CN104610049A - Method for extracting hydroxyl citric acid from garcinia cambogia - Google Patents

Method for extracting hydroxyl citric acid from garcinia cambogia Download PDF

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CN104610049A
CN104610049A CN201510073788.3A CN201510073788A CN104610049A CN 104610049 A CN104610049 A CN 104610049A CN 201510073788 A CN201510073788 A CN 201510073788A CN 104610049 A CN104610049 A CN 104610049A
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hydroxycitric acid
gamboge
citric acid
extracting
moving bed
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CN104610049B (en
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马亚琼
高旭光
贾洪涛
张树元
赵永强
张成亮
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Inner Mongolia Changhui Biological Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • C07C51/47Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Abstract

The invention aims to provide a method for extracting hydroxyl citric acid from garcinia cambogia. The method comprises the following steps: soaking arcinia cambogia into boiling water, extracting and concentrating the arcinia cambogia into extract A; concentrating to obtain a concentrated solution B after dissolving and filtering out pectin; separating and purifying through simulated moving bed chromatography to obtain a component C rich in hydroxyl citric acid; concentrating and recycling a solvent to obtain the hydroxyl citric acid with purity higher than 90%. According to the method for extracting hydroxyl citric acid disclosed by the invention, a simulated moving bed is adopted to separate and purify the hydroxyl citric acid, so that relevant separating parameters are determined, the steps are simple, and the product purity is relatively high. The hydroxyl citric acid obtained by the technical scheme disclosed by the invention has purity higher than 90%, and yield higher than 7%.

Description

A kind of method extracting Hydroxycitric acid from Fructus Resina garciniae
Technical field
The present invention relates to a kind of method extracting Hydroxycitric acid from Fructus Resina garciniae.
Background technology
Hydroxycitric acid (hydroxycitric acid, HCA) be a kind of natural organic acids, be mainly present in abound with in the Indian subcontinent and Sri Lanka western part garcinia plant Garcinia cambogia, Garcinia indica, Garcinia atroviridis fruit shell in.Hydroxycitric acid is soluble in water, is slightly soluble in methyl alcohol, is insoluble in chlorine, sherwood oil and benzene.Hydroxycitric acid is more a lot of by force than natural substrate citric acid to the avidity of citrate lyase, can preferentially be combined with enzyme, suppresses the activity of citrate lyase, reduces body fat synthesis.Therefore, Hydroxycitric acid often by as the main functional component in natural slimming health product, for losing weight, reducing blood fat, depress appetite etc.Field of medicaments, the medicine that Hydroxycitric acid is also applied to preparing cardioprotection, improves the effects such as endurance.
About in prior art to the report of Hydroxycitric acid and derivative thereof, a kind of method of water extraction HCA from gamboge pericarp is disclosed in US5656316, extract is after anionite-exchange resin absorption, and through NaOH/KOH wash-out, elutriant obtains free acid through cation exchange resin column.Deacidite is reported to the separation condition of Hydroxycitric acid crude extract and effect in " ion exchange resin is to the separation and purification of Hydroxycitric acid in Fructus Resina garciniae " (Yi Xinru etc., " food and machinery ", in May, 2014, Vol.30, No.3).A kind of method preparing hydroxycitrate hydrochlorate is disclosed in US6147228.The method is that poach, filtration, filtrate in fresh or dry garcinia plant pericarp, with the process of 80 DEG C of NaOH aqueous solution, are obtained Hydroxycitric acid sodium.
Simulated moving bed chromatography technology introduces in liquid phantom preparing chromatogram by simulation moving-bed design philosophy, both the consumption having maintained liquid phantom preparing chromatogram is little, separation purity is high, and the advantage such as temperature-changeable operation, overcoming again usual liquid phantom preparing chromatogram can not the shortcoming of operate continuously, make it have separating power strong, equipment volume is little, and cost of investment is low, and is particularly conducive to the features such as the system of the high and difficult separation of heat of dissociation sensitivity.
Summary of the invention
The present invention aims to provide a kind of method can extracting Hydroxycitric acid efficiently from gamboge shell.
The involved in the present invention method extracting Hydroxycitric acid from gamboge shell, comprises the following steps:
(1) by the gamboge shell chip of drying, soak extraction in boiling water, extracting solution simmer down to extractum A;
(2) in medicinal extract, add ethanol or methyl alcohol dissolves, filter out pectin, vacuum concentration is concentrated solution B;
(3) concentrated solution B is carried out separating-purifying through simulated moving bed chromatography, obtain the component C being rich in Hydroxycitric acid;
(4) by component C concentration and recovery solvent, the Hydroxycitric acid of purity more than 90% is obtained.
In step of the present invention (1), extraction step can repeat to extract 3-5 time, and united extraction liquid, reconcentration is extractum A.
In step of the present invention (2), preferably add ethanol and dissolve, the mass concentration of concentrated solution B is 3.5g/L.
In step of the present invention (3), the sorbent material that simulated moving bed chromatography is filled is low-pole macroporous adsorbent resin, and water wash zone is purified water, and strippant is 50 ~ 80% ethanol, and its consumption is 1 ~ 3 times of resin volume; Resin absorption regenerated solvent is 95% ethanol or 2 ~ 4% aqueous sodium hydroxide solutions; Adsorption zone flow velocity 1 ~ 2BV/h; Water wash zone flow velocity 1 ~ 3BV/h; Desorption zone flow velocity 1 ~ 3BV/h; Breeding blanket flow velocity 2 ~ 3BV/h; Switching time is 700 ~ 800s; Temperature controls at 40 DEG C ~ 60 DEG C; Pressure-controlling is at 0.2MPa ~ 0.6MPa.
Further, in step of the present invention (3), switching time of simulated moving bed chromatography preferably 700.
Further, in step of the present invention (3), the sorbent material that simulated moving bed chromatography is filled is AB-8.
Although the separating-purifying that simulated moving bed technology can be applied to natural product or medicine has common recognition in the art, but because simulation moving-bed large constructional feature all concentrates into system by key elements such as continuous, the adverse current in chemical industry, rectifying, backflows, it is a multiple degree of freedom, dynamically, be mutually related non-linear system.Therefore, prediction, optimization and control for it are more complicated problems, and especially for a certain natural product kind, the prediction of separation parameter is a very complicated problem.Hydroxycitric acid extracting method of the present invention, adopts and simulation moving-bedly carries out separating-purifying to Hydroxycitric acid, determine relevant separation parameter, step is simple, product purity is higher, and the Hydroxycitric acid purity obtained with technical scheme of the present invention reaches more than 90%, and yield reaches more than 7%.
Embodiment
Embodiment 1
By the gamboge shell (Garcinia cambogia) of 500g drying 700mL boiling deionized water extraction 30min, then repeat extraction 2 times with 400mL boiling deionized water, merge whole extracting solution, simmer down to extractum A.In extractum A, add 95% ethanol dissolve, filter, filtrate enters simulated moving bed chromatography and is separated.Sorbent material is AB-8 macroporous adsorbent resin, and strippant is 50% aqueous ethanolic solution, and its consumption is 3 times of resin volume, water wash zone is purified water, resin absorption regenerated solvent is 95% ethanol, adsorption zone flow velocity 2BV/h, desorption zone flow velocity 3BV/h, water wash zone flow velocity 3BV/h, breeding blanket flow velocity 3BV/h, switching time is 700s, temperature 50 C, pressure 0.5MPa, obtains the component C being rich in Hydroxycitric acid.By component C concentration and recovery ethanol, obtain the Hydroxycitric acid 39g that purity is 91.3%, yield 7.8%.
Embodiment 2
By the gamboge shell (Garcinia cambogia) of 1kg drying 1500mL boiling deionized water extraction 40min, then repeat extraction 3 times with 800mL boiling deionized water, merge whole extracting solution, simmer down to extractum A.In extractum A, add 95% ethanol dissolve, filter, filtrate enters simulated moving bed chromatography and is separated.Sorbent material is AB-8 macroporous adsorbent resin, and strippant is 50% aqueous ethanolic solution, and its consumption is 3 times of resin volume, water wash zone is purified water, resin absorption regenerated solvent is 95% ethanol, adsorption zone flow velocity 2BV/h, desorption zone flow velocity 3BV/h, water wash zone flow velocity 3BV/h, breeding blanket flow velocity 3BV/h, switching time is 700s, temperature 50 C, pressure 0.5MPa, obtains the component C being rich in Hydroxycitric acid.By component C concentration and recovery ethanol, obtain the Hydroxycitric acid 81g that purity is 90.5%, yield 8.1%.
Embodiment 3
By the gamboge shell (Garcinia cambogia) of 2kg drying 3L boiling deionized water extraction 40min, then repeat extraction 3 times with 1500mL boiling deionized water, merge whole extracting solution, simmer down to extractum A.In extractum A, add 95% ethanol dissolve, filter, filtrate enters simulated moving bed chromatography and is separated.Sorbent material is AB-8 macroporous adsorbent resin, and strippant is 50% aqueous ethanolic solution, and its consumption is 3 times of resin volume, water wash zone is purified water, resin absorption regenerated solvent is 95% ethanol, adsorption zone flow velocity 2BV/h, desorption zone flow velocity 3BV/h, water wash zone flow velocity 3BV/h, breeding blanket flow velocity 3BV/h, switching time is 700s, temperature 50 C, pressure 0.5MPa, obtains the component C being rich in Hydroxycitric acid.By component C concentration and recovery ethanol, obtain the Hydroxycitric acid 172g that purity is 90.8%, yield 8.6%.
Embodiment 4
High performance liquid chromatography is adopted to detect Hydroxycitric acid in embodiment 1-3 and Hydroxycitric acid standard substance; Chromatographic condition: chromatographic column is C18 post, 250 × 4.6mm, 5 μm; Moving phase is 0.1% phosphoric acid water-methanol (99:1), isocratic elution; Volumetric flow rate 0.8mL/min; Determined wavelength 210mm; Column temperature 30 DEG C; Sampling volume 10 μ L; Standard substance external standard method is adopted to calculate the content of hydroxycitrate acid product; Analyze through HPLC, the Hydroxycitric acid obtained in embodiment 1-3 and standard substance all have maximum absorption band at retention time 5.3min place.

Claims (5)

1. from gamboge shell, extract a method for Hydroxycitric acid, it is characterized in that comprising the following steps:
(1) by the gamboge shell chip of drying, soak extraction in boiling water, extracting solution simmer down to extractum A;
(2) in medicinal extract, add ethanol or methyl alcohol dissolves, filter out pectin, vacuum concentration is concentrated solution B;
(3) concentrated solution B is carried out separating-purifying through simulated moving bed chromatography, obtain the component C being rich in Hydroxycitric acid; The sorbent material that simulated moving bed chromatography is filled is low-pole macroporous adsorbent resin, and water wash zone is purified water, and strippant is 50 ~ 80% ethanol, and its consumption is 1 ~ 3 times of resin volume; Resin absorption regenerated solvent is 95% ethanol or 2 ~ 4% aqueous sodium hydroxide solutions; Adsorption zone flow velocity 1 ~ 2BV/h; Water wash zone flow velocity 1 ~ 3BV/h; Desorption zone flow velocity 1 ~ 3BV/h; Breeding blanket flow velocity 2 ~ 3BV/h; Switching time is 700 ~ 800s; Temperature controls at 40 DEG C ~ 60 DEG C; Pressure-controlling is at 0.2MPa ~ 0.6MPa;
(4) by component C concentration and recovery solvent, the Hydroxycitric acid of purity more than 90% is obtained.
2. a kind of method extracting Hydroxycitric acid from gamboge shell as claimed in claim 1, is characterized in that: in described step (3), switching time of simulated moving bed chromatography preferably 700.
3. a kind of method extracting Hydroxycitric acid from gamboge shell as claimed in claim 1 or 2, is characterized in that: in described step (3), and the sorbent material that simulated moving bed chromatography is filled is AB-8.
4. a kind of method extracting Hydroxycitric acid from gamboge shell according to any one of claim 1-3, is characterized in that: in described step (2), add ethanol and dissolve, and the mass concentration of concentrated solution B is 3.5g/L.
5. a kind of method extracting Hydroxycitric acid from gamboge shell according to any one of claim 1-4, is characterized in that: in described step (1), and extraction step can repeat to extract 3-5 time, and united extraction liquid, reconcentration is extractum A.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106518653A (en) * 2016-09-24 2017-03-22 合肥信达膜科技有限公司 Membrane extraction process for hydroxycitric acid
CN107473958A (en) * 2017-08-20 2017-12-15 合肥信达膜科技有限公司 A kind of method that hydroxycitric acid is extracted from HCA
CN107927498A (en) * 2017-11-28 2018-04-20 南京伊登生物医学科技有限公司 A kind of beverage composition for treating dental erosion and its application for suppressing lithangiuria and forming and promote dissolve stone
CN110590543A (en) * 2019-08-26 2019-12-20 湖南人文科技学院 Method for extracting hydroxycitrate from lucidus fruit
CN115536521A (en) * 2022-07-17 2022-12-30 李玉山 Preparation method of hydroxycitric acid in lucuma tenuifolia fruits

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
Y. S. LEWIS ET AL.: "(-)-HYDROXYCITRIC ACID-THE PRINCIPAL ACID IN THE FRUITS OF GARCINIA CAMBOGIA DESR.", 《PHYTOCHEMISTRY》, vol. 4, 31 December 1965 (1965-12-31), pages 619 - 625, XP 007903103, DOI: doi:10.1016/S0031-9422(00)86224-X *
刘建奇: "柠檬酸模拟移动床色谱分离的模拟、优化和放大研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》, no. 03, 15 March 2009 (2009-03-15), pages 016 - 9 *
吕裕斌: "模拟移动床分离天然产物的研究", 《中国优秀博硕士学位论文全文数据库 (博士) 工程科技Ⅰ辑》, no. 08, 15 August 2006 (2006-08-15), pages 016 - 2 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106518653A (en) * 2016-09-24 2017-03-22 合肥信达膜科技有限公司 Membrane extraction process for hydroxycitric acid
CN107473958A (en) * 2017-08-20 2017-12-15 合肥信达膜科技有限公司 A kind of method that hydroxycitric acid is extracted from HCA
CN107927498A (en) * 2017-11-28 2018-04-20 南京伊登生物医学科技有限公司 A kind of beverage composition for treating dental erosion and its application for suppressing lithangiuria and forming and promote dissolve stone
CN110590543A (en) * 2019-08-26 2019-12-20 湖南人文科技学院 Method for extracting hydroxycitrate from lucidus fruit
CN110590543B (en) * 2019-08-26 2022-05-06 湖南人文科技学院 Method for extracting hydroxycitrate from lucidus fruit
CN115536521A (en) * 2022-07-17 2022-12-30 李玉山 Preparation method of hydroxycitric acid in lucuma tenuifolia fruits

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