CN101298562A - Extraction method for antioxidant BHT in calla - Google Patents

Extraction method for antioxidant BHT in calla Download PDF

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Publication number
CN101298562A
CN101298562A CNA200710034897XA CN200710034897A CN101298562A CN 101298562 A CN101298562 A CN 101298562A CN A200710034897X A CNA200710034897X A CN A200710034897XA CN 200710034897 A CN200710034897 A CN 200710034897A CN 101298562 A CN101298562 A CN 101298562A
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China
Prior art keywords
antioxidant bht
organic solvent
polar organic
solvent
common calla
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Pending
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CNA200710034897XA
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Chinese (zh)
Inventor
杨志学
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HUAIHUA MEDICAL COLLEGE
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HUAIHUA MEDICAL COLLEGE
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Priority to CNA200710034897XA priority Critical patent/CN101298562A/en
Publication of CN101298562A publication Critical patent/CN101298562A/en
Pending legal-status Critical Current

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  • Cosmetics (AREA)
  • Medicinal Preparation (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a method for extracting natural antioxidant BHT from Zantedeschia plants. In order to overcome the defect of the lacking of methods for extracting the natural antioxidant BHT from the Zantedeschia plants and to develop Zantedeschia plant resources, the invention adopts the treatment of enlarging the surface area of Zantedeschia; immersing by using a polar organic solvent; extracting by using ultrasonic or a thermal extraction method; suspending by adding a polar solvent and extracting by using a non-polar organic solvent; separating by using a chromatographic column; eluting by using an intermediate-polar organic solvent; recrystallizing by using absolute ethyl alcohol or petroleum ether, thus obtaining the antioxidant BHT. The method is used for extracting the natural antioxidant BHT from the Zantedeschia plants, is simple, feasible and pollution free, is suitable for industrialized production, and has the advantages of strong antioxidant effect of the extracted antioxidant BHT, no toxic and side effect and having better application effect than vitamin E, thus the method can be widely applied to industries such as medicine and food, etc. with bright market prospect.

Description

The extracting method of antioxidant BHT in the common calla
Technical field
The present invention relates to a kind of chemical extraction technology, be specially a kind of technology of from the natural phant common calla, extracting antioxidant BHT.
Technical background
At present, produce antioxidant BHT both at home and abroad and mainly adopt chemical synthesis, wherein the manufacturer more than 60% adopts cresols and isobutene reaction to produce BHT.The antioxidant BHT of chemosynthesis is big because of toxicity, has limited use both at home and abroad, thereby seeks natural antioxidants BHT and become global research topic.
In recent years, the inventor has found to contain in the common calla abundant natural antioxidants BHT from early-stage Study such as " trial tests of common calla chemical ingredients ", and it is strong to have antioxygenation, remarkable advantage such as have no side effect, but weak point is that the method and the technology of its extraction are not appeared in the newspapers both at home and abroad.
Summary of the invention
Purpose of the present invention will overcome above-mentioned deficiency exactly, and a kind of method that can extract natural antioxidants BHT from the common calla plant is provided.
For achieving the above object, technical scheme of the present invention is that the extracting method of antioxidant BHT comprises the steps: in this common calla
[1] common calla is done the long-pending processing of enlarged surface;
[2] will soak with polar organic solvent through the common calla that step [1] is handled;
[3] extract with ultrasonic wave or hot extraction;
[4] isolate immersion liquid, reclaim solvent, get medicinal extract;
[5] additive polarity solvent suspendible in medicinal extract extracts with non-polar organic solvent;
[6] tell the non-polar organic solvent layer, reclaim solvent, get paste;
[7] paste dissolves with non-polar organic solvent, separates with chromatographic column;
[8] with middle polarity organic solvent wash-out;
[9] reclaim solvent, get antioxidant BHT.
In the described step [1] common calla is done enlarged surface long-pending be treated to pulverization process.
Polar organic solvent in the described step [2] can be ethanol, methyl alcohol etc.
Hot extraction in the described step [3] can be back to heat up in a steamer.
Polar solvent in the described step [5] can be water, methyl alcohol, ethanol etc.; Described non-polar organic solvent can be sherwood oil, chloroform etc.
Non-polar organic solvent in the described step [7] can be sherwood oil, chloroform etc.; Described chromatographic column can be Al 2O 3Post, silicagel column, D101 post, ODS reversed-phase column etc.
Middle polarity organic solvent in the described step [8] can be ethyl acetate, acetone etc.
Recovery solvent in the described step [9], getting antioxidant BHT is crude product, further with dehydrated alcohol or sherwood oil recrystallization, can get the antioxidant BHT elaboration.
This technology can extract the natural anti-oxidation BHT in the common calla plant, this simple and convenient extraction, feasible, pollution-free, suitability for industrialized production.The structural formula of the natural antioxidants BHT that is extracted, identify at Chinese Academy of Sciences's mass spectrometric measurement center.This natural antioxidants BHT that from the common calla plant, extracts, antioxygenation is strong, has no side effect, and can be used for all conglomeraties such as medicine, food, feed, makeup, and its result of use is stronger than vitamin-E, has vast market prospect.
Embodiment
Embodiment 1
Extract natural antioxidants BHT from the common calla plant, method is as follows:
(1) with common calla drying, pulverizing, mistake 20 mesh sieve;
(2) be the ethanol soaking at room temperature 24 hours of 70-95% with volume ratio, common calla and ethanol volume ratio are 1: 10-30 (control pH2-4);
(3) with ultrasonic wave (model: KQ-1000D) extracted 30-40 minute, repeat to carry united extraction liquid 3 times;
(4) decompression and solvent recovery (use rotary evaporator, vacuum tightness reclaims solvent temperature: 40 ℃ greater than 0.08MPa) gets medicinal extract;
(5) medicinal extract is with purified water suspendible (medicinal extract: water=1: 1-5, control pH is to neutral);
(6) (commercially available, A.R) extraction (normal temperature and pressure) is colourless to petroleum ether layer with sherwood oil;
(7) reclaim under reduced pressure (use rotary evaporator, vacuum tightness reclaims solvent temperature: 34-38 ℃ greater than 0.08MPa) sherwood oil gets paste;
(8) (ratio 1: 1-5, sherwood oil are commercially available, A.R) dissolving, Al on the dry method with sherwood oil with paste 2O 3Post (column chromatography usefulness, commercially available, the 100-200 order) chromatography;
(9) with ethyl acetate (commercially available, A.R) wash-out;
(10) collect the eluent ethyl acetate thing;
(11) reclaim under reduced pressure (use rotary evaporator, vacuum tightness reclaims solvent temperature: 40 ℃ greater than 0.08MPa) ethyl acetate gets the antioxidant BHT crude product;
(12) with the antioxidant BHT crude product with ethyl acetate (commercially available, A.R) dissolving, Al on the dry method 2O 3Post (column chromatography usefulness, commercially available, the 100-200 order) chromatography, (commercially available with ethyl acetate, A.R) wash-out is collected the eluent ethyl acetate thing, and (use rotary evaporator, vacuum tightness is greater than 0.08MPa for reclaim under reduced pressure, reclaim solvent temperature: 40 ℃) ethyl acetate, so repeat 2 times, get antioxidant BHT.
(13) with sherwood oil (commercially available, A.R) or dehydrated alcohol (commercially available, A.R) recrystallization is 2-3 time, must the antioxidant BHT elaboration.
Also available supercritical extraction replaces column chromatography, extraction, separating natural antioxidant BHT from the common calla plant.

Claims (7)

1. the extracting method of antioxidant BHT in the common calla is characterized in that it comprises the steps:
[1] common calla is done the long-pending processing of enlarged surface;
[2] will soak with polar organic solvent through the common calla that step [1] is handled;
[3] extract with ultrasonic wave or hot extraction;
[4] isolate immersion liquid, reclaim solvent, get medicinal extract;
[5] additive polarity solvent suspendible in medicinal extract extracts with non-polar organic solvent;
[6] tell the non-polar organic solvent layer, reclaim solvent, get paste;
[7] paste dissolves with non-polar organic solvent, separates with chromatographic column;
[8] with middle polarity organic solvent wash-out;
[9] reclaim solvent, get antioxidant BHT.
2, the extracting method of antioxidant BHT in the common calla according to claim 1 is characterized in that, in the described step [1] common calla is done enlarged surface long-pending be treated to pulverization process.
3, the extracting method of antioxidant BHT in the common calla according to claim 1 is characterized in that, the polar organic solvent in the described step [2] is an ethanol.
4, the extracting method of antioxidant BHT in the common calla according to claim 1 is characterized in that, the polar solvent in the described step [5] is a water; Described non-polar organic solvent is a sherwood oil.
5, the extracting method of antioxidant BHT in the common calla according to claim 1 is characterized in that, the non-polar organic solvent in the described step [7] is a sherwood oil; Described chromatographic column is Al 2O 3Post.
6, the extracting method of antioxidant BHT in the common calla according to claim 1 is characterized in that, the middle polarity organic solvent in the described step [8] is an ethyl acetate.
7, the extracting method of antioxidant BHT in the common calla according to claim 1 is characterized in that, the recovery solvent in the described step [9], and getting antioxidant BHT is crude product, further with dehydrated alcohol or sherwood oil recrystallization, can get the antioxidant BHT elaboration.
CNA200710034897XA 2007-05-01 2007-05-01 Extraction method for antioxidant BHT in calla Pending CN101298562A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNA200710034897XA CN101298562A (en) 2007-05-01 2007-05-01 Extraction method for antioxidant BHT in calla

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNA200710034897XA CN101298562A (en) 2007-05-01 2007-05-01 Extraction method for antioxidant BHT in calla

Publications (1)

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CN101298562A true CN101298562A (en) 2008-11-05

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102660290A (en) * 2012-04-27 2012-09-12 东北林业大学 Acorn shell pigment with antioxidant activity and preparation method and application thereof
CN112300108A (en) * 2020-10-30 2021-02-02 重庆市蚕业科学技术研究院 Method for rapidly extracting vitamin E from green plant leaves

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102660290A (en) * 2012-04-27 2012-09-12 东北林业大学 Acorn shell pigment with antioxidant activity and preparation method and application thereof
CN102660290B (en) * 2012-04-27 2014-03-12 东北林业大学 Acorn shell pigment with antioxidant activity and preparation method and application thereof
CN112300108A (en) * 2020-10-30 2021-02-02 重庆市蚕业科学技术研究院 Method for rapidly extracting vitamin E from green plant leaves

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Open date: 20081105