CN103408610B - The method of arbutin is extracted from leaf of pear tree - Google Patents
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Abstract
From leaf of pear tree, extract the method for arbutin, from leaf of pear tree, extract the leaf juice containing arbutin, obtain arbutin through concentrated, purification and recrystallization. Step 1, after leaf of pear tree oven dry, pulverizing, with methyl alcohol dipping, filters, by filtrate simmer down to medicinal extract; Step 2, gets resin dress post, by step 1 gained medicinal extract water dissolution, filters, and in filtrate, arbutin content is 2mg/mL, column purification on filtrate, obtains arbutin crude extract; Step 3, gets ENV filler dress post, and after being dissolved by step 2 gained arbutin crude extract, upper post purifies again, obtains arbutin crude product; Step 4, carries out crystallization to step 3 gained arbutin crude product, obtains arbutin. Step 5, carries out recrystallization to step 4 gained arbutin. The present invention's raw material used is the waste material after economical fruit tree is gathered, abundant raw material source, is convenient to obtain, and cost is low. Extracting method technique of the present invention is simple, easy to operate, and gained arbutin purity height.
Description
Technical field
The invention belongs to arbutin extracting method technical field, it relates to a kind of method extracting arbutin from leaf of pear tree.
Background technology
Arbutin (arbutin) is a kind of natural active matter, can effectively suppress the biological tyrosinase activity in skin, block the formation of melanochrome, accelerate decomposition and the excretion of melanochrome, thus reduce Skin pigmentation, dispelling stain and freckle are the main active substances in current skin-lightening cosmetic both at home and abroad. In recent years, along with the development of domestic cosmetic industry, for complying with the trend of skin protection cosmetics " back to nature ", " the green whitening " of natural active matter is also day by day prevailing, and arbutin is as nontoxic, the obvious natural active matter of whitening effect, market demand expands day by day.
At present, the raw material extracting arbutin is mainly fruit tree, and such as blue berry, its operational path is complicated, and due to fruit source limited, the cost therefore causing extracting arbutin is very high.
The concentration of involved reagent is volumetric concentration herein, and per-cent involved by all the other all refers to weight percent.
Summary of the invention
It is an object of the invention to provide a kind of method extracting arbutin from leaf of pear tree, solve the complex process that prior art exists, the problem that cost is high.
The technical scheme of the present invention, extracts the method for arbutin from leaf of pear tree, extracts the leaf juice containing arbutin from leaf of pear tree, obtains arbutin through concentrated, purification and recrystallization.
The feature of the present invention is also, specifically comprises the following steps:
Step 1, after leaf of pear tree oven dry, pulverizing, with methyl alcohol dipping, filters, by filtrate simmer down to medicinal extract;
Step 2, gets resin dress post, by step 1 gained medicinal extract water dissolution, filters, and in filtrate, arbutin content is 2mg/mL, column purification on filtrate, obtains arbutin crude extract;
Step 3, gets ENV filler dress post, and after being dissolved by step 2 gained arbutin crude extract, upper post purifies again, obtains arbutin crude product;
Step 4, carries out crystallization to step 3 gained arbutin crude product, obtains arbutin.
Step 5, carries out recrystallization to step 4 gained arbutin.
In step 1, yield of extract is 7%��10%, arbutin content about 6%��10% in medicinal extract.
Resin in step 2 is LSA-900B resin; Column purification on filtrate, with different concns methyl alcohol drip washing, maintenance flow velocity 0.4��0.5 times of column volume/hour, obtaining scavenging solution, scavenging solution, after concentrated, obtains the arbutin crude extract of solid state, wherein arbutin content 30%��34%.
In step 3, on filtrate after column purification, collect effluent liquid, with the water wash of 2 times of column volumes, in loading effluent liquid, arbutin content is lower than 0.005mg/mL, abandons effluent liquid, then by 10% methanol-eluted fractions of 10 times of column volumes, collecting the elutriant of 1 times of column volume, whole process flow velocity keeps 2��3mL/min every time; In first three wash-out gained elutriant, arbutin content is the highest, is respectively 3.0mg/mL, 4.8mg/mL, 1.6mg/mL, collects the elutriant of first three wash-out gained, concentrated, obtains solid state arbutin crude product, and its arbutin content is greater than 82%.
In step 4, arbutin crude product is added ethyl acetate, reflux 0.5��1h, filtered while hot, hold over night, precipitate out white powder solid, filter, dry, obtain white powder solid, in this pulverulent solids, arbutin content is greater than 95%.
In step 5, recrystallization can repeat repeatedly, and arbutin purity reaches more than 99%.
The present invention has following useful effect:
1, the raw material that the present invention is used is the waste material after economical fruit tree is gathered, abundant raw material source, is convenient to obtain, and cost is low.
2, extracting method technique of the present invention is simple, easy to operate, and gained arbutin purity height.
Accompanying drawing explanation
Fig. 1 is the infrared spectrogram of the arbutin that the method adopting the present invention to extract arbutin from leaf of pear tree obtains.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is further detailed explanation.
From leaf of pear tree, extract the method for arbutin, from leaf of pear tree, extract the leaf juice containing arbutin, obtain arbutin through concentrated, purification and recrystallization. Specifically comprise the following steps:
Step 1, after leaf of pear tree oven dry, pulverizing, with methyl alcohol dipping, filters, by filtrate simmer down to medicinal extract; Yield of extract is 7%��10%, arbutin content about 6%��10% in medicinal extract. Yield of extract and medicinal extract account for the percentage composition of the quality of leaf of pear tree used.
Step 2, gets resin dress post, by step 1 gained medicinal extract water dissolution, filters, and in filtrate, arbutin content is 2mg/mL, column purification on filtrate, obtains arbutin crude extract; Resin is LSA-900B resin; Column purification on filtrate, with different concns methyl alcohol drip washing, maintenance flow velocity 0.4��0.5 times of column volume/hour, obtaining scavenging solution, scavenging solution, after concentrated, obtains the arbutin crude extract of solid state, wherein arbutin content 30%��34%.
Step 3, gets ENV filler dress post, and after being dissolved by step 2 gained arbutin crude extract, upper post purifies again, obtains arbutin crude product; On filtrate after column purification, collect effluent liquid, with the water wash of 2 times of column volumes, in loading effluent liquid, arbutin content is lower than 0.005mg/mL, abandons effluent liquid, then by 10% methanol-eluted fractions of 10 times of column volumes, collecting the elutriant of 1 times of column volume, whole process flow velocity keeps 2��3mL/min every time; In first three wash-out gained elutriant, arbutin content is the highest, is respectively 3.0mg/mL, 4.8mg/mL, 1.6mg/mL, collects the elutriant of first three wash-out, concentrated, obtains solid state arbutin crude product, and its arbutin content is greater than 82%.
Step 4, carries out crystallization to step 3 gained arbutin crude product, obtains arbutin. It is specially and arbutin crude product is added ethyl acetate, reflux 0.5��1h, filtered while hot, hold over night, precipitate out white powder solid, filter, dry, obtain white powder solid, in this pulverulent solids, arbutin content is greater than 95%.
Step 5, carries out recrystallization to step 4 gained arbutin. Can repeating repeatedly recrystallization, arbutin purity reaches more than 99%.
Embodiment 1
Step 1, extracting containing the extract of arbutin from leaf of pear tree, its concrete steps are:
Step 1a: win leaf of pear tree sample, dries in 40 DEG C of baking ovens, pulverizes.
Step 1b: claim the leaf of pear tree sample 400g after pulverizing, add the pure methyl alcohol of 4L, under normal temperature, flood 3, filters, filtrate is carried out rotary evaporation, and concentrated removal methyl alcohol, obtains the medicinal extract containing arbutin, yield of extract 7%, arbutin content about 6% in medicinal extract.
Step 2, with LSA-900B resin Preparation arbutin crude extract:
Step 2a: the screening of resin:
Static Adsorption test is adopted to be studied by the adsorption effect of 4 kinds of different model resins, the 4 kinds of resins selected are LSA-900B, LSA-900C, LX-200 and LX-400, accurately take each model resin 1g, add in tool plug Erlenmeyer flask on request after pre-treatment, get 0.1g leaf of pear tree and extract medicinal extract, add 40mL water dissolution, often kind of resin adds the 10mL medicinal extract aqueous solution, Static Adsorption 1h under room temperature, get the supernatant liquid of often kind of resin, (measuring method is shown in document: Zhao Jie to measure arbutin content by HPLC method, He Qiang, Yao Binghua, Deng, the confirmation of effective constituent arbutin and HPLC detection in leaf of pear tree, Chinese Journal of Modern Applied Pharmacy, 2011), with arbutin comparision contents in initial soln, calculate various resin to the Static Adsorption rate of arbutin, result is as shown in table 1, from table 1, the Static Adsorption rate of LSA-900B type resin is the highest, so selecting LSA-900B type resin to carry out rough purification.
The different model resin of table 1 is to arbutin Static Adsorption rate
| Resin model | LSA-900B | LSA-900C | LX-200 | LX-400 |
| Adsorption rate (%) | 62.8 | 9.4 | 20.8 | 8.5 |
Step 2b: obtain arbutin crude extract by LSA-900B type resin isolation:
Get LSA-900B type resin 300g and fill post (column volume is about 450mL), activate on request, get 8g leaf of pear tree and extract medicinal extract, use 240mL water dissolution, filter, in filtrate, arbutin content is 2mg/mL, column purification on filtrate, maintenance flow velocity 0.4 times of column volume/hour, collect loading effluent liquid (numbering 0), again successively with the distilled water (numbering 1) of 1 times of column volume, 10% methyl alcohol (numbering 2) of 1 times of column volume, 20% methyl alcohol (numbering 3) of 1 times of column volume, 30% methyl alcohol (numbering 4) of 1 times of column volume, 1 times of pure methyl alcohol of column volume (numbering 5), 1 times of pure methyl alcohol of column volume (numbering 6), collect the leacheate in each stage, arbutin content in detection leacheate, result is as shown in table 2.
Arbutin content in the different elutriant of table 2
As can be seen from Table 2, No. 3 elutriants (20% methyl alcohol) start have more arbutin to be eluted, No. 5 elutriants (pure methyl alcohol) are substantially by complete for the arbutin wash-out that adsorbs on resin, so, according to the experimental result in table 2, it is determined that first with the water wash of 1 times of column volume after loading, again with 10% methyl alcohol drip washing of 1 times of column volume, abandoning leacheate, elutriant is through follow-up optimization, and the pure methanol-based of 1.4 times of column volumes originally can be complete by the arbutin wash-out adsorbed on resin. Meoh eluate is concentrated to dry, obtain arbutin crude extract and be about 1.2g, wherein arbutin content about 30%.
Step 3, with ENV polymerization filling purify arbutin crude extract.
Through a large amount of pre-experiment, ENV adsorption stuffing is selected to be purified further by arbutin crude extract. ENV filler is a kind of polystyrene-divinylbenzene copolymer material, arbutin in the aqueous solution there is good adsorption, and the big polar materials such as carbohydrate are not adsorbed substantially, and the arbutin being adsorbed on ENV is easily eluted by 10% methanol solution, other impurity being adsorbed on ENV filler need the methyl alcohol of higher concentration just can elute, thus reach good decontamination effect improving.
Specific experiment step: get 20gENV filler dress post (column volume is about 56mL), successively with the methyl alcohol of 1 times of column volume, the water activation pillar of 1 times of column volume, get the arbutin crude extract that 1.2g obtains through LSA-900B rough purification, use 50mL water dissolution, filter, filtrate crosses column purification, collect effluent liquid, with the water wash of 2 times of column volumes, in loading effluent liquid, arbutin content is all lower than 0.005mg/mL, abandon effluent liquid, again by 10% methanol-eluted fractions of 10 times of column volumes, collect the elutriant (being numbered 1��10) of 1 times of column volume every time, whole process flow velocity keeps 2mL/min, in first three wash-out gained elutriant, arbutin content is the highest, it is respectively 3.0mg/mL, 4.8mg/mL, 1.6mg/mL, in 4th wash-out gained elutriant, arbutin content is lower, it is only 0.06mg/mL, from the 5th elutriant, elutriant is mainly other composition. so according to detection case, collecting first three gained elutriant, concentrated, obtain the higher arbutin crude product of about 0.3g purity (for solid state), after testing, arbutin content is about 82%.
Step 4, recrystallization obtain arbutin monomer
Get the arbutin crude product that about 0.3g is purer, add 10mL ethyl acetate, reflux 0.5h, filtered while hot, hold over night, precipitates out white powder solid, filter, drying, obtains white powder solid and is about 0.2g, and in this pulverulent solids, arbutin content is about 95%, if needing to prepare the higher arbutin of purity, can repeating recrystallization, recrystallization 3 times, arbutin purity can reach more than 99%.
The confirmation of step 5, arbutin
To the arbutin that separation obtains, high performance liquid chromatography, mass spectrum, infrared spectra and nucleus magnetic resonance H spectrum and C spectrum is adopted to confirm, the infrared spectra being wherein separated the arbutin obtained is as shown in Figure 1, consistent with the standard infrared spectrogram of arbutin in standard spectrum storehouse.
Shaanxi Province is the big province of Production of fruit, wherein nearly 1,000,000 mu of the cultivated area of pear tree, the by product that leaf of pear tree is planted as pear tree, originates very abundant, and cost is low.
Embodiment 2
Step 1, extracting containing the extract of arbutin from leaf of pear tree, its concrete steps are:
Step 1a: win leaf of pear tree sample, dries in 50 DEG C of baking ovens, pulverizes.
Step 1b: claim the leaf of pear tree sample 450g after pulverizing, add the pure methyl alcohol of 4.5L, under normal temperature, flood 4, filters, filtrate is carried out rotary evaporation, and concentrated removal methyl alcohol, obtains the medicinal extract containing arbutin, yield of extract 8%, arbutin content about 7% in medicinal extract.
Step 2, with LSA-900B resin Preparation arbutin crude extract:
Step 2a: the screening of resin:
Static Adsorption test is adopted to be studied by the adsorption effect of 4 kinds of different model resins, the 4 kinds of resins selected are LSA-900B, LSA-900C, LX-200 and LX-400, accurately take each model resin 3g, add in tool plug Erlenmeyer flask on request after pre-treatment, get 0.3g leaf of pear tree and extract medicinal extract, add 120mL water dissolution, often kind of resin adds the 30mL medicinal extract aqueous solution, Static Adsorption 1h under room temperature, get the supernatant liquid of often kind of resin, (measuring method is shown in document: Zhao Jie to measure arbutin content by HPLC method, He Qiang, Yao Binghua, Deng, the confirmation of effective constituent arbutin and HPLC detection in leaf of pear tree, Chinese Journal of Modern Applied Pharmacy, 2011), with arbutin comparision contents in initial soln, calculate various resin to the Static Adsorption rate of arbutin, result is as shown in table 3, from table 3, the Static Adsorption rate of LSA-900B type resin is the highest, so selecting LSA-900B type resin to carry out rough purification.
The different model resin of table 3 is to arbutin Static Adsorption rate
| Resin model | LSA-900B | LSA-900C | LX-200 | LX-400 |
| Adsorption rate (%) | 60.6 | 8.3 | 18.1 | 7.4 |
Step 2b: obtain arbutin crude extract by LSA-900B type resin isolation:
Get LSA-900B type resin 350g and fill post (column volume is about 530mL), activate on request, get 9g leaf of pear tree and extract medicinal extract, use 320mL water dissolution, filter, in filtrate, arbutin content is 2mg/mL, column purification on filtrate, maintenance flow velocity 0.4 times of column volume/hour, collect loading effluent liquid (numbering 0), again successively with the distilled water (numbering 1) of 1 times of column volume, 10% methyl alcohol (numbering 2) of 1 times of column volume, 20% methyl alcohol (numbering 3) of 1 times of column volume, 30% methyl alcohol (numbering 4) of 1 times of column volume, 1 times of pure methyl alcohol of column volume (numbering 5), 1 times of pure methyl alcohol of column volume (numbering 6), collect the leacheate in each stage, arbutin content in detection leacheate, result is as shown in table 4.
Arbutin content in the different elutriant of table 4
As can be seen from Table 4, No. 3 elutriants (20% methyl alcohol) start have more arbutin to be eluted, No. 5 elutriants (pure methyl alcohol) are substantially by complete for the arbutin wash-out that adsorbs on resin, so, according to the experimental result in table 2, it is determined that first with the water wash of 1 times of column volume after loading, again with 10%��15% methyl alcohol drip washing of 1 times of column volume, abandoning leacheate, elutriant is through follow-up optimization, and the pure methanol-based of 1.4��1.5 times of column volumes originally can be complete by the arbutin wash-out adsorbed on resin. Meoh eluate is concentrated to dry, obtain arbutin crude extract and be about 2.1g, wherein arbutin content about 30%.
Step 3, with ENV polymerization filling purify arbutin crude extract.
Through a large amount of pre-experiment, ENV adsorption stuffing is selected to be purified further by arbutin crude extract. ENV filler is a kind of polystyrene-divinylbenzene copolymer material, arbutin in the aqueous solution there is good adsorption, and the big polar materials such as carbohydrate are not adsorbed substantially, and the arbutin being adsorbed on ENV is easily eluted by 10% methanol solution, other impurity being adsorbed on ENV filler need the methyl alcohol of higher concentration just can elute, thus reach good decontamination effect improving.
Specific experiment step: get 22gENV filler dress post (column volume is about 60mL), successively with the methyl alcohol of 1��1.5 times of column volume, the water activation pillar of 1��2 times of column volume, get the arbutin crude extract that 2.1g obtains through LSA-900B rough purification, use 55mL water dissolution, filter, filtrate crosses column purification, collect effluent liquid, with the water wash of 2 times of column volumes, in loading effluent liquid, arbutin content is all lower than 0.005mg/mL, abandon effluent liquid, again by 10% methanol-eluted fractions of 10 times of column volumes, collect the elutriant (being numbered 1��10) of 1 times of column volume every time, whole process flow velocity keeps 3mL/min, in first three gained elutriant, arbutin content is the highest, it is respectively 2.8mg/mL, 4.5mg/mL, 1.7mg/mL, in 4th gained elutriant, arbutin content is lower, it is only 0.05mg/mL, from the 5th gained elutriant, elutriant is mainly other composition. so according to detection case, collecting the elutriant of first three wash-out gained, concentrated, obtain the higher arbutin crude product of about 0.44g purity (for solid state), after testing, arbutin content is about 85%.
Step 4, recrystallization obtain arbutin monomer
Get the arbutin crude product that about 0.44g is purer, add 30mL ethyl acetate, reflux 1h, filtered while hot, hold over night, precipitates out white powder solid, filter, drying, obtains white powder solid and is about 0.3g, and in this pulverulent solids, arbutin content is greater than 95%, if needing to prepare the higher arbutin of purity, can repeating recrystallization, recrystallization 3 times, arbutin purity can reach more than 99%.
The confirmation of step 5, arbutin
To the arbutin that separation obtains, high performance liquid chromatography, mass spectrum, infrared spectra and nucleus magnetic resonance H spectrum and C spectrum is adopted to confirm, all can be corresponding with standard spectrum storehouse.
Shaanxi Province is the big province of Production of fruit, wherein nearly 1,000,000 mu of the cultivated area of pear tree, the by product that leaf of pear tree is planted as pear tree, originates very abundant, and cost is low.
Embodiment 3
Step 1, extracting containing the extract of arbutin from leaf of pear tree, its concrete steps are:
Step 1a: win leaf of pear tree sample, dries in 60 DEG C of baking ovens, pulverizes.
Step 1b: claim the leaf of pear tree sample 500g after pulverizing, add the pure methyl alcohol of 5L, under normal temperature, flood 5, filters, filtrate is carried out rotary evaporation, and concentrated removal methyl alcohol, obtains the medicinal extract containing arbutin, yield of extract 10%, arbutin content about 10% in medicinal extract.
Step 2, with LSA-900B resin Preparation arbutin crude extract:
Step 2a: the screening of resin:
Static Adsorption test is adopted to be studied by the adsorption effect of 4 kinds of different model resins, the 4 kinds of resins selected are LSA-900B, LSA-900C, LX-200 and LX-400, accurately take each model resin 5g, add in tool plug Erlenmeyer flask on request after pre-treatment, get 0.5g leaf of pear tree and extract medicinal extract, add 200mL water dissolution, often kind of resin adds the 50mL medicinal extract aqueous solution, Static Adsorption 1h under room temperature, get the supernatant liquid of often kind of resin, (measuring method is shown in document: Zhao Jie to measure arbutin content by HPLC method, He Qiang, Yao Binghua, Deng, the confirmation of effective constituent arbutin and HPLC detection in leaf of pear tree, Chinese Journal of Modern Applied Pharmacy, 2011), with arbutin comparision contents in initial soln, calculate various resin to the Static Adsorption rate of arbutin, result is as shown in table 5, from table 5, the Static Adsorption rate of LSA-900B type resin is the highest, so selecting LSA-900B type resin to carry out rough purification.
The different model resin of table 5 is to arbutin Static Adsorption rate
| Resin model | LSA-900B | LSA-900C | LX-200 | LX-400 |
| Adsorption rate (%) | 69.7 | 10.2 | 21.1 | 9.3 |
Step 2b: obtain arbutin crude extract by LSA-900B type resin isolation:
Get LSA-900B type resin 400g and fill post (column volume is about 600mL), activate on request, get 10g leaf of pear tree and extract medicinal extract, use 500mL water dissolution, filter, in filtrate, arbutin content is 2mg/mL, column purification on filtrate, maintenance flow velocity 0.4 times of column volume/hour, collect loading effluent liquid (numbering 0), again successively with the distilled water (numbering 1) of 1 times of column volume, 10% methyl alcohol (numbering 2) of 1 times of column volume, 20% methyl alcohol (numbering 3) of 1 times of column volume, 30% methyl alcohol (numbering 4) of 1 times of column volume, 1 times of pure methyl alcohol of column volume (numbering 5), 1 times of pure methyl alcohol of column volume (numbering 6), collect the leacheate in each stage, arbutin content in detection leacheate, result is as shown in table 6.
Arbutin content in the different elutriant of table 6
As can be seen from Table 2, No. 3 elutriants (20% methyl alcohol) start have more arbutin to be eluted, No. 5 elutriants (pure methyl alcohol) are substantially by complete for the arbutin wash-out that adsorbs on resin, so, according to the experimental result in table 2, it is determined that first with the water wash of 1 times of column volume after loading, again with 10%��15% methyl alcohol drip washing of 1 times of column volume, abandoning leacheate, elutriant is through follow-up optimization, and the pure methanol-based of 1.4��1.5 times of column volumes originally can be complete by the arbutin wash-out adsorbed on resin. Meoh eluate is concentrated to dry, obtain arbutin crude extract and be about 3.0g, wherein arbutin content about 34%.
Step 3, with ENV polymerization filling purify arbutin crude extract.
Through a large amount of pre-experiment, ENV adsorption stuffing is selected to be purified further by arbutin crude extract. ENV filler is a kind of polystyrene-divinylbenzene copolymer material, arbutin in the aqueous solution there is good adsorption, and the big polar materials such as carbohydrate are not adsorbed substantially, and the arbutin being adsorbed on ENV is easily eluted by 10% methanol solution, other impurity being adsorbed on ENV filler need the methyl alcohol of higher concentration just can elute, thus reach good decontamination effect improving.
Specific experiment step: get 24gENV filler dress post (column volume is about 64mL), successively with the methyl alcohol of 1��1.5 times of column volume, the water activation pillar of 1��2 times of column volume, get the arbutin crude extract that 3.0g obtains through LSA-900B rough purification, use 60mL water dissolution, filter, filtrate crosses column purification, collect effluent liquid, with the water wash of 2 times of column volumes, in loading effluent liquid, arbutin content is all lower than 0.005mg/mL, abandon effluent liquid, again by 10% methanol-eluted fractions of 10 times of column volumes, collect the elutriant (being numbered 1��10) of 1 times of column volume every time, whole process flow velocity keeps 2mL/min, in the elutriant of first three wash-out gained, arbutin content is the highest, it is respectively 2.9mg/mL, 4.9mg/mL, 1.8mg/mL, in the elutriant of the 4th wash-out gained, arbutin content is lower, it is only 0.05mg/mL, from the 5th gained elutriant, elutriant is mainly other composition. so according to detection case, collecting first three gained elutriant, concentrated, obtain the higher arbutin crude product of about 0.84g purity (for solid state), after testing, arbutin content is about 85%.
Step 4, recrystallization obtain arbutin monomer
Get the arbutin crude product that about 0.84g is purer, add 50mL ethyl acetate, reflux 1h, filtered while hot, hold over night, precipitates out white powder solid, filter, drying, obtains white powder solid and is about 0.4g, and in this pulverulent solids, arbutin content is greater than 95%, if needing to prepare the higher arbutin of purity, can repeating recrystallization, recrystallization 3 times, arbutin purity can reach more than 99%.
The confirmation of step 5, arbutin
To the arbutin that separation obtains, high performance liquid chromatography, mass spectrum, infrared spectra and nucleus magnetic resonance H spectrum and C spectrum is adopted to confirm, all can be corresponding with standard spectrum storehouse.
Shaanxi Province is the big province of Production of fruit, wherein nearly 1,000,000 mu of the cultivated area of pear tree, the by product that leaf of pear tree is planted as pear tree, originates very abundant, and cost is low.
Claims (3)
1. from leaf of pear tree, extract the method for arbutin, it is characterised in that, from leaf of pear tree, extract the leaf juice containing arbutin, obtain arbutin through concentrated, purification and recrystallization, specifically comprise the following steps:
Step 1, after leaf of pear tree oven dry, pulverizing, with methyl alcohol dipping, filters, by filtrate simmer down to medicinal extract;
Step 2, get LSA-900B resin dress post, by step 1 gained medicinal extract water dissolution, filtering, in filtrate, arbutin content is 2mg/mL, column purification on filtrate, with different concns methyl alcohol drip washing, maintenance flow velocity 0.4��0.5 times of column volume/hour, obtain scavenging solution, concentrate to obtain arbutin crude extract, wherein arbutin content 30%��34%;
Step 3, gets ENV filler dress post, is purified by post on step 2 gained arbutin crude extract again, and with the water wash of 2 times of column volumes, in loading effluent liquid, arbutin content is all lower than 0.005mg/mL, abandons effluent liquid; Again by 10% methanol-eluted fractions of 10 times of column volumes, collecting the elutriant of 1 times of column volume, whole process flow velocity keeps 2��3mL/min every time; In first three wash-out gained elutriant, arbutin content is the highest, is respectively 3.0mg/mL, 4.8mg/mL, 1.6mg/mL, collects the elutriant of first three wash-out gained, concentrated, obtains solid state arbutin crude product, and its arbutin content is greater than 82%;
Step 4, step 3 gained arbutin crude product is carried out crystallization, and arbutin crude product adds ethyl acetate, reflux 0.5��1h, filtered while hot, hold over night, precipitates out white powder solid, filters, dry, obtaining white powder solid, be arbutin, in this pulverulent solids, arbutin content is greater than 95%.
2. from leaf of pear tree, extract the method for arbutin as claimed in claim 1, it is characterised in that: also comprising step 5, step 5 is for carry out recrystallization to step 4 gained arbutin.
3. from leaf of pear tree, extract the method for arbutin as claimed in claim 1 or 2, it is characterised in that, in step 1, yield of extract 7%��10%; Arbutin content 6%��10% in medicinal extract.
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| CN107163093A (en) * | 2017-06-16 | 2017-09-15 | 江苏天晟药业股份有限公司 | A kind of preparation method of ursin |
| CN107722080A (en) * | 2017-11-08 | 2018-02-23 | 长沙爱扬医药科技有限公司 | A kind of method that ursin is extracted in the leaf from purple bergenia herb |
| CN108558964B (en) * | 2018-04-18 | 2020-06-16 | 山东众山生物科技有限公司 | Purification method of α -arbutin |
| CN110684061B (en) * | 2018-07-05 | 2021-09-03 | 大湾汉唯(广州)中药研究开发有限公司 | Extract containing alpha-arbutin and preparation method thereof |
| CN110551160B (en) * | 2019-09-29 | 2023-04-28 | 无锡知妍生物科技有限公司 | Extraction and purification method of arbutin and application of arbutin in freckle removing and whitening |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006111581A (en) * | 2004-10-15 | 2006-04-27 | Nitto Best Kk | Method for separating and purifying arbutin |
| KR20110011454A (en) * | 2009-07-28 | 2011-02-08 | 이병두 | Extraction and purification of arbutin from asian pear peel by solvent extraction system |
| CN102093442A (en) * | 2011-01-13 | 2011-06-15 | 赵玉红 | Method for separating and purifying arbutin from blueberry |
-
2013
- 2013-07-26 CN CN201310320988.5A patent/CN103408610B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006111581A (en) * | 2004-10-15 | 2006-04-27 | Nitto Best Kk | Method for separating and purifying arbutin |
| KR20110011454A (en) * | 2009-07-28 | 2011-02-08 | 이병두 | Extraction and purification of arbutin from asian pear peel by solvent extraction system |
| CN102093442A (en) * | 2011-01-13 | 2011-06-15 | 赵玉红 | Method for separating and purifying arbutin from blueberry |
Non-Patent Citations (5)
| Title |
|---|
| "发酵法生产α-熊果苷及其分离纯化";刘春巧;《Engineering Science and Technology I》;20110131(第1期);第4章 * |
| "固相萃取-超高效液相色谱-电喷雾串联质谱法检测梨树叶中熊果苷";赵洁等;《分析试验室》;20110228;第30卷(第2期);第58页, 第1.2.2部分 * |
| "大孔树脂对库尔勒香梨果汁脱色的研究";范爱军等;《现代食品科技》;20120315;第28卷(第3期);第285-288页 * |
| "梨树叶中有效成分熊果苷的确证及HPLC检测";赵洁等;《中国现代应用药学》;20111231;第28卷(第12期);第1130页, 第2.1部分 * |
| "熊果苷分离纯化研究";贺绍祥等;《现代食品科技》;20071015;第23卷(第10期);第66页第2.2部分 * |
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