CN101863812A - Method for extracting astaxanthin from adonis vernalis flowers - Google Patents

Method for extracting astaxanthin from adonis vernalis flowers Download PDF

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Publication number
CN101863812A
CN101863812A CN201010191682A CN201010191682A CN101863812A CN 101863812 A CN101863812 A CN 101863812A CN 201010191682 A CN201010191682 A CN 201010191682A CN 201010191682 A CN201010191682 A CN 201010191682A CN 101863812 A CN101863812 A CN 101863812A
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China
Prior art keywords
solvent
astaxanthin
ointment
obtains
propane
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Pending
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CN201010191682A
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Chinese (zh)
Inventor
陶正国
谭爱民
赵典惠
吴秀丽
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LIDAER BIOTECH CO Ltd GUANGZHOU
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LIDAER BIOTECH CO Ltd GUANGZHOU
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Priority to CN201010191682A priority Critical patent/CN101863812A/en
Publication of CN101863812A publication Critical patent/CN101863812A/en
Pending legal-status Critical Current

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Abstract

The invention relates to a method for extracting astaxanthin from adonis vernalis flowers. The method includes the following steps that: (1) the mixed solvent of propane and butane is used for leaching adonis vernalis flower particles; (2) filtration is carried out, and the obtained extract enters a distillation retort, and is distilled, so that ointment containing the astaxanthin and gaseous solvent are obtained; column chromatography is adopted to further purify the ointment, the immobile phase for chromatography is silica gel, the mobile phase is acetone, and thereby the high-purity astaxanthin, the content of which is more than 90 percent, is obtained.

Description

A kind of method of extracting astaxanthin from oxeye
Technical field
The present invention relates to the extractive technique of astaxanthin, specifically is a kind of method of extracting astaxanthin from oxeye.
Technical background
Astaxanthin is a kind of in the carotenoid; be a kind of powerful antioxidant and biological tinting material; in food nutrition, makeup, feed additive industry widespread use, higher utility value is arranged at prevention of arterial sclerosis and cardiovascular and cerebrovascular diseases, protection eye and central nervous system, anti-inflammatory, aspect such as antitumor.Thereby have a extensive future.
Because the nature astaxanthin seldom, main source is processing of aquatic products waste, red Fife's yeast and Haematocoocus Pluvialls, its source and limited.
Summary of the invention
The objective of the invention is at astaxanthin source defect of insufficient, provide a kind of oxeye that derives from natural high and stable yields to extract the method for astaxanthin.
Described oxeye has another name called the spring adonis amurensis, and Ranunculaceae (Ranunculaceae) Adonis (Adonis) is a kind of perennial flowering plant, contains astaxanthin in the oxeye, and content astaxanthin is about 2% in its dried flower.
Method from oxeye extraction astaxanthin of the present invention may further comprise the steps:
(1) with propane and butane mixed solvent leaching Herba Adonidis dried flower particle, solvent and Herba Adonidis dried flower particulate envelope-bulk to weight ratio are 1.5~2.0 liters: 1 kilogram, propane is 0~2: 8~10 with the volume parts ratio of butane, and total umber is 10;
(2) filter, the extraction liquid that obtains advances retort, 30~50 ℃ ,-0.8MPa~-distill under the 1MPa condition, obtain containing the ointment and the gaseous solvent of astaxanthin.
This ointment that contains astaxanthin can be directly used in food, makeup and dietary supplements.Gaseous solvent is cooled to normal temperature through the cooling tank of band refrigerant coil pipe.
As preferred version, the leaching number of times is 3~5 times in the step (1), adopts fresh solvent at every turn.
Compressed again machine is forced into 0.3MPa~0.8MPa after the gaseous solvent cooling that step (2) obtains, and this moment, gaseous solvent changed liquid solvent into, recycling.
(3) adopt column chromatography to be further purified the ointment that step (2) obtains, the stationary phase of chromatography is a silica gel, and moving phase is acetone.Fractional Collections adopts spectrophotometer 478nm place to survey light absorption value then.Separating back astaxanthin purity reaches more than 90%.
The present invention compared with prior art has following advantage:
(1) distillation condition of the present invention's employing does not need to consume steam, thereby has reduced the use of coal, greatly reduces the discharging of the three wastes.
(2) developed the new source of natural astaxanthin;
(3) the present invention adopts the propane and the butane solvent of specified proportion, and the extraction yield height of astaxanthin reaches more than 95%;
(4) the solvent recovering rate height reaches more than 90%
Embodiment
Embodiment 1 adopts spectrophotometry to survey the content of astaxanthin in the oxeye, and method is as follows:
Mix and extract spring adonis amurensis dried particles 5g, pulverized 60 mesh sieves.Accurately take by weighing spring adonis amurensis powder G0.5g, use the extracting solution chloroform of total amount 100ml and 1: 1 mixed solvent of ethanol to extract three times, merge No. three times extracting solution, constant volume 100ml acutely rocks, and 3~5min is left standstill in the dark place;
In the volumetric flask of 100ml, add above-mentioned solution 10ml, add extracting solution 100ml again, shake and mix 1min;
Do blank with chloroform and alcohol mixed solvent, the 478nm place is colorimetric as early as possible, measures light absorption value A 478
Calculating formula: the content of astaxanthin (g/kg)=K * A 478/ (160 * G)
K is an extension rate, K=100 * 10;
Note: (1) agents useful for same is all analytical pure;
(2) all operations as far as possible in the dark carries out.
Record that ointment content is 12% in the oxeye dried flower particle, content astaxanthin is 14% in the ointment
Embodiment 2
(1) leach Herba Adonidis dried flower particle 4 times with propane and butane mixed solvent, solvent and Herba Adonidis dried flower particulate envelope-bulk to weight ratio are 1.5 liters: 1 kilogram, propane is 2: 8 with the volume parts ratio of butane;
(2) filter, the extraction liquid that obtains advances retort, 30 ℃ ,-distill under the 1MPa condition, obtain containing the ointment and the gaseous solvent of astaxanthin.Compressed again machine is forced into 0.3MPa after the gaseous solvent cooling, and this moment, gaseous solvent changed liquid solvent into, recycling, and solvent recovering rate is 94%.
The ointment that obtains accounts for oxeye dried flower particulate 11% quality, and astaxanthin accounts for 13% quality of ointment.
Ointment directly adds in food, beverage, the makeup; antioxidants such as natural dimension E, β-Hu Luobusu and Q10 can be replaced as superpower antioxidant and tinting material comprehensively, strengthening immunity, anti-ultraviolet radiation, protection eye and central nervous system, prevention of arterial sclerosis and cardiovascular disorder, inhibition diabetics's renal impairment and anti-inflammatory, effect such as anti-infective can be played.
Embodiment 3
(1) leach Herba Adonidis dried flower particle 5 times with propane and butane mixed solvent, solvent and Herba Adonidis dried flower particulate envelope-bulk to weight ratio are 2.0 liters: 1 kilogram, propane is 0: 10 with the volume parts ratio of butane;
(2) filter, the extraction liquid that obtains advances retort, 50 ℃ ,-distill under the 0.8MPa condition, obtain containing the ointment and the gaseous solvent of astaxanthin.Compressed again machine is forced into 0.8MPa after the gaseous solvent cooling that obtains, and this moment, gaseous solvent changed liquid solvent into, recycling, and solvent recovering rate is 90%.
(3) adopt column chromatography to be further purified the ointment that step (2) obtains, the stationary phase of chromatography is a silica gel, and moving phase is acetone; Fractional Collections adopts spectrophotometer 478nm place to survey light absorption value then.Separate back astaxanthin purity and reach 95%.
The high purity astaxanthin that obtains through column chromatography for separation can be used as medical material, is used for the medicine of production for treating tumour and arteriosclerosis, cardiovascular disorder.Also can be used as superpower antioxidant and be used for protective foods, play effects such as improving immunizing power.
Embodiment 4
(1) with propane and butane mixed solvent leaching Herba Adonidis dried flower particle, solvent and Herba Adonidis dried flower particulate envelope-bulk to weight ratio are 1.5~2.0 liters: 1 kilogram, propane is 1: 9 with the volume parts ratio of butane, and total umber is 10; The leaching number of times is 5 times, adopts fresh solvent at every turn
(2) filter, the extraction liquid that obtains advances retort, 30-50 ℃ ,-0.8MPa~-distill under the 1MPa condition, obtain containing the ointment and the gaseous solvent of astaxanthin.Compressed again machine is forced into 0.3MPa after the gaseous solvent cooling that obtains, and this moment, gaseous solvent changed liquid solvent into, recycling, and solvent recovering rate is 92.5%.
This ointment that contains astaxanthin can be directly used in food, makeup and dietary supplements.Gaseous solvent is cooled to normal temperature through the cooling tank of band refrigerant coil pipe.
(3) adopt column chromatography to be further purified the ointment that step (2) obtains, the stationary phase of chromatography is a silica gel, and moving phase is acetone; Fractional Collections adopts spectrophotometer 478nm place to survey light absorption value then.Separate back astaxanthin purity and reach 97%.
The high purity astaxanthin that obtains through column chromatography for separation can be used as medical material, is used for the medicine of production for treating tumour and arteriosclerosis, cardiovascular disorder.Also can be used as superpower antioxidant and be used for protective foods, play effects such as improving immunizing power.

Claims (4)

1. one kind is extracted the method for astaxanthin from oxeye, it is characterized in that may further comprise the steps:
(1) with propane and butane mixed solvent leaching Herba Adonidis dried flower particle, solvent and Herba Adonidis dried flower particulate envelope-bulk to weight ratio are 1.5~2.0 liters: 1 kilogram, propane is 0-2: 8-10 with the volume parts ratio of butane, and total umber is 10;
(2) filter, the extraction liquid that obtains advances retort, 30-50 ℃ ,-0.8MPa~-distill under the 1MPa condition, obtain containing the ointment and the gaseous solvent of astaxanthin.
2. method according to claim 1 is characterized in that the leaching number of times is 3-5 time in the step (1), adopts fresh solvent at every turn.
3. method according to claim 1 and 2, it is characterized in that gaseous solvent cooling that step (2) obtains after compressed again machine be forced into 0.3MPa~0.8MPa, this moment, gaseous solvent changed liquid solvent into, recycling.
4. method according to claim 3 is characterized in that adopting column chromatography to be further purified the ointment that step (2) obtains, and the stationary phase of chromatography is a silica gel, and moving phase is acetone.
CN201010191682A 2010-05-28 2010-05-28 Method for extracting astaxanthin from adonis vernalis flowers Pending CN101863812A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104447464A (en) * 2013-09-24 2015-03-25 浙江医药股份有限公司新昌制药厂 Carotenoid compound derived from plant source and containing natural astaxanthin as well as preparation method and composition of carotenoid compound
CN104502289A (en) * 2014-12-18 2015-04-08 贵州航天乌江机电设备有限责任公司 Measurement method for detecting astaxanthin content

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104447464A (en) * 2013-09-24 2015-03-25 浙江医药股份有限公司新昌制药厂 Carotenoid compound derived from plant source and containing natural astaxanthin as well as preparation method and composition of carotenoid compound
WO2015043112A1 (en) 2013-09-24 2015-04-02 浙江医药股份有限公司新昌制药厂 Carotenoid compound coming from plant and containing natural astaxanthin, preparation method therefor, and composition
CN104447464B (en) * 2013-09-24 2016-11-23 浙江医药股份有限公司新昌制药厂 A kind of plant origin carotenoid compounds containing natural astaxanthin and preparation method thereof and compositions
CN104502289A (en) * 2014-12-18 2015-04-08 贵州航天乌江机电设备有限责任公司 Measurement method for detecting astaxanthin content

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Application publication date: 20101020