively 99: 1,75~88: 12~25,50~60: 40~50,0: 100.
Preferably, three kinds of macroreticular resin materials are respectively XDA-1, XDA-6 and XAD-16 in the step S3.
Compared with prior art, the beneficial effects of the invention are as follows：
1st, the present invention carries out primary broken wall first with the method for cryogrinding to haematococcus pluvialis, then in conjunction with cellulose
Enzyme and pectase carry out secondary broken wall, and so as to realize the abundant broken wall of cell, and temperature during secondary broken wall is 0~4 DEG C, is dashed forward
The broken wall temperature selection thinking of routine has been broken, destruction of the high temperature to haematococcus pluvialis active ingredient has been avoided, is follow-up shrimp
Blue or green element extraction provides good basis.
2nd, the present invention is by way of multistage is extracted, mild condition, will not produce destruction to astaxanthin, while employ group
Mould assembly macroreticular resin is purified, and substantially increases the recovery rate and purity of astaxanthin, so as to improve the profit of haematococcus pluvialis
With value, increase economic benefit, solid foundation is established for industrialized production.
Embodiment
The invention will now be further described with reference to specific embodiments, advantages of the present invention and feature will be with description and
It is apparent, but protection scope of the present invention is not limited to following examples.
Embodiment 1：
A kind of extracting method of astaxanthin, comprises the following steps：
S1：Take haematococcus pluvialis algae powder 3g, carry out cryogrinding, add 0.4mg/mL cellulase and 0.1mg/mL
The common 300mL of pectase carries out broken wall, 0 DEG C of broken wall temperature, broken time 60min, enzyme reaction pH 4, adds 0.7g/mL chlorination
Sodium solution 50ml, mix 10min, 2000rpm centrifugation 5min, separation supernatant precipitation；
S2：The precipitation in step S1 is taken, by solid-liquid ratio 1: 2, the methanol solution containing 3% sodium hydroxide is added, reacts 1h, add
Enter edible oil-acetone and ethyl acetate (volume ratio 52: 29: 19) to be extracted, separate, obtain extract solution a and filter residue X；Take filter
Slag X is extracted successively with the acetone-methanol solution that volume ratio is 99: 1,88: 12,60: 40,0: 100 respectively, is separated, and is merged
After obtain filter residue Y and extract solution b；Take filter residue Y to be extracted with ethanol, separate, obtain extract solution c；
S3：Extract solution a, extract solution b and extract solution c are mixed, freeze-drying, selection is mixed with three kinds of macroreticular resin materials
The combined macroreticular resin formed is purified, and three kinds of macroreticular resin materials are XDA-1, XDA-6 and XAD-16, obtains this
Invention astaxanthin.
Embodiment 2：
A kind of extracting method of astaxanthin, comprises the following steps：
S1：Take haematococcus pluvialis algae powder 5g, carry out cryogrinding, add 0.3mg/mL cellulase and 0.1mg/mL
The common 200mL of pectase carries out broken wall, 4 DEG C of broken wall temperature, broken time 45min, enzyme reaction pH 3.5, adds 2g/mL chlorination
Sodium solution 50ml, mix 10min, 2000rpm centrifugation 10min, separation supernatant precipitation；
S2：The precipitation in step S1 is taken, by solid-liquid ratio 1: 3, the methanol solution containing 2% sodium hydroxide is added, reacts 2h, add
Enter edible oil-acetone and ethyl acetate (volume ratio 50: 25: 25) to be extracted, separate, obtain extract solution a and filter residue X；Take filter
Slag X is extracted successively with the acetone-methanol solution that volume ratio is 99: 1,75: 25,60: 40,0: 100 respectively, is separated, and is merged
After obtain filter residue Y and extract solution b；Take filter residue Y to be extracted with ethanol, separate, obtain extract solution c；
S3：Extract solution a, extract solution b and extract solution c are mixed, freeze-drying, selection is mixed with three kinds of macroreticular resin materials
The combined macroreticular resin formed is purified, and three kinds of macroreticular resin materials are XDA-1, XDA-6 and XAD-16, obtains this
Invention astaxanthin.
Embodiment 3：
A kind of extracting method of astaxanthin, comprises the following steps：
S1：Take haematococcus pluvialis algae powder 3g, carry out cryogrinding, add 0.6mg/mL cellulase and 0.3mg/mL
The common 300mL of pectase carries out broken wall, 0 DEG C of broken wall temperature, broken time 45min, enzyme reaction pH 5.0, adds 0.5g/mL chlorine
Change sodium solution 20ml, mix 5min, 3000rpm centrifugation 5min, separation supernatant precipitation；
S2：The precipitation in step S1 is taken, by solid-liquid ratio 1: 3, the methanol solution containing 3% sodium hydroxide is added, reacts 1h, add
Enter edible oil-acetone and ethyl acetate (volume ratio 52: 29: 19) to be extracted, separate, obtain extract solution a and filter residue X；Take filter
Slag X is extracted successively with the acetone-methanol solution that volume ratio is 99: 1,88: 12,50: 50,0: 100 respectively, is separated, and is merged
After obtain filter residue Y and extract solution b；Take filter residue Y to be extracted with ethanol, separate, obtain extract solution c；
S3：Extract solution a, extract solution b and extract solution c are mixed, freeze-drying, selection is mixed with three kinds of macroreticular resin materials
The combined macroreticular resin formed is purified, and three kinds of macroreticular resin materials are XDA-1, XDA-6 and XAD-16, obtains this
Invention astaxanthin.
Embodiment 4：
A kind of extracting method of astaxanthin, comprises the following steps：
S1：Take haematococcus pluvialis algae powder 4g, carry out cryogrinding, add 0.5mg/mL cellulase and 0.2mg/mL
The common 250mL of pectase carries out broken wall, 2 DEG C of broken wall temperature, broken time 50min, enzyme reaction pH 4.5, adds 1.5g/mL chlorine
Change sodium solution 25ml, mix 5min, 2000rpm centrifugation 5min, separation supernatant precipitation；
S2：The precipitation in step S1 is taken, by solid-liquid ratio 1: 3, the methanol solution containing 3% sodium hydroxide is added, reacts 1h, add
Enter edible oil-acetone and ethyl acetate (volume ratio 52: 29: 19) to be extracted, separate, obtain extract solution a and filter residue X；Take filter
Slag X is extracted successively with the acetone-methanol solution that volume ratio is 99: 1,80: 20,55: 45,0: 100 respectively, is separated, and is merged
After obtain filter residue Y and extract solution b；Take filter residue Y to be extracted with ethanol, separate, obtain extract solution c；
S3：Extract solution a, extract solution b and extract solution c are mixed, freeze-drying, selection is mixed with three kinds of macroreticular resin materials
The combined macroreticular resin formed is purified, and three kinds of macroreticular resin materials are XDA-1, XDA-6 and XAD-16, obtains this
Invention astaxanthin.
Comparative example 1：
A kind of extracting method of astaxanthin, comprises the following steps：
S1：Take haematococcus pluvialis algae powder 3g, carry out cryogrinding, add 0.1mg/mL cellulase and 0.1mg/mL
The common 100mL of pectase carries out broken wall, 0 DEG C of broken wall temperature, broken time 60min, enzyme reaction pH 3.5, adds 2g/mL chlorination
Sodium solution 20ml, mix 10min, 3000rpm centrifugation 5min, separation supernatant precipitation；
S2：The precipitation in step S1 is taken, by solid-liquid ratio 1: 2, the methanol solution containing 1% sodium hydroxide is added, reacts 1h, add
Enter edible oil-acetone and ethyl acetate (volume ratio 30: 40: 30) to be extracted, separate, obtain extract solution a and filter residue X；Take filter
Slag X is extracted successively with the acetone-methanol solution that volume ratio is 99: 1,60: 40,30: 70,0: 100 respectively, is separated, and is merged
After obtain filter residue Y and extract solution b；Take filter residue Y to be extracted with ethanol, separate, obtain extract solution c；
S3：Extract solution a, extract solution b and extract solution c are mixed, freeze-drying, selection is mixed with three kinds of macroreticular resin materials
The combined macroreticular resin formed is purified, and three kinds of macroreticular resin materials are XDA-1, XDA-6 and XAD-16, obtains this
Invention astaxanthin.
Comparative example 2：
A kind of extracting method of astaxanthin, it is characterised in that comprise the following steps：
S1：Haematococcus pluvialis algae powder 3g is taken, cryogrinding is carried out, adds 1mg/mL cellulase and 0.5mg/mL fruit
The common 200mL of glue enzyme carries out broken wall, 0 DEG C of broken wall temperature, broken time 60min, enzyme reaction pH 3.5, adds 2g/mL sodium chloride
Solution 20ml, mix 10min, 3000rpm centrifugation 5min, separation supernatant precipitation；
S2：The precipitation in step S1 is taken, by solid-liquid ratio 1: 2, the methanol solution containing 5% sodium hydroxide is added, reacts 1h, add
Enter edible oil-acetone and ethyl acetate (volume ratio 60: 35: 5) to be extracted, separate, obtain extract solution a and filter residue X；Take filter
Slag X is extracted successively with the acetone-methanol solution that volume ratio is 99: 1,95: 5,70: 30,10: 90 respectively, is separated, after merging
Obtain filter residue Y and extract solution b；Take filter residue Y to be extracted with ethanol, separate, obtain extract solution c；
S3：Extract solution a, extract solution b and extract solution c are mixed, freeze-drying, selection is mixed with three kinds of macroreticular resin materials
The combined macroreticular resin formed is purified, and three kinds of macroreticular resin materials are XDA-1, XDA-6 and XAD-16, obtains this
Invention astaxanthin.
Comparative example 3：
A kind of extracting method of astaxanthin, comprises the following steps：
S1：It is same as Example 1；
S2：It is identical in embodiment 1；
S3：Extract solution a, extract solution b and extract solution c are mixed, freeze-drying, selection is carried out pure with AB-8 types macroreticular resin
Change, obtain astaxanthin of the present invention.
Comparative example 4：
A kind of extracting method of astaxanthin, comprises the following steps：
S1：Haematococcus pluvialis algae powder 3g is taken, the cellulase 200mL for adding 0.4mg/mL carries out broken wall, broken wall temperature 0
DEG C, broken time 60min, enzyme reaction pH 4, add 0.7g/mL sodium chloride solution 50ml, mix 10min, 2000rpm centrifugations
5min, separation supernatant precipitation；
S2：The precipitation in step S1 is taken, by solid-liquid ratio 1: 2, the methanol solution containing 3% sodium hydroxide is added, reacts 1h, add
Enter edible oil-acetone and ethyl acetate (volume ratio 52: 29: 19) to be extracted, separate, obtain extract solution；
S3：Extract solution is freeze-dried, selects the combined macropore tree mixed with three kinds of macroreticular resin materials
Fat is purified, and three kinds of macroreticular resin materials are XDA-1, XDA-6 and XAD-16, obtain astaxanthin of the present invention.
Comparative example 5：
A kind of extracting method of astaxanthin, comprises the following steps：
S1：Same as Example 1, difference is that broken wall temperature is 40 DEG C；
S2：It is same as Example 1；
S3：It is same as Example 1.
Experimental example：
Embodiment and the Astaxanthin extraction rate and purity in comparative example are determined respectively.Measurement result is shown in Table 1.
Table 1：Measurement result
It can be seen from experimental result, the recovery rate of the inventive method astaxanthin is up to 99.1%, high purity 99.8%, carries
Rate and purity is taken to be significantly larger than comparative example.Carried it can be seen that the present invention combines cryogrinding, enzyme process low temperature broken wall, organic solvent multistage
Take with the technological means such as combined macroporous resin purification, achieve the technique effect for being substantially better than comparative example method.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements done etc., should be included within the scope of protection of the invention with principle.
Claims (4)
1. a kind of extracting method of astaxanthin, it is characterised in that comprise the following steps：
S1：Take haematococcus pluvialis algae 3~5g of powder, carry out cryogrinding, add 0.3~0.6mg/mL cellulase and 0.1~
Totally 200~300mL carries out broken wall, 0~4 DEG C of broken wall temperature, 45~60min of broken time, enzyme reaction to 0.3mg/mL pectase
PH 3.5~5.0,0.5~2g/mL sodium chloride solution is added, mix 5~10min, separation supernatant precipitation；
S2：The precipitation in step S1 is taken, by solid-liquid ratio 1: 2~3, adds the methanol solution containing 2~3% sodium hydroxides, reaction 1~
2h, add edible oil-acetone and ethyl acetate and extracted, separate, obtain extract solution a and filter residue X；Take filter residue X respectively with difference
The acetone-methanol solution of volume ratio is extracted successively, separation, filter residue Y and extract solution b is obtained after merging；Filter residue Y is taken with ethanol
Extraction, separation, obtains extract solution c；
S3：Extract solution a, extract solution b and extract solution c are mixed, freeze-drying, selection is mixed with three kinds of macroreticular resin materials
Combined macroreticular resin purified, obtain astaxanthin of the present invention.
A kind of 2. extracting method of astaxanthin according to claim 1, it is characterised in that sodium chloride in the step S1
Addition is 20~50ml, and parameter of noncentricity is：2000~3000rpm centrifuges 5~10min.
A kind of 3. extracting method of astaxanthin according to claim 1, it is characterised in that edible oil in the step S2-
The volume ratio of acetone and ethyl acetate is 50~52: 25~29: 19~25, the volume ratio of acetone-methanol is respectively 99: 1,75~
88: 12~25,50~60: 40~50,0: 100.
A kind of 4. extracting method of astaxanthin according to claim 1, it is characterised in that three kinds of macropores in the step S3
Resin material is respectively XDA-1, XDA-6 and XAD-16.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108866144A (en) * | 2018-07-24 | 2018-11-23 | 杭州园泰生物科技有限公司 | A method of preparing and purifying astaxanthin |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108866144A (en) * | 2018-07-24 | 2018-11-23 | 杭州园泰生物科技有限公司 | A method of preparing and purifying astaxanthin |
| CN108866144B (en) * | 2018-07-24 | 2020-11-17 | 杭州园泰生物科技有限公司 | Method for preparing and purifying astaxanthin |
| CN109480285A (en) * | 2018-12-10 | 2019-03-19 | 丽江程海湖天然螺旋藻生产基地有限公司 | A kind of haematococcus pluvialis soft capsule |
| CN109645295A (en) * | 2019-01-17 | 2019-04-19 | 云南龙布瑞生物科技有限公司 | A kind of Astaxanthin In Haematococcus Pluvialis solid beverage maintaining cardiovascular system health |
| WO2022021612A1 (en) | 2020-07-27 | 2022-02-03 | 中国海洋大学 | Method for preparing water-soluble astaxanthin, and astaxanthin aqueous solution prepared using said method |
| CN113249291A (en) * | 2021-07-01 | 2021-08-13 | 海南三元星生物科技股份有限公司 | Method for inducing haematococcus pluvialis cell type conversion and accumulating astaxanthin by using seawater |
| CN116622797A (en) * | 2023-04-03 | 2023-08-22 | 广州优卡思农业技术有限公司 | Method for extracting astaxanthin from haematococcus pluvialis |
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