CN106465930A - A kind of extraction process of Lonicera standishii soluble sugar - Google Patents

A kind of extraction process of Lonicera standishii soluble sugar Download PDF

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Publication number
CN106465930A
CN106465930A CN201610860032.8A CN201610860032A CN106465930A CN 106465930 A CN106465930 A CN 106465930A CN 201610860032 A CN201610860032 A CN 201610860032A CN 106465930 A CN106465930 A CN 106465930A
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Prior art keywords
lonicera standishii
gained
weight
filtering residue
lonicera
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CN201610860032.8A
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Chinese (zh)
Inventor
蒋元勇
文继承
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GUILIN MINGXING BIOTECHNOLOGY Co Ltd
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GUILIN MINGXING BIOTECHNOLOGY Co Ltd
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Publication of CN106465930A publication Critical patent/CN106465930A/en
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Abstract

The invention discloses a kind of extraction process of Lonicera standishii soluble sugar, this extraction process is with Lonicera standishii fruit as raw material, Lonicera standishii soluble sugar is obtained through colloid mill grinding, cellulase and the step such as pectinase enzymatic hydrolysis, microwave extraction, supersound extraction, water extraction and filter membrane and polyamide column purification.This extraction process can improve extraction ratio and the efficiency of Lonicera standishii soluble sugar, and this promotes application and the development of Lonicera standishii in certain degree.

Description

A kind of extraction process of Lonicera standishii soluble sugar
Technical field
The present invention relates to a kind of extraction process of Lonicera standishii soluble sugar, belong to technical field of plant extraction.
Background technology
Lonicera standishii (Lonicera standishii) also known as seedless Fructus Pruni pseudocerasi, body-building fruit, belong to Caprifoliaceae Lonicera, for wood This dwarfing wild fruit tree, is distributed in Henan WEST QINLING mountain range.Lonicera standishii fruit deep red, after maturation fruit present pleasing translucent Shape, thin skin, the dense sweet fragrance of fruity.The province mountain area masses such as Shan, sweet, Henan have the custom of Lonicera standishii of searching for food long it is believed that eating its fruit Energy building body, has good health-care effect.This has due to containing soluble sugar, mineral element and vitamin C etc. in Lonicera standishii Effect composition.Wherein, in Lonicera standishii soluble sugar content apparently higher than Fructus Rosae Normalis, Fructus Hippophae and Fructus actinidiae chinensiss, especially its fruit acid content Relatively low (0.18%), sugar-acid ratio is up to 39: 1, and this has fully showed that Lonicera standishii is that a kind of have very much the wild of Development volue to eat raw Fruit.Although soluble sugar content is higher in Lonicera standishii, the extraction about Lonicera standishii soluble sugar is studied still very Limited, this limits application and the development of Lonicera standishii in certain degree.Therefore, continue to explore and research Lonicera standishii soluble sugar Extraction be exceptional values.
Content of the invention
For above-mentioned the deficiencies in the prior art, the technical problem to be solved is that to propose a kind of Lonicera standishii solvable Property sugar extraction process.
A kind of extraction process of Lonicera standishii soluble sugar, comprises the following steps:
1) the Lonicera standishii fruit air-drying is cleaned, sterilized, be ground into 100~120 mesh, and dry 15 under the conditions of 60 DEG C~ After 20min, after adding Lonicera standishii fruit to be dried, 60~80% ethanol stirrings of 5~10 times of weight, use glue after stirring 5~10min Body grinds grinding 20~30min;
2) by step 1) feed liquid of gained is maintained at 40~50 DEG C of temperature, and to adjust pH be 4~6, and it is simultaneously introduced and account for wooden fork rake Complex enzyme zymohydrolysis 1~the 2h of weight 0.1~0.3% after fruits are dry, wherein, compound enzyme is by 4~6 part by weight of cellulose enzymes Mix with 1~3 weight portion pectase;
3) by step 2) after the enzymolysis solution of gained keeps 6~9min sterilizing in 90~100 DEG C, it is placed in and enters under 600~700W Row microwave extraction, extracts 3~5min, filters, obtains filtrate 1 and filtering residue 1, standby;
4) in step 3) add 60~70% ethanol stirrings of 6~8 times of filtering residue 1 weight in the filtering residue 1 of gained, stirring 10~ Grind 30~40min with colloid mill after 15min, be placed in supersonic frequency 30~40kHz, at 30~40 DEG C of temperature, carry out ultrasonic carrying Take, extract 10~15min, filter, obtain filtrate 2 and filtering residue 2, standby;
5) in step 4) add the water stirring of 4~8 times of filtering residue 2 weight in the filtering residue 2 of gained, use after stirring 15~20min Colloid mill grinds 30~60min, and is heated to 90~100 DEG C, extracts 30~40min, filters, obtains filtrate 3, standby;
6) merging filtrate 1,2,3, and filtrate is placed in centrifugation 6~10min, mistake on the centrifuge of 4000~5000 turns/min Filter, obtains Lonicera standishii extracting solution 1, standby;
7) by step 6) the Lonicera standishii extracting solution 1 of gained passes sequentially through the micro-filtration membrane that aperture is 0.1~1 μm, aperture is 0.01~0.2 μm of ultrafilter membrane carries out purification, obtains Lonicera standishii extracting solution 2, standby;
8) by step 7) the Lonicera standishii extracting solution 2 of gained passes through polyamide column chromatography, and first wash post with water and clarify to effluent, With 30~40% ethanol waters, 50~60% ethanol aqueous wash posts, collect 50~60% ethanol elution with respectively again, dense Contracting, is dried, you can obtain Lonicera standishii soluble sugar.
Further,
Step 2) in, by step 1) feed liquid of gained is maintained at temperature 45 C, and to adjust pH be 5, and it is simultaneously introduced and account for wooden fork rake The complex enzyme zymohydrolysis 1.5h of weight 0.2% after fruits are dry, wherein, compound enzyme is by 5 part by weight of cellulose enzymes and 2 weight portions Pectase mixes.
Further,
Step 4) in, in step 3) add 65% ethanol stirring of 7 times of filtering residue 1 weight, stirring in the filtering residue 1 of gained Grind 35min with colloid mill after 12min, be placed in supersonic frequency 35kHz, at 35 DEG C of temperature, carry out supersound extraction, extract 12min, filters, obtains filtrate 2 and filtering residue 2, standby.
Further,
Step 8) in, by step 7) the Lonicera standishii extracting solution 2 of gained passes through polyamide column chromatography, first washes post with water to flowing out Liquid is clarified, then with 35% ethanol water, 55% ethanol aqueous wash post, is collected 55% ethanol elution, concentrate, do with respectively Dry, you can to obtain Lonicera standishii soluble sugar.
Compared with prior art, the invention has the beneficial effects as follows:
1st, the present invention adopts colloid mill grinding, cellulase and pectinase enzymatic hydrolysis technology, microwave extraction technology, supersound extraction Technology, water extraction technology and filter membrane and polyamide column purification technique etc., improve extraction ratio and the efficiency of Lonicera standishii soluble sugar. Wherein, multiple colloid mill grinds, and improves cell crashing ratio, and epigranular, thus improving extraction efficiency;Filter membrane and polyamide Column purification technology, improves impurities removing efficiency, thus improving soluble sugar purification rate.
2nd, the present invention adopts the fruit (including peel, sarcocarp) of whole Lonicera standishii to extract Lonicera standishii, to make Lonicera standishii solvable Property sugared content more increase, reached the purpose of reasonable utilization raw material simultaneously, it is to avoid waste.
Specific embodiment
Embodiment 1
A kind of extraction process of Lonicera standishii soluble sugar, comprises the following steps:
1) the Lonicera standishii fruit air-drying is cleaned, sterilization, be ground into 120 mesh, and after 18min being dried under the conditions of 60 DEG C, After adding Lonicera standishii fruit to be dried, 70% ethanol stirring of 8 times of weight, grinds 25min with colloid mill after stirring 8min;
2) by step 1) feed liquid of gained is maintained at temperature 45 C, and to adjust pH be 5, and it is simultaneously introduced and account for Lonicera standishii fruit and do The complex enzyme zymohydrolysis 1.5h of dry rear weight 0.2%, wherein, compound enzyme is to be mixed by 5 part by weight of cellulose enzymes and 2 weight portion pectases Conjunction forms;
3) by step 2) after the enzymolysis solution of gained keeps 8min sterilizing in 95 DEG C, it is placed in and carries out microwave extraction under 700W, carry Take 4min, filter, obtain filtrate 1 and filtering residue 1, standby;
4) in step 3) add 65% ethanol stirring of 7 times of filtering residue 1 weight in the filtering residue 1 of gained, use glue after stirring 12min Body mill grinds 35min, is placed in supersonic frequency 35kHz, carries out supersound extraction at 35 DEG C of temperature, extracts 12min, filters, obtains Filtrate 2 and filtering residue 2, standby;
5) in step 4) add the water stirring of 6 times of filtering residue 2 weight in the filtering residue 2 of gained, use colloid barreling after stirring 18min Mill 45min, and it is heated to 95 DEG C, extract 35min, filter, obtain filtrate 3, standby;
6) merging filtrate 1,2,3, and filtrate is placed in centrifugation 8min on the centrifuge of 5000 turns/min, filter, obtain wooden fork PAGUO extracting solution 1, standby;
7) by step 6) the Lonicera standishii extracting solution 1 of gained passes sequentially through the micro-filtration membrane that aperture is 1 μm, aperture is 0.2 μm Ultrafilter membrane carries out purification, obtains Lonicera standishii extracting solution 2, standby;
8) by step 7) the Lonicera standishii extracting solution 2 of gained passes through polyamide column chromatography, and first wash post with water and clarify to effluent, With 35% ethanol water, 55% ethanol aqueous wash post, collected 55% ethanol elution, concentrate, be dried with respectively again, you can Obtain Lonicera standishii soluble sugar.
Embodiment 2
A kind of extraction process of Lonicera standishii soluble sugar, comprises the following steps:
1) the Lonicera standishii fruit air-drying is cleaned, sterilization, be ground into 100 mesh, and after 15min being dried under the conditions of 60 DEG C, After adding Lonicera standishii fruit to be dried, 60% ethanol stirring of 5 times of weight, grinds 20min with colloid mill after stirring 5min;
2) by step 1) feed liquid of gained is maintained at 40 DEG C of temperature, and to adjust pH be 4, and it is simultaneously introduced and account for Lonicera standishii fruit and do The complex enzyme zymohydrolysis 1h of dry rear weight 0.1%, wherein, compound enzyme is by 4 part by weight of cellulose enzymes and the mixing of 1 weight portion pectase Form;
3) by step 2) after the enzymolysis solution of gained keeps 6min sterilizing in 90 DEG C, it is placed in and carries out microwave extraction under 600W, carry Take 3min, filter, obtain filtrate 1 and filtering residue 1, standby;
4) in step 3) add 60% ethanol stirring of 6 times of filtering residue 1 weight in the filtering residue 1 of gained, use glue after stirring 10min Body mill grinds 30min, is placed in supersonic frequency 30kHz, carries out supersound extraction at 30 DEG C of temperature, extracts 10min, filters, obtains Filtrate 2 and filtering residue 2, standby;
5) in step 4) add the water stirring of 4 times of filtering residue 2 weight in the filtering residue 2 of gained, use colloid barreling after stirring 15min Mill 30min, and it is heated to 90 DEG C, extract 30min, filter, obtain filtrate 3, standby;
6) merging filtrate 1,2,3, and filtrate is placed in centrifugation 6min on the centrifuge of 4000 turns/min, filter, obtain wooden fork PAGUO extracting solution 1, standby;
7) by step 6) the Lonicera standishii extracting solution 1 of gained passes sequentially through the micro-filtration membrane that aperture is 0.1 μm, aperture is 0.01 μm Ultrafilter membrane carry out purification, obtain Lonicera standishii extracting solution 2, standby;
8) by step 7) the Lonicera standishii extracting solution 2 of gained passes through polyamide column chromatography, and first wash post with water and clarify to effluent, With 30% ethanol water, 50% ethanol aqueous wash post, collected 50% ethanol elution, concentrate, be dried with respectively again, you can Obtain Lonicera standishii soluble sugar.
Embodiment 3
A kind of extraction process of Lonicera standishii soluble sugar, comprises the following steps:
1) the Lonicera standishii fruit air-drying is cleaned, sterilization, be ground into 120 mesh, and after 20min being dried under the conditions of 60 DEG C, After adding Lonicera standishii fruit to be dried, 80% ethanol stirring of 10 times of weight, grinds 30min with colloid mill after stirring 10min;
2) by step 1) feed liquid of gained is maintained at temperature 50 C, and to adjust pH be 6, and it is simultaneously introduced and account for Lonicera standishii fruit and do The complex enzyme zymohydrolysis 2h of dry rear weight 0.3%, wherein, compound enzyme is by 6 part by weight of cellulose enzymes and the mixing of 3 weight portion pectases Form;
3) by step 2) after the enzymolysis solution of gained keeps 9min sterilizing in 100 DEG C, it is placed in and carries out microwave extraction under 700W, carry Take 5min, filter, obtain filtrate 1 and filtering residue 1, standby;
4) in step 3) add 70% ethanol stirring of 8 times of filtering residue 1 weight in the filtering residue 1 of gained, use glue after stirring 15min Body mill grinds 40min, is placed in supersonic frequency 40kHz, carries out supersound extraction at 40 DEG C of temperature, extracts 15min, filters, obtains Filtrate 2 and filtering residue 2, standby;
5) in step 4) add the water stirring of 8 times of filtering residue 2 weight in the filtering residue 2 of gained, use colloid barreling after stirring 20min Mill 60min, and it is heated to 100 DEG C, extract 40min, filter, obtain filtrate 3, standby;
6) merging filtrate 1,2,3, and filtrate is placed in centrifugation 10min on the centrifuge of 5000 turns/min, filter, obtain wooden fork PAGUO extracting solution 1, standby;
7) by step 6) the Lonicera standishii extracting solution 1 of gained passes sequentially through the micro-filtration membrane that aperture is 1 μm, aperture is 0.2 μm Ultrafilter membrane carries out purification, obtains Lonicera standishii extracting solution 2, standby;
8) by step 7) the Lonicera standishii extracting solution 2 of gained passes through polyamide column chromatography, and first wash post with water and clarify to effluent, With 40% ethanol water, 60% ethanol aqueous wash post, collected 60% ethanol elution, concentrate, be dried with respectively again, you can Obtain Lonicera standishii soluble sugar.
In addition, the soluble sugar that applicant prepares to embodiment 1~3 is measured, measurement result is as shown in table 1.
Table 1 soluble sugar measurement result
Type Soluble sugar yield (%)
Embodiment 1 6.92
Embodiment 2 6.81
Embodiment 3 6.89
Certainly, it is that the preferred embodiments of the disclosure is described in detail above, not the present invention is limited with this Practical range, the equivalence changes that all principles under this invention, construction and structure are made, the protection of the present invention all should be covered by In the range of.

Claims (4)

1. a kind of extraction process of Lonicera standishii soluble sugar it is characterised in that:Comprise the following steps:
1) the Lonicera standishii fruit air-drying is cleaned, sterilized, be ground into 100~120 mesh, and dry 15 under the conditions of 60 DEG C~ After 20min, after adding Lonicera standishii fruit to be dried, 60~80% ethanol stirrings of 5~10 times of weight, use glue after stirring 5~10min Body grinds grinding 20~30min;
2) by step 1) feed liquid of gained is maintained at 40~50 DEG C of temperature, and to adjust pH be 4~6, and it is simultaneously introduced and account for Lonicera standishii fruit Do solid work the complex enzyme zymohydrolysis 1~2h of dry rear weight 0.1~0.3%, wherein, compound enzyme is by 4~6 part by weight of cellulose enzymes and 1 ~3 weight portion pectases mix;
3) by step 2) after the enzymolysis solution of gained keeps 6~9min sterilizing in 90~100 DEG C, be placed in carry out under 600~700W micro- Ripple extracts, and extracts 3~5min, filters, obtains filtrate 1 and filtering residue 1, standby;
4) in step 3) add 60~70% ethanol stirrings of 6~8 times of filtering residue 1 weight in the filtering residue 1 of gained, stirring 10~ Grind 30~40min with colloid mill after 15min, be placed in supersonic frequency 30~40kHz, at 30~40 DEG C of temperature, carry out ultrasonic carrying Take, extract 10~15min, filter, obtain filtrate 2 and filtering residue 2, standby;
5) in step 4) add the water stirring of 4~8 times of filtering residue 2 weight in the filtering residue 2 of gained, use colloid after stirring 15~20min Mill grinding 30~60min, and it is heated to 90~100 DEG C, extract 30~40min, filter, obtain filtrate 3, standby;
6) merging filtrate 1,2,3, and filtrate is placed in centrifugation 6~10min on the centrifuge of 4000~5000 turns/min, filter, Obtain Lonicera standishii extracting solution 1, standby;
7) by step 6) the Lonicera standishii extracting solution 1 of gained passes sequentially through the micro-filtration membrane that aperture is 0.1~1 μm, aperture be 0.01~ 0.2 μm of ultrafilter membrane carries out purification, obtains Lonicera standishii extracting solution 2, standby;
8) by step 7) the Lonicera standishii extracting solution 2 of gained passes through polyamide column chromatography, and first wash post with water and clarify to effluent, then use Respectively with 30~40% ethanol waters, 50~60% ethanol aqueous wash posts, collect 50~60% ethanol elution, concentrate, It is dried, you can obtain Lonicera standishii soluble sugar.
2. Lonicera standishii soluble sugar according to claim 1 extraction process it is characterised in that:Step 2) in, by step 1) feed liquid of gained is maintained at temperature 45 C, and adjusts pH for 5, is simultaneously introduced and accounts for weight 0.2% after Lonicera standishii fruit is dried Complex enzyme zymohydrolysis 1.5h, wherein, compound enzyme is to be mixed by 5 part by weight of cellulose enzymes and 2 weight portion pectases.
3. Lonicera standishii soluble sugar according to claim 1 extraction process it is characterised in that:Step 4) in, in step 3) add 65% ethanol stirring of 7 times of filtering residue 1 weight in the filtering residue 1 of gained, after stirring 12min, grind 35min with colloid mill, and It is placed in supersonic frequency 35kHz, at 35 DEG C of temperature, carries out supersound extraction, extract 12min, filter, obtain filtrate 2 and filtering residue 2, standby With.
4. Lonicera standishii soluble sugar according to claim 1 extraction process it is characterised in that:Step 8) in, by step 7) the Lonicera standishii extracting solution 2 of gained passes through polyamide column chromatography, first washes post with water and clarifies to effluent, then with using 35% second respectively Alcohol-water solution, 55% ethanol aqueous wash post, collect 55% ethanol elution, concentrate, and are dried, you can obtain Lonicera standishii solubility Sugar.
CN201610860032.8A 2016-09-27 2016-09-27 A kind of extraction process of Lonicera standishii soluble sugar Pending CN106465930A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112877481A (en) * 2020-12-28 2021-06-01 河北省农林科学院遗传生理研究所(河北省农林科学院农产品质量安全研究中心) Purification treatment method for soluble sugar in fruits and vegetables

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101461514A (en) * 2009-01-22 2009-06-24 韩金光 Bitter melon extract and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101461514A (en) * 2009-01-22 2009-06-24 韩金光 Bitter melon extract and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
杨明等: "《药剂学》", 31 August 2014, 中国医药科技出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112877481A (en) * 2020-12-28 2021-06-01 河北省农林科学院遗传生理研究所(河北省农林科学院农产品质量安全研究中心) Purification treatment method for soluble sugar in fruits and vegetables

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Application publication date: 20170301