CN109259052A - Hydroxymethylfurfural removal methods in a kind of honey - Google Patents
Hydroxymethylfurfural removal methods in a kind of honey Download PDFInfo
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- CN109259052A CN109259052A CN201811314385.3A CN201811314385A CN109259052A CN 109259052 A CN109259052 A CN 109259052A CN 201811314385 A CN201811314385 A CN 201811314385A CN 109259052 A CN109259052 A CN 109259052A
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- honey
- hydroxymethylfurfural
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
- A23L5/27—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption
- A23L5/273—Removal of unwanted matter, e.g. deodorisation or detoxification by chemical treatment, by adsorption or by absorption using adsorption or absorption agents, resins, synthetic polymers, or ion exchangers
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L21/00—Marmalades, jams, jellies or the like; Products from apiculture; Preparation or treatment thereof
- A23L21/20—Products from apiculture, e.g. royal jelly or pollen; Substitutes therefor
- A23L21/25—Honey; Honey substitutes
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- Health & Medical Sciences (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Jellies, Jams, And Syrups (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
Hydroxymethylfurfural removal methods in a kind of honey, deionized water is added into honey, and stirring is uniformly mixed honey with water, then macroporous absorbent resin is added, 5-HMF in honey is removed under stirring, refilters, be concentrated, obtains the honey of removing hydroxymethylfurfural.5-HMF in honey is removed with macroporous adsorption resin technology, realize that the green to 5-HMF harmful substance in honey removes, its limitation is up to state standards and EU criteria, and it is suitable for a variety of honey such as acacia honey, honey of lungan flowers, fructus lycii honey, buckwheat honey, Mel Jujubae, honey of lychee flowers and rape honey；Macroporous absorbent resin belongs to physical method, honey physical and chemical index in honey and aesthetic quality are influenced smaller, honey after this method removes 5-HMF can realize making full use of for honey, economic benefits directly as additive application in feed industry, food industry.
Description
Technical field
The present invention relates to hydroxymethylfurfural removal methods in a kind of honey.
Background technique
Honey is the major product of honeybee, is honeybee herborization nectar, secretion or honeydew, mixes with itself secretion
Afterwards, natural sweet substance made of sufficiently being made.Honey vouchsafes the precious gift of the mankind as the Nature, is rich in glucose, fruit
A variety of nutriments such as sugar, protein, amino acid, vitamin, microelement and phenols, in nutritional supplementation, disease prevention, strong
Physique etc. has unique effect.China is bee-keeping big country of the world, bee colony quantity, bee-keeping practitioner, honey output and bee
Sweet export volume is at the forefront in the world, play an important role on world bee's product market.However, honey acquisition, processing and
During storage pin, often generating some poisonous and harmful substances, (such as microorganism, metal ion, 5 hydroxymethyl furfural, pesticide are residual
Stay, antibiotic etc.), very big hidden danger is caused to the safety in production of honey, consumption and outlet.
5 hydroxymethyl furfural (5-HMF) is to be easy to the one kind generated in honey processing and storage to have bad smell
Black noxious material.5-HMF content is very low in Fresh Honey, does not exceed 10mg/kg generally, however, honey is in hot-working
In the process or storage requirement can all not generate a large amount of 5-HMF at that time.Honey heat when be easy to occur Maillard reaction or
Dehydration and generate 5-HMF；In addition, during storage, when 5-HMF content can be increased and be stored with reserve temperature in honey
Between extend gradually increase, be even exceeded.5-HMF, which exists, does not only result in the change of honey flavor and color burn, and influences honey
Edible safety.Studies have shown that 5-HMF is irritant to eyes, mucous membrane or skin, intake can excessively cause to be poisoned, or even draw
Hair cancer causes animal band myoparalysis and visceral injury.In international trade, 5-HMF belongs to strong inspection index, and countries in the world are to bee
5-HMF makes limitation regulation in honey, China Standard for Honey GH/T18796-2012 regulation, and 5-HMF content requirement in honey≤
40mg/kg。
5-HMF content is to measure the important indicator of honey quality in honey, can reflect honey freshness, working process item
Part and adulterated situation.When 5-HMF content is high in honey, often indicate that honey purity is inadequate, hot-working is excessive or storage
Environment is unreasonable, period of storage is too long.Mode is raised bees mostly based on tradition, dispersion, small-scale family's feeding manner by China, in order to
It devotes exclusive attention to output, bee-keeping mode has certain predatoriness, causes honey raw material quality very different, to guarantee that final honey index is closed
Lattice generally use higher-strength heating and carry out processing concentration；In addition, honey is usually stored and transported and is sold at room temperature, it is extraneous
Environmental condition is very big on honey quality influence, causes 5-HMF content in commercially available honey often exceeded.5-HMF is exceeded not in honey
The quality safety for only influencing honey, is also directly related to numerous beekeepers, bee product enterprise and consumer's vital interests.Especially exist
In honey outlet, once discovery 5-HMF content is exceeded, will be destroyed, huge economic loss is brought to enterprise and beekeeper.Cause
This, reduces 5-HMF content in honey, has important social effect and economic value to honey safety and quality is improved.
Up to the present, about 5-HMF content in honey is reduced, there are no a kind of good methods both at home and abroad.There is research to use
Active carbon adsorption removes 5-HMF in honey, i.e., by changing activated carbon particle size size, reaches and adsorb purpose to 5-HMF, but is living
Property carbon adsorption has disadvantages that, such as adsorptive selectivity is poor, mechanical strength is low, service life is short and operating cost is high.And
Macroporous absorbent resin has many advantages, such as that selectivity is good, adsorption capacity is big, regeneration treatment is convenient and it is rapid to adsorb, and a large amount of
It is clarified in decoloration process for fruit drink, but lacks the removing research that macroporous adsorption resin technology is applied to 5-HMF in honey.
Summary of the invention
The present invention provides a kind of methods of hydroxymethylfurfural in removing honey, through macroporous adsorption resin technology, in not shadow
Under the premise of ringing or influencing honey nutritional ingredient and bioactive ingredients less, the green removing of hydroxymethylfurfural, 5-HMF limitation are realized
It is up to state standards and EU criteria requirement, utilizes the exceeded honey of 5-HMF content again.
The purpose of the present invention is achieved through the following technical solutions:
Hydroxymethylfurfural removal methods in a kind of honey, deionized water is added into honey, and stirring mixes honey with water
Uniformly, macroporous absorbent resin is then added, 5-HMF in honey is removed under stirring, is refiltered, is concentrated, is taken off
Except the honey of hydroxymethylfurfural.
A further improvement of the present invention lies in that the mass ratio of honey and water is (0.8-1.2): 1.
A further improvement of the present invention lies in that the mass ratio of honey and water is 1:1.
A further improvement of the present invention lies in that macroreticular resin LSA-960, XDA-300 or LSI-3 type macroporous absorption tree
Rouge.
A further improvement of the present invention lies in that macroreticular resin is LSI-3 type macroporous absorbent resin
A further improvement of the present invention lies in that carrying out removing design parameter to 5-HMF in honey under stirring are as follows: per ton
43-45kg resin is added in honey, and control removal temperature is 25 DEG C, the stirring removing 80min under 100rpm/min revolving speed.
A further improvement of the present invention lies in that using 150-200 mesh net filtration.
A further improvement of the present invention lies in that the honey obtained after filtering is carried out after 45-50 DEG C of preheating 20min dense
Contracting.
A further improvement of the present invention lies in that the temperature of concentration is 45-55 DEG C, vacuum degree 0.05-0.07Mpa.
A further improvement of the present invention lies in that being concentrated into honey moisture content is 18-20%.
Compared with prior art, the invention has the benefit that (1) with macroporous adsorption resin technology to 5- in honey
HMF is removed, and realizes that the green to 5-HMF harmful substance in honey removes, and limitation is up to state standards and EU criteria,
And it is suitable for a variety of honey such as acacia honey, honey of lungan flowers, fructus lycii honey, buckwheat honey, Mel Jujubae, honey of lychee flowers and rape honey；(2) macropore
Absorption resin belongs to physical method, smaller on honey physical and chemical index in honey and aesthetic quality's influence, after this method removes 5-HMF
Honey can realize making full use of for honey, economic benefit can directly as additive application in feed industry, food industry
It sees；(3) present invention use macroporous adsorption resin technology regeneration treatment simplicity, less energy consumption, use condition mildly, adsorption rate
Fastly, safe and pollution-free, resin regeneration is easy, and cost is relatively low.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
The method of the present invention includes the following steps:
(1) appropriate amount of deionized water is added into honey, being sufficiently stirred is uniformly mixed honey with water；
(2) suitable macroporous absorbent resin is added in honey, 5-HMF in honey is removed under stirring；
(3) resin is recovered by filtration with 150-200 mesh screen in the honey for removing 5-HMF；
(4) honey is concentrated in vacuo after recycling resin, and honey moisture is concentrated to 18-20%.
In above-mentioned steps (1), the mass ratio of honey and water is 0.8:1-1.2:1, preferably 1:1.
Macroreticular resin in above-mentioned steps (2) is LSA-960, XDA-300 or LSI-3 type macroporous absorbent resin, preferably
LSI-3 type.
43-45kg resin is added by honey per ton, control adsorption temp is 25 DEG C, right under the stirring of 100rpm/min revolving speed
5-HMF removes 80min in honey.
In above-mentioned steps (4), honey is concentrated in vacuo after 45-50 DEG C of preheating 20min after recycling resin, thickening temperature
45-55 DEG C, vacuum degree 0.05-0.07Mpa.
LSA-960, XDA-300 or LSI-3 type macroporous absorbent resin used in the present invention: it is purchased from Xi'an Lan Xiao scientific & technical corporation.
70mg5-HMF standard items are added in 1kg acacia honey, is placed under 4 DEG C of cryogenic conditions and saves, as simulating cutting is store
The exceeded honey sample of 5-HMF content after depositing.
The screening of optimal macroporous absorbent resin type:
The exceeded acacia honey sample of 100.0g5-HMF content is accurately weighed, is uniformly mixed with distilled water with quality 1:1, room temperature
Lower sonic oscillation 10min.6 parts, every part of 20mL, 1 part are classified as blank control, remaining 5 parts be separately added into 0.3g LSI-3,
LSA-960, XDA-300, LX-260 and LX-670 type macroreticular resin, are stirred under 100rpm/min revolving speed under 25 DEG C of constant temperatures
2h.Absorption front and back 5-HMF content is measured with high performance liquid chromatograph, and calculates adsorption rate.
Referring to table 1, the results showed that LSI-3 type macroreticular resin is best to 5-HMF removal effect in honey.
Removal efficiency of the 1 variety classes macroporous absorbent resin of table to 5-HMF in honey
The optimization of macroporous absorbent resin removing process condition is as follows:
(1) determination of optimal resin adsorption temp
The exceeded acacia honey sample of 60.0g5-HMF content is accurately weighed, is uniformly mixed with distilled water with quality 1:1, under room temperature
Sonic oscillation 10min.4 parts, every part of 20mL are classified as, wherein 1 part is blank control, remaining 3 parts of addition quality are
0.3gLSI-3 resin, respectively at stirring 2h under 100rpm/min revolving speed at 45 DEG C, 35 DEG C and 25 DEG C of adsorption temp.
Referring to table 2, as the result is shown: LSI-3 type resin is at 25 DEG C to 5-HMF removal efficiency highest.
Removal efficiency of the LSI-3 type resin to 5-HMF in honey under 2 different temperatures of table
(2) determination of optimum resin and honey quality ratio
The exceeded acacia honey of 120.0g 5-HMF content is accurately weighed, is uniformly mixed with distilled water with quality 1:1, is surpassed under room temperature
Sound oscillation 10min.9 parts, every part of 20mL, 1 part are classified as blank control, remaining 8 parts are separately added into 0.1g to 0.8gLSI-3
Resin stirs 2h under 100rpm/min revolving speed under 25 DEG C of stationary temperatures.
Referring to table 3, as the result is shown: LSI-3 type macroreticular resin acts on as resin quality increases the removing of 5-HMF in honey
Add and gradually increase, but after resin quality reaches 44g/kg honey, removal efficiency growth rate slows down, and comprehensively considers economic factor,
Therefore choosing resin quality 44g/kg honey is the optimum resin dosage for removing 5-HMF in honey.
Removal efficiency of the 3 different quality LSI-3 type resin of table to 5-HMF in honey
(3) determination of optimal resin adsorption time
The exceeded acacia honey sample of 5-HMF content is accurately weighed, is uniformly mixed with distilled water with quality 1:1, it is ultrasonic under room temperature
Vibrate 10min.7 parts, every part of 20mL are classified as, wherein 1 part is blank control, remaining 6 parts to be separately added into 0.3gLSI-3 type big
Hole resin stirs at 25 DEG C of shaking bath under 100rpm/min revolving speed, in 20,40,60,80,100,120min and 150min
Sampling measures 5-HMF content in honey sample solution with high performance liquid chromatograph, and calculates adsorption rate.
Referring to table 4, as the result is shown: as time went on, LSI-3 resin enhances the removing ability of 5-HMF in honey,
80min or so reaches balance, therefore choosing LSI-3 type macroreticular resin is 80min to the optimal adsorption time of 5-HMF in honey.
To the removal efficiency of 5-HMF in honey under table 4LSI-3 resin difference adsorption time
(4) verifying of macroporous absorbent resin removing process condition
Using LSI-3 type resin, resin quality 44g/Kg honey, at 25 DEG C of adsorption temp, adsorption time is 80min optimization
Under the conditions of 5-HMF in acacia honey is removed, referring to table 5, the results showed that in optimal conditions, through LSI-3 type resin adsorption
Afterwards, 5-HMF removal efficiency reaches 60% or more, and 5-HMF content is down to 40mg/kg hereinafter, meeting national standard in honey.
Table 5LSI-3 type resin is in optimal conditions to the removal efficiency of 5-HMF in honey
Macroporous absorbent resin removes the influence to honey nutritive index:
Detecting LSI-3 type macroporous absorbent resin, the conductivity of acacia honey, amylase value, pH and reduced sugar contain before and after the processing
Amount, after as a result handling referring to table 6:LSI-3 type macroporous absorbent resin, amylase value only has faint reduction in honey, and to conductance
Rate, pH and content of reducing sugar do not influence.
The conductivity of acacia honey, amylase value, pH and the reduction before and after the processing of table 6LSI-3 type macroporous absorbent resin
Sugared content influences
Macroporous absorbent resin removes the applicability of 5-HMF in honey:
Honey of lungan flowers, fructus lycii honey, buckwheat honey, Mel Jujubae, honey of lychee flowers and six kinds of rape honey different honey are chosen, LSI-3 is utilized
Type macroporous absorbent resin removes 5-HMF in variety classes honey.
Referring to table 7, the results showed that, fructus lycii honey higher for 5-HMF content, Mel Jujubae, honey of lychee flowers and rape honey, warp
The removal efficiency of 5-HMF respectively reaches 44.31%, 50.37%, 45.66% and 60.45% after LSI-3 type resin adsorption, for 5-
HMF comparision contents low honey of lungan flowers and buckwheat honey, are not detected 5-HMF after resin adsorption.This explanation, LSI-3 type macropore are inhaled
Attached resin all has good removal effect to 5-HMF in variety classes honey, has certain generality.
Removal effect of the table 7LSI-3 type macroporous absorbent resin to 5-HMF in variety classes honey
Embodiment 1
The exceeded honey of 1t5-HMF content (5-HMF content is greater than 40mg/kg) is placed in jacketed pan, 1t deionization is added
Water, being sufficiently stirred is uniformly mixed honey with water, and the LSI-3 macroporous absorbent resin of 44kg, the control of interlayer pot temperature is then added
At 25 DEG C, 80min is stirred under 100rpm/min revolving speed, to complete the removing of 5-HMF in honey.Removing 5-HMF honey is used
To recycle resin, filtered honey is placed in 50 DEG C of jacketed pans and preheats 20min 150 mesh net filtrations.By preheated honey-pump
Enter in vacuum concentration pot, under the conditions of thickening temperature is 45 DEG C, vacuum degree is 0.06Mpa, honey moisture is concentrated to 18%, is obtained
To up-to-standard honey (5-HMF content is less than 40mg/kg), that is, remove the honey of hydroxymethylfurfural.
Embodiment 2
By mulse mass ratio 0.8:1, deionized water is added into Mel Jujubae, stirring is uniformly mixed honey with water, then
Be added XDA-300 type macroporous absorbent resin, wherein by honey per ton be added 43kg resin, under 100rpm/min revolving speed and
Removing 80min carried out to 5-HMF in honey at 25 DEG C, then uses 160 mesh net filtrations, then preheat at 45 DEG C after 20min
55 DEG C, vacuum degree is concentrated into honey moisture content under being 0.05-0.07Mpa be 20%, obtains the jujube flower of removing hydroxymethylfurfural
Honey.
Embodiment 3
By mulse mass ratio 1.2:1, deionized water is added into fructus lycii honey, stirring is uniformly mixed honey with water, then
Be added LSA-960 type macroporous absorbent resin, wherein by honey per ton be added 45kg resin, under 100rpm/min revolving speed and
Removing 80min carried out to 5-HMF in honey at 25 DEG C, then uses 200 mesh net filtrations, then preheat at 45 DEG C after 20min
50 DEG C, vacuum degree is concentrated into honey moisture content under being 0.05-0.07Mpa be 19%, obtains the fructus lycii of removing hydroxymethylfurfural
Honey.
Claims (10)
1. hydroxymethylfurfural removal methods in a kind of honey, which is characterized in that deionized water is added into honey, stirring makes honey
It is uniformly mixed with water, macroporous absorbent resin is then added, 5-HMF in honey is removed under stirring, is refiltered, it is dense
Contracting obtains the honey of removing hydroxymethylfurfural.
2. hydroxymethylfurfural removal methods in a kind of honey according to claim 1, which is characterized in that the matter of honey and water
Amount is than being (0.8-1.2): 1.
3. hydroxymethylfurfural removal methods in a kind of honey according to claim 2, which is characterized in that the matter of honey and water
Amount is than being 1:1.
4. hydroxymethylfurfural removal methods in a kind of honey according to claim 1, which is characterized in that macroreticular resin is
LSA-960, XDA-300 or LSI-3 type macroporous absorbent resin.
5. hydroxymethylfurfural removal methods in a kind of honey according to claim 4, which is characterized in that macroreticular resin is
LSI-3 type macroporous absorbent resin.
6. hydroxymethylfurfural removal methods in a kind of honey according to claim 1, which is characterized in that right under stirring
5-HMF carries out removing design parameter in honey are as follows: 43-45kg resin is added by honey per ton, control removal temperature is 25 DEG C,
Lower removing 80min is stirred under 100rpm/min revolving speed.
7. hydroxymethylfurfural removal methods in a kind of honey according to claim 1, which is characterized in that use 150-200
Mesh net filtration.
8. hydroxymethylfurfural removal methods in a kind of honey according to claim 1, which is characterized in that will be obtained after filtering
Honey be concentrated after 45-50 DEG C of preheating 20min.
9. hydroxymethylfurfural removal methods in a kind of honey according to claim 1, which is characterized in that thickening temperature is
45-55 DEG C, vacuum degree 0.05-0.07Mpa.
10. hydroxymethylfurfural removal methods in a kind of honey according to claim 1, which is characterized in that be concentrated into honey
Moisture content is 18-20%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811314385.3A CN109259052A (en) | 2018-11-06 | 2018-11-06 | Hydroxymethylfurfural removal methods in a kind of honey |
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| CN201811314385.3A CN109259052A (en) | 2018-11-06 | 2018-11-06 | Hydroxymethylfurfural removal methods in a kind of honey |
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| CN201811314385.3A Pending CN109259052A (en) | 2018-11-06 | 2018-11-06 | Hydroxymethylfurfural removal methods in a kind of honey |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113826808A (en) * | 2021-09-27 | 2021-12-24 | 佛山科学技术学院 | Method for removing 5-hydroxymethylfurfural and application of method in food processing |
| CN115316573A (en) * | 2022-08-23 | 2022-11-11 | 西安冰峰饮料股份有限公司 | Gas-containing plum syrup flavored beverage and preparation method thereof |
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| CN105795312A (en) * | 2016-03-17 | 2016-07-27 | 哈尔滨商业大学 | Method of removing hydroxymethyl furfural in honey |
| CN106689980A (en) * | 2016-11-30 | 2017-05-24 | 西北大学 | Method for removing pesticide and antibiotic residues from honey |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113826808A (en) * | 2021-09-27 | 2021-12-24 | 佛山科学技术学院 | Method for removing 5-hydroxymethylfurfural and application of method in food processing |
| CN113826808B (en) * | 2021-09-27 | 2024-02-06 | 佛山科学技术学院 | Method for removing 5-hydroxymethylfurfural and application of method in food processing |
| CN115316573A (en) * | 2022-08-23 | 2022-11-11 | 西安冰峰饮料股份有限公司 | Gas-containing plum syrup flavored beverage and preparation method thereof |
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Application publication date: 20190125 |