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Method of combined extraction of essential oil, pectin, hesperidin, synephrine and limonin from citrus

A technology for joint extraction and limonin, which is applied in the field of joint extraction of essential oils, pectin, hesperidin, synephrine and limonin, can solve the problem that the economic value of citrus peel processing and utilization is reduced, and joint extraction and citrus peel cannot be realized. Low utilization rate and other problems, to achieve the effect of reducing the enzymatic hydrolysis time and enzyme dosage, saving time and labor costs, and the production process being safe and easy to operate

Active Publication Date: 2016-06-15
HUNAN AGRI PRODS PROCESSING INST
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

None of the above methods can realize the joint extraction of five active ingredients such as pectin, essential oil, hesperidin, synephrine and limonin, and there are disadvantages such as low utilization rate of citrus peel and waste of resources.
Pressing is one of the main technologies for large-scale industrial extraction of citrus essential oils. In order to increase the yield of essential oils, lime or CaCl 2 Treat citrus peels to increase the hardness of citrus peels to increase the pressing effect and the yield of essential oils, but lime will cause the degradation of pectin, and the presence of calcium ions prevents pectin from being extracted by traditional hydrochloric acid method; steam distillation is an industrial production method Another important method of citrus peel essential oil, this method exposes the active ingredients in citrus peel to high temperature environment for a long time, which easily leads to the decomposition of thermally unstable components, such as essential oil, hesperidin, pectin, lemon bitter Alkaline extraction and acid analysis method is a commonly used method for extracting hesperidin, which uses a large amount of strong acid and alkali, which is easy to pollute the environment; the waste liquid and waste residue produced in the process of joint production of citrus components are not If it is fully utilized, it is discarded, and the economic value of citrus peel processing and utilization is greatly reduced, resulting in a great waste of resources

Method used

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  • Method of combined extraction of essential oil, pectin, hesperidin, synephrine and limonin from citrus
  • Method of combined extraction of essential oil, pectin, hesperidin, synephrine and limonin from citrus
  • Method of combined extraction of essential oil, pectin, hesperidin, synephrine and limonin from citrus

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] see figure 1 , a method for jointly extracting essential oil, pectin, hesperidin, synephrine and limonin from citrus, comprising the steps of:

[0042] (1) Take fresh and clean citrus, inactivate plant enzymes at 100°C for 8 minutes, pierce the epidermis with an acupuncture dermabrasion machine, rinse the surface of citrus with water spray, and collect the oil-water mixture, skin residue and dermabrasion citrus respectively.

[0043] (2) Enzymolyze the skin dregs and peeled citrus with cellulase, specifically: add 11.5% ammonium sulfate to the mixture of skin dregs and grinded citrus according to the ratio of solid to liquid (w / v) of 1:8 and 0.4% cellulase, shaken in a water bath at 45°C for 45 minutes; then heated at 85°C for 5 minutes, and ultrasonically extracted for 90 minutes to obtain the enzymatic hydrolysis product. Squeeze and filter the enzymatic hydrolysis product with a screw press, and collect the squeeze liquid and skin dregs respectively.

[0044] (3) C...

Embodiment 2

[0076] Investigate the influence of different cation exchange resins on the extraction effect of synephrine:

[0077] Weigh 30mL of different types of cation exchange resins (732, D72, Dowex50(H+), DL08, DL10, D006) that have been processed, and pack them into columns (300mm×15mm) by wet method, adjust the volume flow rate to 2.5BV / h, and implement each addition The aqueous phase collected in example 1 step (3), collect effluent, carry out elution with ethyl acetate, collect eluent; Measure the mass concentration of synephrine in effluent and eluent, calculate adsorption capacity and desorption Table 1 shows the results of adsorption capacity and resolution capacity of different cation exchange resins.

[0078] Adsorption rate (%) = (C 0 -C 1 ) / C 0 ×100

[0079] Desorption rate (%) = (C 2 / )C 0 -C 1 ))×100

[0080] In the formula: C 0 is the solution concentration of the target component in the initial sample, mg / mL;

[0081] C 1 is the concentration of the target c...

Embodiment 3

[0087] Investigate the influence of different macroporous resins on the extraction effect of limonin:

[0088] Weigh each 2.0g of 7 kinds of macroporous resins that have been processed, add the supernatant obtained in 30mL embodiment 1 step (6) respectively, leave to stand at room temperature and fully adsorb and reach saturation (24h) filter, measure the sample before and after adsorption The content of limonin in the liquid and the content of limonin in the eluate after elution with 70% ethanol, Table 2 shows the results of the adsorption capacity and analytical capacity of different macroporous resins.

[0089] Calculate the adsorption rate and desorption rate of limonin by the macroporous resin according to the following formula.

[0090] Adsorption rate (%) = (C 0 -C 1 ) / C 0 ×100

[0091] Desorption rate (%) = (C 2 / )C 0 -C 1 ))×100

[0092] In the formula: C 0 is the solution concentration of the target component in the initial sample, mg / mL;

[0093] C 1is th...

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Abstract

The invention relates to the technical field of plant separation and extraction, and in particularly discloses a method of combined extraction of essential oil, pectin, hesperidin, synephrine and limonin from citrus. The method comprises the following steps: inactivating the citrus, buffing and performing enzymolysis to obtain essential oil, a water phase and skin residues; separating the water phase through strong acidic cation-exchange resin to collect effusive liquid, and eluting to obtain synephrine; separating the effusive liquid using ultra-filtration method to obtain pectin and liquid passing through the ultra-filtration film; refluxing and extracting the liquid passing through the ultra-filtration film using ethanol to obtain supernatant and filter residue; crystallizing, and freeze-drying the filter residues to obtain aurantiamarin; separating the supernatant using macroporous resin, and eluting using ethanol to obtain limonin. The method is used for processing fresh citrus to co-produce the citrus pericarp essential oil, pectin, hesperidin, synephrine and limonin; the utilization rate of the resource is improved, the environment pollution is reduced, and the economic and social benefits are notable.

Description

technical field [0001] The invention relates to the technical field of plant separation and extraction, in particular to a method for jointly extracting essential oil, pectin, hesperidin, synephrine and limonin from citrus. Background technique [0002] Citrus peel is a by-product of citrus processing, accounting for about 20% of the whole fruit weight. It is rich in natural active ingredients such as pectin, essential oil, hesperidin, synephrine and limonin, and can be used as an important medicine after extraction Industry, food additives and daily chemicals. [0003] At present, there are related technologies for the joint extraction of essential oil and pectin, or flavonoids and pectin, or essential oil and hesperidin in citrus peel. Extract pectin; or extract flavonoids first, then extract pectin. None of the above methods can realize the joint extraction of five active ingredients such as pectin, essential oil, hesperidin, synephrine and limonin, and there are disadv...

Claims

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Application Information

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IPC IPC(8): C07H17/07C07H1/08C07C213/10C07C215/60C07J73/00C11B9/02C08B37/06
CPCC07C213/10C07H1/08C07H17/07C07J73/003C08B37/0003C08B37/0045C11B9/02C07C215/60
Inventor 单杨李高阳梁曾恩妮付复华张菊华苏东林刘伟
Owner HUNAN AGRI PRODS PROCESSING INST
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