CN103110671A - Method for removing ginkgolic acid and heavy metals in ginkgo biloba extract by using nanometer material - Google Patents
Method for removing ginkgolic acid and heavy metals in ginkgo biloba extract by using nanometer material Download PDFInfo
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- CN103110671A CN103110671A CN2013100330524A CN201310033052A CN103110671A CN 103110671 A CN103110671 A CN 103110671A CN 2013100330524 A CN2013100330524 A CN 2013100330524A CN 201310033052 A CN201310033052 A CN 201310033052A CN 103110671 A CN103110671 A CN 103110671A
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Abstract
The invention discloses a method for removing ginkgolic acid and heavy metals in a ginkgo biloba extract by using a nanometer material. The method is characterized in that the ginkgo biloba extract is obtained by extraction, column chromatography, adsorption of the nanometer material, separation of the nanometer material, concentration and drying of separation liquid; a ferroferric oxide nanometer material is used as the nanometer material; and a magnetic separation process is used as a nanometer material separation process. As the improvement, the method further can comprise a step of recovering the nanometer material. According to the method provided by the invention, the ginkgolic acid, urushiol, isourushiol and the heavy metals are adsorbed by a Fe3O4 nanometer material; solid-liquid separation is carried out by using the magnetic separation process; and a finished product can be obtained by concentrating and drying the medicine liquid. The method provided by the invention has the double effects of environmental friendliness and simultaneous removal of the ginkgolic acid and the heavy metals.
Description
Technical field
The invention belongs to the natural product preparing technical field, be specifically related to a kind of method of utilizing the nano material adsorption to remove Ginkgolic Acid in Extract of Ginkgo biloba Leaves and heavy metal.
Background technology
Folium Ginkgo is the dried leaves of Ginkgoaceae plant Ginkgo biloba (Ginkgo biloba L.), and property is sweet, bitter, puckery, flat, and GUIXIN, lung meridian have astringing the lung, relieving asthma, the effects such as blood circulation promoting and blood stasis dispelling, pain relieving, are used for coronary heart diseases and angina pectoris and hyperlipemia.Folium Ginkgo extract is the extract of Folium Ginkgo through being processed into, activating blood circulation to dissipate blood stasis and dredge the collateral, and it is tongue-tied to be used for the treatment of obstruction of qi in the chest and cardialgia, apoplexy, hemiplegia, stiff tongue that obstruction of collaterals by blood stasis causes; Treating Stable Angina Pectoris of Coronary Artery Disease, cerebral infarction are seen above-mentioned patient.Folium Ginkgo and Folium Ginkgo extract are as raw material, be widely used in treating the preparation of cardiovascular and cerebrovascular disease, only " Chinese pharmacopoeia has just been recorded 5 relevant kinds that comprise Folium Ginkgo, " European Pharmacopoeia " stipulated the standard of Folium Ginkgo and Folium Ginkgo extract, and " American Pharmacopeia " also includes Folium Ginkgo and preparation thereof as food supplement.But also contain a kind of toxic component-ginkgoic acid in the ginkgo agent, have the effects such as sensitization, cytotoxicity, so international standard requires the content of ginkgoic acid less than 5ppm, require simultaneously content of beary metal less than 10ppm.The content of ginkgoic acid and heavy metal substantially exceeds international standard in the ginkgo agent that China produces at present.Cause China most of Folium Ginkgo extract manufacturing enterprise to be in and stop production or half state that stops production, ginkgoic acid and the heavy metal of how effectively to remove in the Folium Ginkgo extract are the subject matter of current China chemist research.
At present, the method that removes ginkgoic acid has: (1) Schwabe company propose acetone extraction+extraction; (2) acetone extraction+chromatography+organic solvent extraction; (3) ethanol extraction+chromatography+organic solvent extraction; (4) supercritical extraction.Solvent extraction very easily produces emulsifying and causes production time prolongation and extraction not exclusively, has dissolvent residual in the product, and is unfriendly to operator and environment simultaneously.Patent documentation " removing process of gingkolic acid in the Folium Ginkgo extract " (CN101194918A) adopts twin columns stack way to remove ginkgoic acid, but affected more complicated, and the pretreatment of twin columns can produce a certain amount of industrial wastewater with activation.
It is the bottleneck of restriction China Folium Ginkgo extract outlet that Ginkgolic Acid in Extract of Ginkgo biloba Leaves and content of beary metal exceed standard, and has also affected the safety of domestic pharmacy simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing nano material to remove Ginkgolic Acid in Extract of Ginkgo biloba Leaves and heavy metal, the method has environmental friendliness, removes simultaneously the double effects of ginkgoic acid and heavy metal.
A kind of method of utilizing nano material to remove Ginkgolic Acid in Extract of Ginkgo biloba Leaves and heavy metal provided by the invention, the method obtains Folium Ginkgo extract by extraction, column chromatography, nano material absorption, nano material separation, separating medium concentrate drying; Described nano material is ferriferrous oxide nanometer material, and described nano material isolation technics is magnetic separation technique.
As a kind of improvement of technique scheme, the method also comprises the nano material recycling step.
Another kind as technique scheme improves, described extraction comprises following detailed process: Folium Ginkgo adds respectively 60-70% ethanol, the mass volume ratio of Folium Ginkgo and alcoholic solution is 1: 5-1: 10, and reflux, extract, at least 2 times, each 1-3 hour, merge extractive liquid,, decompression recycling ethanol, the water of 3-5 times of Folium Ginkgo weight of adding leaves standstill, filter filtrate for later use.
Another improvement as technique scheme, described column chromatography comprises following detailed process: adopt AB-8, the HP-20 after activating, any one dress post in these 4 kinds of resins of DA201, D101, filtrate with gained in the extraction step, washing post with 3-6 times of resin bed volume, adopt the 60-80% ethanol desorbing of 2-4 times of resin bed volume, collection ethanol elution part is for subsequent use.
As further improvement in the technical proposal, described nano material is adsorbed following detailed process: add ferriferrous oxide nanometer material in the ethanol elution of collecting, the quality of ferroso-ferric oxide is 0.01%-1% with the ratio of ethanol elution volume, ultrasonic absorption 0.5-8h.
As further improving again of technique scheme, the mode of described separating medium concentrate drying is vacuum drying or spray drying.
Further improvement as technique scheme, described nano material removal process is: the ferriferrous oxide nanometer material that the nano material separating step obtains is collected, with 0.05%-2% soak with hydrochloric acid 0.5-24h, then dry for several times with deionized water rinsing.
Fe
3O
4Nano material and catechol and derivant thereof have higher affinity, so the phytochemicals of some carboxyls of selective absorption or ortho position phenolic hydroxyl group.The Semen Ginkgo total acid comprises ginkgoic acid, Semen Ginkgo laccol, different Semen Ginkgo laccol, ginkgolic acid etc., and its basic structure all has carboxyl or ortho-phenolic hydroxyl, Fe
3O
4Nano material can be adsorbed ginkgoic acid, laccol, different laccol etc., utilizes magnetic separation technique that the Semen Ginkgo total acid is separated from mother solution.The invention has the advantages that and utilize Fe
3O
4Nano material not only can be removed ginkgoic acid, and can removal heavy metal, reaches the effect of killing two birds with one stone, simultaneously can also be with Fe
3O
4Nano material is by the pickling recycling, and the ginkgoic acid of industrialized great production enrichment can be made biological insecticides and other purposes.
The specific embodiment
The nano material of utilizing that the specific embodiment of the invention provides removes the method for Ginkgolic Acid in Extract of Ginkgo biloba Leaves and heavy metal, specifically finishes by following steps:
The 1st step extracted: Folium Ginkgo adds respectively 60-70% ethanol, and the proportioning of Folium Ginkgo and alcoholic solution is 5-10 (W/V), reflux, extract, at least 2 times, each 1-3 hour, merge extractive liquid,, decompression recycling ethanol, the water of 3-5 times of Folium Ginkgo weight of adding, leave standstill, filter filtrate for later use.
The 2nd step column chromatography: adopt AB-8, the HP-20 after activating, any one dress post in these 4 kinds of resins of DA201, D101, the filtrate upper prop of gained will be extracted, with 3-6 times of volume washing post, adopt the 60-80% ethanol desorbing of 2-4 times of resin bed volume, collection ethanol elution part is for subsequent use.
The 3rd step nano material absorption: in the ethanol elution of collecting, add the ferriferrous oxide nanometer material of 0.01-1% (W/V), ultrasonic absorption 0.5-8h.
The 4th step nano material is separated: adopt permanent magnetism or electromagnetism that ferriferrous oxide nanometer material is adsorbed, finish solid-liquid separation.
The 5th step separating medium concentrate drying: vacuum drying or spray drying.
The 6th step nano material reclaims: the ferriferrous oxide nanometer material that the nano material separating step obtains is collected, with 0.05%-2% soak with hydrochloric acid 0.5-24h, then with dry getting final product behind the deionized water rinsing several.
Below in conjunction with example the specific embodiment of the present invention is described further.Need to prove at this, understand the present invention for the explanation of these embodiments for helping, but do not consist of limitation of the invention.In addition, below in each embodiment of described the present invention involved technical characterictic just can mutually not make up as long as consist of each other conflict.
Embodiment 1
Get Folium Ginkgo 500g, add 10,8 times of amount 60% ethanol, respectively reflux, extract, 2h, the leaching medicinal liquid, merge, decompression recycling ethanol to medicinal liquid does not contain alcohol, then adds water to 1500ml, leave standstill, filter, filtrate is added on and processes the DA201 resin column, and pure water is crossed post and cleaned, when effluent is more limpid, use the 2000mL80% ethanol elution, collect ethanol elution, add the 0.2g ferriferrous oxide nanometer material, ultrasonic absorption 2h, Magnet is put into the liquid absorption ferriferrous oxide nanometer material, medicinal liquid concentrating under reduced pressure Recycled ethanol, extractum vacuum drying.Collect ferriferrous oxide nanometer material, put into 0.1% hydrochloric acid and soak 4h, magnetic separates, the deionized water rinsing several, and vacuum drying is for subsequent use.After dry Folium Ginkgo extract weigh, sampling and measuring total flavones, total lactone, ginkgoic acid and content of beary metal.The result is: Folium Ginkgo extract 9.1g, general flavone content are 28.3%, total lactone 8.6%, ginkgoic acid 2ppm, heavy metal 4ppm.
Embodiment 2
Get Folium Ginkgo 500g, add 8,6 times of amount 70% ethanol, difference reflux, extract, 1.5h, the leaching medicinal liquid merges, decompression recycling ethanol to medicinal liquid does not contain alcohol, then adds water to 1500ml, leaves standstill, filter, filtrate is added on and processes the D101 resin column, and pure water is crossed post and cleaned, when effluent is more limpid, use the 2500mL80% ethanol elution, collect ethanol elution, when decompression recycling ethanol reaches 1.08-1.10 to the medicinal liquid solid content, stop to concentrate, add the 0.5g ferriferrous oxide nanometer material in the medicinal liquid, ultrasonic absorption 5h, electric magnet is put into the liquid absorption ferriferrous oxide nanometer material, medicinal liquid concentrating under reduced pressure, when solid content reaches 1.25-1.30, spray drying.Collect ferriferrous oxide nanometer material, put into 1% hydrochloric acid and soak 2h, magnetic separates, the deionized water rinsing several, and vacuum drying is for subsequent use.After dry Folium Ginkgo extract weigh, sampling and measuring total flavones, total lactone, ginkgoic acid and content of beary metal.The result is: Folium Ginkgo extract 10.2g, general flavone content are 27.2%, total lactone 8.2%, ginkgoic acid 2ppm, heavy metal 5ppm.
Embodiment 3
Get Folium Ginkgo 500g, add 10,5 times of amount 70% ethanol, difference reflux, extract, 3h, the leaching medicinal liquid merges, and decompression recycling ethanol to medicinal liquid does not contain alcohol, then add water to 1500ml, leave standstill, filter, filtrate is added on and processes the AB-8 resin column, pure water is crossed post and is cleaned, when effluent is more limpid, use the 2000mL60% ethanol elution, collect ethanol elution, add the 1.0g ferriferrous oxide nanometer material, ultrasonic absorption 8h, Magnet is put into the liquid absorption ferriferrous oxide nanometer material, medicinal liquid concentrating under reduced pressure, when solid content reaches 1.25-1.30, spray drying.Collect ferriferrous oxide nanometer material, put into 2% hydrochloric acid and soak 24h, magnetic separates, the deionized water rinsing several, and vacuum drying is for subsequent use.After dry Folium Ginkgo extract weigh, sampling and measuring total flavones, total lactone, ginkgoic acid and content of beary metal.The result is: Folium Ginkgo extract 8.8g, general flavone content are 26.6%, total lactone 7.4%, ginkgoic acid 1ppm, heavy metal 3ppm.
Embodiment 4
Get Folium Ginkgo 500g, add 10,8 times of amount 65% ethanol, difference reflux, extract, 2h, the leaching medicinal liquid merges, decompression recycling ethanol to medicinal liquid does not contain alcohol, then adds water to 1500ml, leaves standstill, filter, filtrate is added on and processes the HP-20 resin column, and pure water is crossed post and cleaned, when effluent is more limpid, use the 2800mL80% ethanol elution, collect ethanol elution, when decompression recycling ethanol reaches 1.08-1.10 to the medicinal liquid solid content, stop to concentrate, add the 5.0g ferriferrous oxide nanometer material, ultrasonic absorption 3h, Magnet is put into the liquid absorption ferriferrous oxide nanometer material, medicinal liquid concentrating under reduced pressure, when solid content reaches 1.25-1.30, spray drying.Collect ferriferrous oxide nanometer material, put into 2% hydrochloric acid and soak 3h, magnetic separates, the deionized water rinsing several, and vacuum drying is for subsequent use.After dry Folium Ginkgo extract weigh, sampling and measuring total flavones, total lactone, ginkgoic acid and content of beary metal.The result is: Folium Ginkgo extract 9.5g, general flavone content are 28.6%, total lactone 7.6%, ginkgoic acid 1ppm, heavy metal 2ppm.
Among the present invention, the concentration of ethanol and hydrochloric acid all refers to concentration of volume percent.
The above is preferred embodiment of the present invention, but the present invention should not be confined to the disclosed content of this embodiment.So everyly do not break away from the equivalence of finishing under the spirit disclosed in this invention or revise, all fall into the scope of protection of the invention.
Claims (7)
1. method that removes Ginkgolic Acid in Extract of Ginkgo biloba Leaves and heavy metal, the method by extraction, column chromatography, nano material absorption, nano material separate, the separating medium concentrate drying obtains Folium Ginkgo extract; Described nano material is ferriferrous oxide nanometer material, and described nano material isolation technics is magnetic separation technique.
2. the method that removes Ginkgolic Acid in Extract of Ginkgo biloba Leaves and heavy metal according to claim 1 is characterized in that, the method also comprises the nano material recycling step.
3. the method that removes Ginkgolic Acid in Extract of Ginkgo biloba Leaves and heavy metal according to claim 1, it is characterized in that described extraction comprises following detailed process: Folium Ginkgo adds respectively 60-70% ethanol, and the mass volume ratio of Folium Ginkgo and alcoholic solution is 1: 5-1: 10, reflux, extract, at least 2 times, each 1-3 hour, merge extractive liquid,, decompression recycling ethanol, the water that adds 3-5 times of Folium Ginkgo weight, leave standstill, filter filtrate for later use.
4. the method that removes Ginkgolic Acid in Extract of Ginkgo biloba Leaves and heavy metal according to claim 1, it is characterized in that, described column chromatography comprises following detailed process: adopt AB-8, the HP-20 after activating, any one dress post in these 4 kinds of resins of DA201, D101, filtrate with gained in the extraction step, washing post with 3-6 times of resin bed volume, adopt the 60-80% ethanol desorbing of 2-4 times of resin bed volume, collection ethanol elution part is for subsequent use.
5. the method that removes Ginkgolic Acid in Extract of Ginkgo biloba Leaves and heavy metal according to claim 1, it is characterized in that, described nano material absorption comprises following detailed process: add ferriferrous oxide nanometer material in the ethanol elution of collecting, the quality of ferroso-ferric oxide is 0.01%-1% with the ratio of ethanol elution volume, ultrasonic absorption 0.5-8h.
6. the method that removes Ginkgolic Acid in Extract of Ginkgo biloba Leaves and heavy metal according to claim 1 is characterized in that, the mode of described separating medium concentrate drying is vacuum drying or spray drying.
7. the method that removes Ginkgolic Acid in Extract of Ginkgo biloba Leaves and heavy metal according to claim 2, it is characterized in that, described nano material removal process is: the ferriferrous oxide nanometer material that the nano material separating step obtains is collected, with 0.05%-2% soak with hydrochloric acid 0.5-24h, then dry for several times with deionized water rinsing.
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Address after: 430074 Hubei Province, Wuhan city Hongshan District Luoyu Road No. 1037 Patentee after: Huazhong University of Science and Technology Patentee after: Hubei Nuo Kete medicine company limited-liability company Address before: 430074 Hubei Province, Wuhan city Hongshan District Luoyu Road No. 1037 Patentee before: Huazhong University of Science and Technology Patentee before: Hubei Nuokete Pharmaceutical Co., Ltd. |