CN101912480A - Method for preparing procyanidin extract of lycium ruthenicum murr - Google Patents
Method for preparing procyanidin extract of lycium ruthenicum murr Download PDFInfo
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- CN101912480A CN101912480A CN2010102413513A CN201010241351A CN101912480A CN 101912480 A CN101912480 A CN 101912480A CN 2010102413513 A CN2010102413513 A CN 2010102413513A CN 201010241351 A CN201010241351 A CN 201010241351A CN 101912480 A CN101912480 A CN 101912480A
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- procyanidin
- hydrochloric acid
- lycium ruthenicum
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- ruthenicum murr
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- CWEZAWNPTYBADX-UHFFFAOYSA-N Procyanidin Natural products OC1C(OC2C(O)C(Oc3c2c(O)cc(O)c3C4C(O)C(Oc5cc(O)cc(O)c45)c6ccc(O)c(O)c6)c7ccc(O)c(O)c7)c8c(O)cc(O)cc8OC1c9ccc(O)c(O)c9 CWEZAWNPTYBADX-UHFFFAOYSA-N 0.000 title claims abstract description 109
- 229920002414 procyanidin Polymers 0.000 title claims abstract description 109
- XFZJEEAOWLFHDH-UHFFFAOYSA-N (2R,2'R,3R,3'R,4R)-3,3',4',5,7-Pentahydroxyflavan(48)-3,3',4',5,7-pentahydroxyflavan Natural products C=12OC(C=3C=C(O)C(O)=CC=3)C(O)CC2=C(O)C=C(O)C=1C(C1=C(O)C=C(O)C=C1O1)C(O)C1C1=CC=C(O)C(O)=C1 XFZJEEAOWLFHDH-UHFFFAOYSA-N 0.000 title claims abstract description 108
- MOJZMWJRUKIQGL-FWCKPOPSSA-N Procyanidin C2 Natural products O[C@@H]1[C@@H](c2cc(O)c(O)cc2)Oc2c([C@H]3[C@H](O)[C@@H](c4cc(O)c(O)cc4)Oc4c3c(O)cc(O)c4)c(O)cc(O)c2[C@@H]1c1c(O)cc(O)c2c1O[C@@H]([C@H](O)C2)c1cc(O)c(O)cc1 MOJZMWJRUKIQGL-FWCKPOPSSA-N 0.000 title claims abstract description 108
- HGVVOUNEGQIPMS-UHFFFAOYSA-N procyanidin Chemical compound O1C2=CC(O)=CC(O)=C2C(O)C(O)C1(C=1C=C(O)C(O)=CC=1)OC1CC2=C(O)C=C(O)C=C2OC1C1=CC=C(O)C(O)=C1 HGVVOUNEGQIPMS-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 239000000284 extract Substances 0.000 title claims abstract description 54
- 241000169546 Lycium ruthenicum Species 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 56
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000012528 membrane Substances 0.000 claims abstract description 30
- 239000003480 eluent Substances 0.000 claims abstract description 24
- 239000011347 resin Substances 0.000 claims abstract description 24
- 229920005989 resin Polymers 0.000 claims abstract description 24
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
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- 238000002360 preparation method Methods 0.000 claims description 18
- 239000012141 concentrate Substances 0.000 claims description 17
- 238000001179 sorption measurement Methods 0.000 claims description 11
- 239000000919 ceramic Substances 0.000 claims description 10
- 230000006837 decompression Effects 0.000 claims description 9
- 235000015203 fruit juice Nutrition 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 3
- 235000013824 polyphenols Nutrition 0.000 abstract description 14
- 150000008442 polyphenolic compounds Chemical class 0.000 abstract description 13
- 235000010208 anthocyanin Nutrition 0.000 abstract description 11
- 239000004410 anthocyanin Substances 0.000 abstract description 11
- 229930002877 anthocyanin Natural products 0.000 abstract description 11
- 150000004636 anthocyanins Chemical class 0.000 abstract description 11
- 238000000605 extraction Methods 0.000 abstract description 8
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- 102000004169 proteins and genes Human genes 0.000 description 9
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- 241000219095 Vitis Species 0.000 description 7
- 238000001471 micro-filtration Methods 0.000 description 7
- 229920001864 tannin Polymers 0.000 description 7
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- FGRBYDKOBBBPOI-UHFFFAOYSA-N 10,10-dioxo-2-[4-(N-phenylanilino)phenyl]thioxanthen-9-one Chemical compound O=C1c2ccccc2S(=O)(=O)c2ccc(cc12)-c1ccc(cc1)N(c1ccccc1)c1ccccc1 FGRBYDKOBBBPOI-UHFFFAOYSA-N 0.000 description 1
- TVEXGJYMHHTVKP-UHFFFAOYSA-N 6-oxabicyclo[3.2.1]oct-3-en-7-one Chemical compound C1C2C(=O)OC1C=CC2 TVEXGJYMHHTVKP-UHFFFAOYSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
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- 241001106041 Lycium Species 0.000 description 1
- 208000019255 Menstrual disease Diseases 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- 230000002019 anti-mutation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 235000021028 berry Nutrition 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
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- 235000015961 tonic Nutrition 0.000 description 1
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- 229960000716 tonics Drugs 0.000 description 1
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a method for preparing a procyanidin extract of lycium ruthenicum murr. The method comprises the following steps of: separating lycium ruthenicum murr juice or lycium ruthenicum murr concentrated solution serving as raw materials by using nonpolar macroporous absorption resins, eluting the obtained product with deionized water to make the obtained product sugar-free, and eluting the sugar-free product again with the solution of hydrochloric acid and ethanol to obtain procyanidin-containing eluent; then concentrating the procyanidin-containing eluent under vacuum and reduced pressure or by using nanofiltration membrane to obtain procyanidin concentrated solution; and finally, performing spray drying or freeze drying on the concentrated solution to obtain the procyanidin extract of the lycium ruthenicum murr, which contains more than or equal to 50 percent of procyanidins, more than or equal to 50 percent of total polyphenols and more than or equal to 1 percent of anthocyanins. By combining membrane separation technology with column chromatography separation technology, the method reduces production cost, time for extraction and separation and energy consumption in the process; moreover, the obtained product has high purity and stable performance and can be applied to natural pigment food additives and raw materials of medicaments and health products having antioxidant effects.
Description
Technical field
The present invention relates to a kind of preparation method of procyanidin extract, relate in particular to a kind of preparation method of procyanidin extract of lycium ruthenicum murr.
Background technology
Procyanidin is the general name of an extensive big class natural polyphenol chemical compound that exists in the plant, has pharmacologically actives such as the free radical of removing, antioxidation, anti-mutation, enzyme inhibition and treatment disease of capillaries.At present, mainly extract procyanidin from Semen Vitis viniferae, generally about 75%, international first-class its procyanidin content of Semen Vitis viniferae extract product can reach 85% to the Semen Vitis viniferae extract procyanidin content of domestic production.Total polyphenols in the Semen Vitis viniferae extract is generally between 75～95%, China's Semen Vitis viniferae extract total polyphenols mostly is greatly about 85%, and grape pip procyanidin extract antioxidation index ORAC (oxygen radicalabsorbance capacity) is worth about 5000 (μ molTE/g).Domestic individual manufacturer Semen Vitis viniferae extract procyanidin content 〉=90%, ORAC are 18782 μ molTE/g.
Black Fructus Lycii (Lycium ruthenicum Murr.) is a Solanaceae Lycium plant, is the common wild bushes in NORTHWEST CHINA some areas, is circular behind its berry fruit maturation, darkly purple.Tibetan medicine and dimension medicine are used to treat heart-heat syndrome, heart disease, blood pressure lowering and menoxenia etc., the strengthening by means of tonics that is used among the people.Procyanidin content is 0.62% in the black fruit lyceum juice, and the ORAC value is 66737 μ molTE/L, and the procyanidin content of dry fruit is 7.2%, illustrates that black Fructus Lycii has good antioxidant activity.
Summary of the invention
It is the preparation method of raw material, procyanidin extract of lycium ruthenicum murr with low cost with the black Fructus Lycii that technical problem to be solved by this invention provides a kind of.
For addressing the above problem, the preparation method of a kind of procyanidin extract of lycium ruthenicum murr of the present invention may further comprise the steps:
(1) be raw material with black fruit lyceum juice or black Fructus Lycii concentrated solution, after nonpolar macroporous adsorption resin separates, be eluted to sugar-free with deionized water, the hydrochloric acid of 2～50 times of bed volume of reuse-alcoholic solution eluting is adsorbed on the procyanidin on the macroporous resin, obtains containing the eluent of procyanidin; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 40～100%, the hydrochloric acid mass concentration is 0.5～3%;
(2) the described eluent that contains procyanidin is concentrated or after NF membrane concentrates, obtains the procyanidin concentrated solution through vacuum decompression;
(3) described procyanidin concentrated solution after the spray-dried or lyophilization, can be obtained procyanidin extract of lycium ruthenicum murr.
Black fruit lyceum juice in the described step (1) is meant the squeezing of fresh black Fructus Lycii fruit after 0.5～300 μ m filter or 3000～8000r/min centrifuge filter and remove residue, and cross 0.02～10 μ m ceramic membrane and remove the fruit juice of float.
After black Fructus Lycii concentrated solution in the described step (1) is meant and squeezes the juice the fresh black Fructus Lycii fruit that drying is crossed back remaining seed skin or exsiccant black Fructus Lycii fruit pulverize, extract 2～3 times down at 25～60 ℃ with the hydrochloric acid-alcoholic solution of its 3～10 times of weight, and with the extracting solution that obtains successively through 0.5～300 μ m filter filters, vacuum decompression concentrates or NF membrane obtains after concentrating concentrated solution; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 10～100%, the hydrochloric acid mass concentration is 0.5～3%.
The spissated condition of described NF membrane is meant that the NF membrane molecular cut off is 50～300, and pressure is 2～20kg, and temperature is 15～50 ℃, and flow velocity is 50～1000ml/min.
The present invention compared with prior art has the following advantages:
1, because the present invention adopts membrane separation technique set column chromatography for separation technology, promptly earlier can effectively remove impurity such as tannin in the fruit juice, phlegmatic temperament with ceramic membrane, separate by macroporous resin again, therefore, not only shortened the time of extraction separation effectively, reduced the energy consumption in the technical process, and resulting product purity height, stable performance, the Medicines and Health Product raw material that can be applicable to the natural pigment food additive and have antioxidation.Through high-efficient liquid phase chromatogram HPLC (source: U.S. Agilent company, Agilent 1100) test, the procyanidin content of products obtained therefrom 〉=50%, total polyphenols content 〉=50%, anthocyanin content 〉=1%.
2, because the present invention adopts NF membrane to concentrate, and NF membrane has the higher property held back to small organic molecule, therefore, has reduced equipment investment effectively, has also reduced power consumption simultaneously.
3, because the black Fructus Lycii fruit that the present invention adopts the raw material resources amount to enrich is a raw material, therefore, reduced production cost effectively.
4, because the present invention adopts the ethanol elution of different quality concentration, therefore, in separation process, can obtain the procyanidin extract of lycium ruthenicum murr product of various content, thereby satisfy the market demand of different levels on the international market.
The specific embodiment
The preparation method of 1 one kinds of procyanidin extract of lycium ruthenicum murr of embodiment may further comprise the steps:
(1) with the 10kg black fruit lyceum juice, after nonpolar macroporous adsorption resin separates, use the deionized water eluting, to remove protein, saccharide impurity, the hydrochloric acid of 2 times of bed volume of reuse-alcoholic solution eluting is adsorbed on the procyanidin on the macroporous resin, obtains containing the eluent of procyanidin; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 40%, the hydrochloric acid mass concentration is 0.5%;
Wherein: black fruit lyceum juice is meant the squeezing of fresh black Fructus Lycii fruit after 0.5 μ m filter filters fine particle removes slag, and is that 0.2Mpa, flow velocity are that the 0.02 μ m ceramic membrane microfiltration of 120ml/min is removed float, tannin and mucilaginous fruit juice through pressure.
(2) eluent that will contain procyanidin is after 55 ℃, pressure are that vacuum decompression concentrates under the condition of 0.07Mpa, to reclaim ethanol in temperature, obtains the procyanidin concentrated solution.
(3) the procyanidin concentrated solution is at the import hot blast temperature that 160 ℃, outlet hot blast temperature are that 80 ℃, dry matter content are 12%, feeding temperature is that 60 ℃, centrifugal atomizer rotating speed are after carrying out spray drying under the condition of 25000r/min, can obtain the 0.4kg procyanidin extract of lycium ruthenicum murr.
Through the HPLC test, procyanidin content is 50.6% in this extract, and total polyphenols content is 52.3%, and anthocyanin content is 1.46%.
The preparation method of 2 one kinds of procyanidin extract of lycium ruthenicum murr of embodiment may further comprise the steps:
(1) with the 10kg black fruit lyceum juice, after nonpolar macroporous adsorption resin separates, use the deionized water eluting, to remove protein, saccharide impurity, the hydrochloric acid of 5 times of bed volume of reuse-alcoholic solution eluting is adsorbed on the procyanidin on the macroporous resin, obtains containing the eluent of procyanidin; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 100%, the hydrochloric acid mass concentration is 3%;
Wherein: black fruit lyceum juice is meant the squeezing of fresh black Fructus Lycii fruit after 300 μ m filters filter fine particle removes slag, and is that 0.05Mpa, flow velocity are that the 10 μ m ceramic membrane microfiltration of 220ml/min are removed float, tannin and mucilaginous fruit juice through pressure.
(2) eluent that will contain procyanidin is that 25 ℃, flow velocity are that 50ml/min, pressure are under the condition of 11kg in temperature, and adopting molecular cut off is that 50 NF membrane concentrates, reclaim ethanol after, obtain the procyanidin concentrated solution.
(3) be after 80 ℃, vacuum are to carry out lyophilization under the condition of 20Pa, can obtain the 0.43kg procyanidin extract of lycium ruthenicum murr with the procyanidin concentrated solution for-30 ℃, temperature of heating plate at condenser temperature.
Through the HPLC test, procyanidin content is 53.7% in this extract, and total polyphenols content is 56.9%, and anthocyanin content is 1.52%.
The preparation method of 3 one kinds of procyanidin extract of lycium ruthenicum murr of embodiment may further comprise the steps:
(1) with the 10kg black fruit lyceum juice, after nonpolar macroporous adsorption resin separates, use the deionized water eluting, to remove protein, saccharide impurity, the hydrochloric acid of 10 times of bed volume of reuse-alcoholic solution eluting is adsorbed on the procyanidin on the macroporous resin, obtains containing the eluent of procyanidin; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 70%, the hydrochloric acid mass concentration is 1%;
Wherein: black fruit lyceum juice is meant the squeezing of fresh black Fructus Lycii fruit after 150 μ m filters filter fine particle removes slag, and is that 0.1Mpa, flow velocity are that the 5 μ m ceramic membrane microfiltration of 150ml/min are removed float, tannin and mucilaginous fruit juice through pressure.
(2) eluent that will contain procyanidin is that 30 ℃, flow velocity are that 300ml/min, pressure are under the condition of 8kg in temperature, and adopting molecular cut off is that 300 NF membrane concentrates, reclaim ethanol after, obtain the procyanidin concentrated solution.
(3) with concentrated solution spray-dried after, can obtain the 0.39kg procyanidin extract of lycium ruthenicum murr.
Through the HPLC test, procyanidin content is 54% in this extract, and total polyphenols content is 53%, and anthocyanin content is 1.57%.
The preparation method of 4 one kinds of procyanidin extract of lycium ruthenicum murr of embodiment may further comprise the steps:
(1) with the 25kg black fruit lyceum juice, after nonpolar macroporous adsorption resin separates, use the deionized water eluting, to remove protein, saccharide impurity, the hydrochloric acid of 15 times of bed volume of reuse-alcoholic solution eluting is adsorbed on the procyanidin on the macroporous resin, obtains containing the eluent of procyanidin; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 50%, the hydrochloric acid mass concentration is 2%;
Wherein: black fruit lyceum juice is meant the squeezing of fresh black Fructus Lycii fruit after 3000r/min centrifuge centrifugal filtration fine particle removes slag, and is that 0.2Mpa, flow velocity are that the 0.05 μ m ceramic membrane microfiltration of 120ml/min is removed float, tannin and mucilaginous fruit juice through pressure.
(2) eluent that will contain procyanidin is that 15 ℃, flow velocity are that 200ml/min, pressure are under the condition of 2kg in temperature, and adopting molecular cut off is that 200 NF membrane concentrates, reclaim ethanol after, obtain the procyanidin concentrated solution.
(3) with the procyanidin concentrated solution after lyophilization, can obtain the 1.2kg procyanidin extract of lycium ruthenicum murr.
Through the HPLC test, procyanidin content is 65.1% in this extract, and total polyphenols content is 69.1%, and anthocyanin content is 1.79%.
The preparation method of 5 one kinds of procyanidin extract of lycium ruthenicum murr of embodiment may further comprise the steps:
(1) with the 25kg black fruit lyceum juice, after nonpolar macroporous adsorption resin separates, use the deionized water eluting, to remove protein, saccharide impurity, the hydrochloric acid of 10 times of bed volume of reuse-alcoholic solution eluting is adsorbed on the procyanidin on the macroporous resin, obtains containing the eluent of procyanidin; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 90%, the hydrochloric acid mass concentration is 3%;
Wherein: black fruit lyceum juice is meant the squeezing of fresh black Fructus Lycii fruit after 8000r/min centrifuge centrifugal filtration fine particle removes slag, and is that 0.04Mpa, flow velocity are that the 8 μ m ceramic membrane microfiltration of 240ml/min are removed float, tannin and mucilaginous fruit juice through pressure.
(2) eluent that will contain procyanidin is that 21 ℃, flow velocity are that 121ml/min, pressure are under the condition of 9kg in temperature, and adopting molecular cut off is that 100 NF membrane concentrates, reclaim ethanol after, obtain the procyanidin concentrated solution.
(3) with the procyanidin concentrated solution after lyophilization, can obtain the 1.1kg procyanidin extract of lycium ruthenicum murr.
Through the HPLC test, procyanidin content is 95.7% in this extract, and total polyphenols content is 94.7%, and anthocyanin content is 4.8%.
The preparation method of 6 one kinds of procyanidin extract of lycium ruthenicum murr of embodiment may further comprise the steps:
(1) with the 25kg black fruit lyceum juice, after nonpolar macroporous adsorption resin separates, use the deionized water eluting, to remove protein, saccharide impurity, the hydrochloric acid of 20 times of bed volume of reuse-alcoholic solution eluting is adsorbed on the procyanidin on the macroporous resin, obtains containing the eluent of procyanidin; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 60%, the hydrochloric acid mass concentration is 1%;
Wherein: black fruit lyceum juice is meant the squeezing of fresh black Fructus Lycii fruit after 5000r/min centrifuge centrifugal filtration fine particle removes slag, and is that 0.1Mpa, flow velocity are that the 6 μ m ceramic membrane microfiltration of 150ml/min are removed float, tannin and mucilaginous fruit juice through pressure.
(2) eluent that will contain procyanidin is that 35 ℃, flow velocity are that 1000ml/min, pressure are under the condition of 5kg in temperature, and adopting molecular cut off is that 150 NF membrane concentrates, reclaim ethanol after, obtain the procyanidin concentrated solution.
(3) with the procyanidin concentrated solution spray-dried after, can obtain the 1.4kg procyanidin extract of lycium ruthenicum murr.
Through the HPLC test, procyanidin content is 75.5% in this extract, and total polyphenols content is 72.3%, and anthocyanin content is 1.62%.
The preparation method of 7 one kinds of procyanidin extract of lycium ruthenicum murr of embodiment may further comprise the steps:
(1) with 50kg black Fructus Lycii concentrated solution, after nonpolar macroporous adsorption resin separates, use the deionized water eluting, to remove protein, saccharide impurity, the hydrochloric acid of 50 times of bed volume of reuse-alcoholic solution eluting is adsorbed on the procyanidin on the macroporous resin, obtains containing the eluent of procyanidin; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 85%, the hydrochloric acid mass concentration is 0.5%;
Wherein: after the black Fructus Lycii concentrated solution is meant exsiccant black Fructus Lycii fruit pulverized, extract 2 times down at 25 ℃ with the hydrochloric acid-alcoholic solution of its 3 times of weight, the extraction time first time is 60min, and all the other extraction times are 30min, merge extractive liquid; And with the extracting solution that obtains through 300 μ m filters filter remove fine particle after, be that 50 ℃, pressure are to carry out vacuum decompression under the condition of 0.06Mpa to concentrate the concentrated solution that obtains in temperature; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 10%, the hydrochloric acid mass concentration is 3%.
(2) eluent that will contain procyanidin is after 50 ℃, pressure are that vacuum decompression concentrates under the condition of 0.06Mpa, to reclaim ethanol in temperature, obtains the procyanidin concentrated solution.
(3) with after the procyanidin concentrated solution employing spray drying, can obtain the 2kg procyanidin extract of lycium ruthenicum murr.
Through the HPLC test, procyanidin content is 73.2% in this extract, and total polyphenols content is 79.0%, and total anthocyanin content is 1.58%.
The preparation method of 8 one kinds of procyanidin extract of lycium ruthenicum murr of embodiment may further comprise the steps:
(1) with 50kg black Fructus Lycii concentrated solution, after nonpolar macroporous adsorption resin separates, use the deionized water eluting, to remove protein, saccharide impurity, the hydrochloric acid of 10 times of bed volume of reuse-alcoholic solution eluting is adsorbed on the procyanidin on the macroporous resin, obtains containing the eluent of procyanidin; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 60%, the hydrochloric acid mass concentration is 0.8%;
Wherein: the black Fructus Lycii concentrated solution be meant the fresh black Fructus Lycii fruit that drying is crossed squeeze the juice the back remaining seed corium farinosum broken after, hydrochloric acid-alcoholic solution with its 10 times of weight extracts 3 times down at 60 ℃, extraction time is 50min for the first time, and all the other extraction times are 40min, merge extractive liquid; And it is the extracting solution that obtains is first through 0.5 μ m filter filtration removal fine particle, filtrate is after 0.10Mpa, flow velocity are the 10 μ m ceramic membrane microfiltration of 300ml/min through pressure, being 100 NF membrane again through molecular cut off, is that 50 ℃, pressure are that 20kg, flow velocity are to concentrate the concentrated solution that obtains under the condition of 50ml/min in temperature; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 100%, the hydrochloric acid mass concentration is 1.5%.
(2) eluent that will contain procyanidin is that 40 ℃, flow velocity are that 20ml/min, pressure are under the condition of 10kg in temperature, and adopting molecular cut off is after 100 NF membrane concentrates, to reclaim ethanol, obtains the procyanidin concentrated solution.
(3) with after the procyanidin concentrated solution employing lyophilization, can obtain the 2.6kg procyanidin extract of lycium ruthenicum murr.
Through the HPLC test, procyanidin content is 52.8% in this extract, and total polyphenols content is 58.6%, and total anthocyanin content is 1.32%.
The preparation method of 9 one kinds of procyanidin extract of lycium ruthenicum murr of embodiment may further comprise the steps:
(1) with 50kg black Fructus Lycii concentrated solution, after nonpolar macroporous adsorption resin separates, use the deionized water eluting, to remove protein, saccharide impurity, the hydrochloric acid of 2 times of bed volume of reuse-alcoholic solution eluting is adsorbed on the procyanidin on the macroporous resin, obtains containing the eluent of procyanidin; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 80%, the hydrochloric acid mass concentration is 2%;
Wherein: after the black Fructus Lycii concentrated solution is meant exsiccant black Fructus Lycii fruit pulverized, extract 3 times down at 50 ℃ with the hydrochloric acid-alcoholic solution of its 7 times of weight, the extraction time first time is 70min, and all the other extraction times are 20min, merge extractive liquid; And with the extracting solution that obtains through 180 μ m filters filter remove fine particle after, be that 50 ℃, pressure are to carry out vacuum decompression under the condition of 0.06Mpa to concentrate the concentrated solution that obtains in temperature; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 70%, the hydrochloric acid mass concentration is 0.5%.
(2) eluent that will contain procyanidin is after 60 ℃, pressure are that vacuum decompression concentrates under the condition of 0.05Mpa, to reclaim ethanol in temperature, obtains the procyanidin concentrated solution.
(3) with after the procyanidin concentrated solution employing spray drying, can obtain the 2.2kg procyanidin extract of lycium ruthenicum murr.
Through the HPLC test, procyanidin content is 76% in this extract, and total polyphenols content is 75%, and total anthocyanin content is 2.33%.
Claims (4)
1. the preparation method of a procyanidin extract of lycium ruthenicum murr may further comprise the steps:
(1) be raw material with black fruit lyceum juice or black Fructus Lycii concentrated solution, after nonpolar macroporous adsorption resin separates, be eluted to sugar-free with deionized water, the hydrochloric acid of 2～50 times of bed volume of reuse-alcoholic solution eluting is adsorbed on the procyanidin on the macroporous resin, obtains containing the eluent of procyanidin; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 40～100%, the hydrochloric acid mass concentration is 0.5～3%;
(2) the described eluent that contains procyanidin is concentrated or after NF membrane concentrates, obtains the procyanidin concentrated solution through vacuum decompression;
(3) described procyanidin concentrated solution after the spray-dried or lyophilization, can be obtained procyanidin extract of lycium ruthenicum murr.
2. the preparation method of a kind of procyanidin extract of lycium ruthenicum murr as claimed in claim 1 is characterized in that: the black fruit lyceum juice in the described step (1) is meant fresh black Fructus Lycii fruit squeezing after 0.5～300 μ m filter or 3000～8000r/min centrifuge filter and remove residue, and cross 0.02～10 μ m ceramic membrane and remove the fruit juice of float.
3. the preparation method of a kind of procyanidin extract of lycium ruthenicum murr as claimed in claim 1, it is characterized in that: after the black Fructus Lycii concentrated solution in the described step (1) is meant and squeezes the juice the fresh black Fructus Lycii fruit that drying is crossed back remaining seed skin or exsiccant black Fructus Lycii fruit pulverize, extract 2～3 times down at 25～60 ℃ with the hydrochloric acid-alcoholic solution of its 3～10 times of weight, and with the extracting solution that obtains successively through 0.5～300 μ m filter filters, vacuum decompression concentrates or NF membrane obtains after concentrating concentrated solution; Wherein the ethanol mass concentration in hydrochloric acid-alcoholic solution is 10～100%, the hydrochloric acid mass concentration is 0.5～3%.
4. as the preparation method of claim 1 or 3 described a kind of procyanidin extract of lycium ruthenicum murr, it is characterized in that: the spissated condition of described NF membrane is meant that the NF membrane molecular cut off is 50～300, pressure is 2～20kg, and temperature is 15～50 ℃, and flow velocity is 50～1000ml/min.
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