CN101530193A - Method for comprehensively extracting and purifying oxidation-resistant active ingredient in sugarcane toppers or slag - Google Patents
Method for comprehensively extracting and purifying oxidation-resistant active ingredient in sugarcane toppers or slag Download PDFInfo
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Abstract
The invention discloses a method for comprehensively extracting and purifying general flavone and anthocyanin in sugarcane toppers or slag. The method comprises the steps of firstly extracting the sugarcane toppers or slag by an organic solvent, concentrating the extract and passing the extract through a chromatographic column filled with a macro-porous adsorptive resin, removing water-soluble impurities such as glucide by a gradient elution method, respectively collecting the ethanol eluent with a high concentration and the ethanol eluent with a low concentration to obtain two sites of the general flavone and anthocyanin, and respectively enriching and purifying the sites of the general flavone and anthocyanin by an acid and alkali treatment method and a solvent extraction method so as to obtain the general flavone and anthocyanin. Compared with the reported methods for extraction and separation of similar ingredients, the method of the invention can not only completely extract two main oxidation-resistant ingredients in the sugarcane toppers or slag, also the reagents consumed in the technological process can be recycled. The method has low production cost, high purity and mature technology, and is easily controlled and in favour of industrial production.
Description
Technical field
The invention belongs to the method and technology field of main oxidation-resistant active ingredient in comprehensive extraction separation and purification sugarcane toppers or the slag, be specifically related to main oxidation-resistant active ingredient---the method for general flavone, anthocyanidin in a kind of comprehensive extraction and purifying sugarcane toppers or the slag.
Background technology
Sugarcane (Saccharum officenarum L.) is a grass family saccharum plant, originates in the torrid zone, subtropical zone, its light saturation point height, carbon dioxide compensation point is low, the light respiration rate is low, and rate of photosynthisis is big, and the cultivated area of sugarcane 90% is distributed between the tropic of north and south.China is the earliest the country of growing cane in the world, and history in 2500 is arranged so far approximately, sugarcane biological yield height, and income is big, is the primary raw material of sugaring.Sugar is one of human essential edible product, it also is the important source material of food industry such as candy, beverage, and sugarcane juice flavor cold in nature is sweet, have clearing heat and promoting fluid, moisturize the function of the long-pending therapeutic method to keep the adverse qi flowing downward of quenching the thirst, disappear, be applicable to pyreticosis Tianjin wound, restlessness and thirst, gastric disorder causing nausea vomiting, xeropulmonary cough, all diseases of dry feces, be the good beverage of four seasons health care, China cures the disease with the sugar that sugarcane and sugarcane are made before more than 1,000 years.Simultaneously, sugarcane still is the important source material of light industry, chemical industry and energy field.
Recent study finds to also have some to have the composition of higher antioxidation activity in the sugarcane except containing a large amount of sucrose.Studies show that antioxidant content mainly is some polyphenols such as flavones in the sugarcane, anthocyanidin etc., they all have been widely used in industry such as food, cosmetics, medicine.Flavone compound has different physiological roles and medical value, mainly contains: antitumor, anti-oxidant, suppress pharmacological actions such as platelet aggregation, antiviral, estrogen adjusting, angiocardiopathy preventing, hypoglycemic and neuroprotective system.Anthocyanidin is different with other antioxidant, can directly protect brain and nervous system by blood-brain barrier, and therefore its pharmacologically active also becomes more powerful, wider than other antioxidant purposes; Its physiological action is mainly reflected in can remove human free radical, anticancer, and the enzyme inhibition of living protect aspects such as cardiovascular and immunoregulatory activity.Therefore above two constituents have use value and DEVELOPMENT PROSPECT preferably.
The existing a small amount of report of the research of chromocor compound in the relevant bagasse, as Renata Colombo (Renata Colombo, Fernando M.Lancas, Janete H.Yariwake.Determination of flavonoids in cultivated sugarcane leaves, bagasse, juice and in transgenic sugarcane by liquid chromatography-UV detection[J] .Journal of Chromatography A, 2006,118-124; Renata Colombo, Janete H.Yariwake, Emerson F.Queiroz, On-line Identification of FurtherFlavone C-and O-Glycosides from Sugarcane (Saccharum officinarum L., Gramineae) by HPLC-UV-MS[J] .Phytochemical Analysis, 2006 (17): 337-343; Renata Colombo, Janete H.Yariwake, Emerson F.Queiroz etal, On-line identification of sugarcane (Saccharum officinarum L.) methoxyflavones by liquid chromatography-UVdetection using post-column derivatization and liquid chromatography-mass spectrometry[J] .Journal ofChromatography A, 2005,51-59) wait the use high performance liquid chromatography, liquid-light such as matter coupling, the chromatogram means are to sugarcane top, sugar-cane juice, part flavonoid glycoside monomer has carried out chromatography and structure evaluation in the bagasse, and general flavone content is measured.But the research of flavones only rests on the micro-analysis context of detection in the bagasse, its separation purifying technique method is not studied, and the research for flavones in the sugarcane toppers had not simultaneously also had bibliographical information.And about the research of anthocyanidin in the sugarcane toppers except the inventor, have not yet to see any relevant report.
The industrial purification method of flavone compound mainly contains supercritical fluid extraction, and (what expands, Li Yufeng, Zhang Xiuyuan is etc. the research [J] of supercritical fluid extraction ginko leaves flavone class material. Shanxi food industry, 2005 (4): 2-5), polyamide chromatography method (Guo Yanhua, Xu Jiangyang, the Preliminary Identification [J] of the extraction purifying of cordate houttuynia total flavones and flavones type. Food Science, 2007,28 (9): 287-291) etc., above method equipment complexity, cost is higher.In addition, it is the method that solvent extracts polyphenoils in the sugarcane top with the alcohol-water that Wu Jianzhong (CN 1814695A) etc. discloses a kind of, the oxidation-resistant active ingredient in the heating reflux method lixiviate sugarcane top is used in this invention, can cause to a certain degree destruction to its active component like this, and n-butanol extraction purifying oxidation-resistant active ingredient is only adopted in this invention, and specific aim is not strong.And the raw material of this invention also is subjected to certain limitation, and only adopting sugarcane top is raw material, and finds that according to the study flavones content in the sugarcane toppers is far above sugarcane top.The purification process of anthocyanidin mainly contains polyamide column chromatography method (Wu Chaoxia, Meng Xianjun, gold Lei. the Primary Study [J] that polyamide separation and purification grape pip procyanidin and portion of product component constitute. food research and development, 2007,28 (2): 71-74), macroporous absorption column chromatography (Li Runfeng, Lv Xiaoling, Wang Qinghua. proanthocyanidin extracts and the Primary Study of separating [J] in the grape pip. grain and oil processing and food machinery, 2003 (6): 67-69), supercritical fluid extraction (Zheng Yongli. the analysis of proanthocyanidin in the grape pip, extraction and purification [D]. Hebei University of Technology, 2004) etc.Sun Xiaoxue (Sun Xiaoxue, the extraction of aldehydes matter and application study [D] in the sugarcane toppers. Guangxi University, 2007) the total aldehydes matter in the sugarcane toppers (comprising flavones, anthocyanidin and other phenols) qualitative and quantitative analysis and anti-oxidant and fresh-keeping application study thereof have been carried out, polyphenol in this The thesis polyamide chromatography method purifying sugarcane toppers, and polyamide is not strong to the selectivity of flavones in the sugarcane and anthocyanidin, these two kinds of compositions effectively can't be separated.At present, comparatively economical and practical macroporous absorbent resin method is not useful on the report of anthocyanidin in the separation and purification sugarcane as yet.The present invention handles soda acid first with the macroporous absorption column chromatography and is applied in the separation and purification of general flavone and anthocyanidin in sugarcane toppers or the bagasse, that its method is compared with existing document is with low cost, method is ripe, with strong points, by technical economic analysis as can be known, the profit margin of technology of the present invention can reach 10%～25%, is easier to medium-sized and small enterprises and realizes industrialization.
Sugar content in the sugarcane toppers is very low, and main component is a polyphenols.It is squeezed the extraction syrup with the sugarcane mobile jib, then strengthened the content of coexistent impurity in the sugar, both having purified to sucrose has increased burden, also is unfavorable for the wherein development and use of active ingredient except that sugar.If before entering press machines, simply the very low sugarcane toppers of sugar content is cut down, effectively utilize---extract antioxidation activity composition wherein, then can solve this contradiction substantially.In addition, bagasse mainly as the fuel of steam boiler, make the main raw material(s) of low-density and medium density fiber sheet material etc., anti-oxidant composition wherein goes out of use, resource is underutilized.As previously mentioned, research for effective active composition in the sugarcane only relates to wherein micro-analysis detection, physicochemical property or the preliminary activity research of a certain active ingredient, and only rest on theoretical research stage mostly, in sugarcane toppers or the slag in the extraction of a certain active ingredient, separation, purifying, the especially sugarcane the comprehensive extraction of active ingredient, separation, purifying bibliographical information is not also arranged.Therefore carry out the comprehensive utilization of sugarcane industrial waste sugarcane toppers, bagasse resource, not only reduced environmental pollution, made full use of resource, but also can increase economic efficiency, have favorable social and economic worth.
The present inventor has done comprehensive assay determination first for the content of polyphenoils in the various materials (kind surplus in the of 10) in the various raw materials in the cane sugar manufacture industrial process, the technical process, has established important basis for developing effective comprehensive utilization active principle wherein.
The present invention proposes comprehensively to extract anti-oxidation active substance (general flavone in the separation of sugarcane tip or the slag first, anthocyanidin) method, adopting source cane sugar manufacture industrial waste product sugarcane toppers, bagasse sufficient, cheap, that power of regeneration is strong is raw material, the method of using repeatedly extraction to combine with the macroporous absorption column chromatography on the basis that does not influence original sugaring operation is extracted simultaneously and is isolated two kinds of high anti-oxidation active components, this method technology is simple, with low cost, low in the pollution of the environment, possess favorable industrial trend and wide application prospect.
Summary of the invention
The objective of the invention is to adopt source cane sugar manufacture industrial waste product sugarcane toppers, bagasse sufficient, cheap, that power of regeneration is strong is raw material, proposes the method for anti-oxidation active substance (general flavone, anthocyanidin) in a kind of comprehensive extraction separation of sugarcane tip or the slag.This method can not damage oxidation-resistant active ingredient contained in sugarcane toppers or the slag on the one hand, and can obtain two kinds of active ingredient positions simultaneously, improved resource utilization, adopted the sugar industry waste products as raw material on the other hand, it is with low cost, technology is easy, be easy to control, with strong points, extracting cycle is short, do not influence original sugaring operation, have good industrial advantages and exploitation meaning.
(the general flavone of anti-oxidation active substance in a kind of comprehensively extracting and purifying sugarcane toppers that reaches the object of the invention and provide or the slag, anthocyanidin) method, it is characterized in that this method is earlier with sugarcane toppers or bagasse raw material pulverizing, lixiviate, then with leaching liquor by being filled with the chromatographic column of macroporous absorbent resin, with pure water wash away sugar and other water-solubility impurities after, re-use concentration of volume percent and be 10～100% ethanol-water solution and carry out gradient elution, concentrate, regulating concentrate eluant pH value with aqueous slkali is alkalescence, use the extractant of 1～3 times of volume to extract 1～4 time, collect the buck layer, again the gained aqueous slkali is transferred to acidity with the pH conditioning agent, and then go up step gained acid solution with the extractant extraction, wash with water to neutrality, concentrate, vacuum drying gets general flavone.The collected volume percent concentration is 50～100% eluent, re-uses the ethyl acetate extraction 1～3 time of 1～3 times of volume, concentrate, freeze drying, anthocyanidin.
The concrete grammar of sugar-cane juice raw material lixiviate is that discarded object sugarcane toppers or bagasse with the sugar industry after pulverizing are raw material in the said method, to use concentration of volume percent be 60～95% solvent extracts each 1～3 hour 2～4 times with the solid-liquid ratio of 1:5～1:15 (mass volume ratio).
The concrete grammar of leaching liquor column chromatography is by being filled with the chromatographic column of macroporous absorbent resin with leaching liquor in the said method, with pure water wash away sugar and other water-solubility impurities after, the ethanol-water solution that re-uses concentration of volume percent 10～100% carries out gradient elution, the collected volume percent concentration is 50～100% eluent, after concentrating through reducing pressure, the pH value of regulating concentrate eluant with aqueous slkali is 8～12, use the extractant of 1～3 times of volume to extract 1～4 time, collect the buck layer, again aqueous slkali being regulated its pH value with the pH conditioning agent is 3～6, extractant with 1～3 times of volume extracts acid solution 2～4 times, wash with water again to neutrality, after reduction vaporization concentrates then, vacuum drying, through high-performance liquid chromatogram determination, promptly get the general flavone amount and count 0.28～1.3mg/g based on sugarcane raw material (moisture sugarcane toppers or slag after the squeezing).
The concrete grammar of leaching liquor column chromatography is by being filled with the chromatographic column of macroporous absorbent resin with leaching liquor in the said method, with pure water wash away sugar and other water-solubility impurities after, re-use the ethanol-water solution gradient elution of concentration of volume percent 10～100%, the collected volume percent concentration is 10～40% eluent, re-use the ethyl acetate extraction 1～3 time of 1～3 times of volume, after reduction vaporization concentrates, vacuum drying, through high-performance liquid chromatogram determination, promptly get the anthocyanidin amount and count 0.053～0.63mg/g based on sugarcane raw material (moisture sugarcane toppers or slag), purity is 60～85%.
Used solvent is ethanol-water solution or methanol-water solution in general flavone, the anthocyanidin raw material leaching process, and extracting mode is that ultrasonic extraction or infusion process are extracted or percolation extracts.The used pH conditioning agent of its leaching liquor column chromatography purification process is hydrochloric acid or acid or glacial acetic acid or phosphoric acid or sulfuric acid, aqueous slkali is NaOH or potassium hydroxide or sodium carbonate or sodium bicarbonate solution, used macroporous absorbent resin is D101 or D301 or AB-8 or D100 or D141 type macroporous absorbent resin, and extractant is ethyl acetate or n-butanol.
Compared with the prior art the present invention has the following advantages:
1, because integrated extraction technique provided by the invention can all extract two kinds of main oxidation-resistant active ingredients in sugarcane toppers or the slag, and methodological science is efficient, and is with strong points, resource utilization significantly improves.
2, since the present invention to adopt the sugarcane trade waste be raw material, raw material sources are abundant, and are cheap, renewable is strong, production cost is low, does not influence the carrying out of original sugaring operation.
3, because product of the present invention is taken from natural plants, have no side effect substantially, can be used as in medicine or food or the cosmetic additive agent, security is good, has very high development and application values.
4, because the present invention adopts the sugar industry waste products, not only significantly reduce environmental pollution, made resource obtain more making full use of, also increased the industry added value.
5,, the comprehensive utilizating research of later cane sugar manufacture industrial product high added value composition is laid the foundation because the present invention sets up from the sugar industry waste products the comprehensive method of extracting multiple oxidation-resistant active ingredient first.
6, because the present invention adopts is to extract or the purifying mode all is comparatively ripe, whole in addition technical process mild condition, each process procedure solvent for use is recyclable, thereby it is simple to operate, be easy to control, production cost is low, not only meets the resource that makes full use of that country vigorously advocates, the recycling economy that reduces environmental pollution requires and the Scientific Outlook on Development, and helps realizing suitability for industrialized production.
The specific embodiment
Below by embodiment the present invention is specifically described; be necessary to be pointed out that at this following examples only are used for that the invention will be further described; can not be interpreted as limiting the scope of the invention; the person skilled in the art in this field makes some nonessential improvement and adjustment according to the invention described above content to the present invention, still belongs to protection domain of the present invention.
Embodiment 1
The ethanol of the use of the sugarcane toppers raw material 100g after the chopping 60% is extracted each 1 hour 2 times with the solid-liquid ratio infusion process of 1:15 (mass volume ratio).Then with the raw material extract by being filled with the chromatographic column of D101 type macroporous absorbent resin, wash away sugar and other water-solubility impurities with pure water after, re-use concentration of volume percent and be 10～100% ethanol water and carry out gradient elution.The collected volume percent concentration is 60% eluent, concentrate, the pH value of using sodium hydroxide solution to regulate concentrate eluant is 10, the ethyl acetate extraction of 3 times of volumes of use 2 times, it is 6 that the sodium hydroxide solution part is adjusted to the pH value with hydrochloric acid, and then with the ethyl acetate extraction of 3 times of volumes 2 times, wash with water to neutrality, after reduction vaporization concentrates then, freeze drying, through high-performance liquid chromatogram determination, calculate acquisition general flavone amount and count 1.0mg/g based on sugarcane raw material (the moisture sugarcane toppers after the squeezing).The collected volume percent concentration is 30% eluent, re-uses the ethyl acetate extraction 3 times of 2 times of volumes, concentrates, freeze drying, through high-performance liquid chromatogram determination, promptly get the anthocyanidin amount and count 0.58mg/g based on sugarcane raw material (moisture sugarcane toppers), purity is 85%.
Embodiment 2
Use 60% methyl alcohol with the ultrasonic lixiviate of the solid-liquid ratio of 1:6 (mass volume ratio) 4 times, each 1 hour the bagasse raw material 100g after squeezing.Then with the raw material extract by being filled with the chromatographic column of D301 type macroporous absorbent resin, wash away sugar and other water-solubility impurities with pure water after, re-use concentration of volume percent and be 10～100% ethanol water and carry out gradient elution.The collected volume percent concentration is 70% eluent, concentrate, the pH value of using potassium hydroxide solution to regulate concentrate eluant is 9, the extracting n-butyl alcohol of 1 times of volume of use 2 times, it is 5 that the potassium hydroxide solution part is adjusted to the pH value with acetic acid, and then with the extracting n-butyl alcohol of 2 times of volumes 3 times, wash with water to neutrality, after reduction vaporization concentrates then, freeze drying, through high-performance liquid chromatogram determination, calculate acquisition general flavone amount and count 0.28mg/g based on sugarcane raw material (the moisture bagasse after the squeezing).The collected volume percent concentration is 40% eluent, re-uses the ethyl acetate extraction 1 time of 3 times of volumes, concentrates, freeze drying, through high-performance liquid chromatogram determination, promptly get the anthocyanidin amount and count 0.054mg/g based on sugarcane raw material (moisture bagasse), purity is 75%.
Embodiment 3
Sugarcane toppers raw material 100g after the chopping used 80% ethanol extract each 1 hour 3 times with the solid-liquid ratio percolation of 1:8 (mass volume ratio).Then with the raw material extract by being filled with the chromatographic column of AB-8 type macroporous absorbent resin, wash away sugar and other water-solubility impurities with pure water after, re-use concentration of volume percent and be 10～100% ethanol water and carry out gradient elution.The collected volume percent concentration is 80% eluent, concentrate, the pH value of using sodium carbonate liquor to regulate concentrate eluant is 9, the extracting n-butyl alcohol of 2 times of volumes of use 3 times, it is 4 that the sodium carbonate liquor part is adjusted to the pH value with formic acid, and then with the ethyl acetate extraction of 1 times of volume 4 times, wash with water to neutrality, after reduction vaporization concentrates then, freeze drying, through high-performance liquid chromatogram determination, calculate acquisition general flavone amount and count 1.1mg/g based on sugarcane raw material (the moisture sugarcane toppers after the squeezing).The collected volume percent concentration is 30% eluent, re-uses the ethyl acetate extraction 2 times of 1 times of volume, concentrates, freeze drying, through high-performance liquid chromatogram determination, promptly get the anthocyanidin amount and count 0.59mg/g based on sugarcane raw material (moisture sugarcane toppers), purity is 80%.
Embodiment 4
The ethanol of the use of the bagasse raw material 100g after squeezing 70% is extracted each 1 hour 4 times with the solid-liquid ratio infusion process of 1:9 (mass volume ratio).Then with the raw material extract by being filled with the chromatographic column of D100 type macroporous absorbent resin, wash away sugar and other water-solubility impurities with pure water after, re-use concentration of volume percent and be 10～100% ethanol water and carry out gradient elution.The collected volume percent concentration is 90% eluent, concentrate, the pH value of using sodium bicarbonate solution to regulate concentrate eluant is 8, the ethyl acetate extraction of 2 times of volumes of use 4 times, it is 3 that the sodium bicarbonate solution part is adjusted to the pH value with phosphoric acid, and then with the extracting n-butyl alcohol of 1 times of volume 4 times, wash with water to neutrality, after reduction vaporization concentrates then, freeze drying, through high-performance liquid chromatogram determination, calculate acquisition general flavone amount and count 0.3mg/g based on sugarcane raw material (the moisture bagasse after the squeezing).The collected volume percent concentration is 40% eluent, re-uses the ethyl acetate extraction 3 times of 2 times of volumes, concentrates, freeze drying, through high-performance liquid chromatogram determination, promptly get the anthocyanidin amount and count 0.058mg/g based on sugarcane raw material (moisture bagasse), purity is 70%.
Embodiment 5
Use 80% methyl alcohol with the ultrasonic lixiviate of the solid-liquid ratio of 1:11 (mass volume ratio) 2 times, each 2 hours the sugarcane toppers raw material 100g after the chopping.Then with the raw material extract by being filled with the chromatographic column of D141 type macroporous absorbent resin, wash away sugar and other water-solubility impurities with pure water after, re-use concentration of volume percent and be 10～100% ethanol water and carry out gradient elution.The collected volume percent concentration is 100% eluent, concentrate, the pH value of using sodium hydroxide solution to regulate concentrate eluant is 12, the extracting n-butyl alcohol of 3 times of volumes of use 4 times, it is 5 that the sodium hydroxide solution part is adjusted to the pH value with sulfuric acid, and then with the extracting n-butyl alcohol of 2 times of volumes 3 times, wash with water to neutrality, after reduction vaporization concentrates then, freeze drying, through high-performance liquid chromatogram determination, calculate acquisition general flavone amount and count 1.2mg/g based on sugarcane raw material (the moisture sugarcane toppers after the squeezing).The collected volume percent concentration is 30% eluent, re-uses the ethyl acetate extraction 1 time of 3 times of volumes, concentrates, freeze drying, through high-performance liquid chromatogram determination, promptly get the anthocyanidin amount and count 0.63mg/g based on sugarcane raw material (moisture sugarcane toppers), purity is 75%.
Embodiment 6
Use 90% methyl alcohol with the ultrasonic lixiviate of the solid-liquid ratio of 1:13 (mass volume ratio) 3 times, each 2 hours the bagasse raw material 100g after squeezing.Then with the raw material extract by being filled with the chromatographic column of D141 type macroporous absorbent resin, wash away sugar and other water-solubility impurities with pure water after, re-use concentration of volume percent and be 10～100% ethanol water and carry out gradient elution.The collected volume percent concentration is 60% eluent, concentrate, the pH value of using potassium hydroxide solution to regulate concentrate eluant is 11, the extracting n-butyl alcohol of 1 times of volume of use 3 times, it is 6 that the potassium hydroxide solution part is adjusted to the pH value with sulfuric acid, and then with the ethyl acetate extraction of 3 times of volumes 2 times, wash with water to neutrality, after reduction vaporization concentrates then, freeze drying, through high-performance liquid chromatogram determination, calculate acquisition general flavone amount and count 0.32mg/g based on sugarcane raw material (the moisture bagasse after the squeezing).The collected volume percent concentration is 20% eluent, re-uses the ethyl acetate extraction 2 times of 1 times of volume, concentrates, freeze drying, through high-performance liquid chromatogram determination, promptly get the anthocyanidin amount and count 0.055mg/g based on sugarcane raw material (moisture bagasse), purity is 65%.
Embodiment 7
The ethanol of the use of the sugarcane toppers raw material 100g after the chopping 95% is extracted each 2 hours 2 times with the solid-liquid ratio infusion process of 1:12 (mass volume ratio).Then with the raw material extract by being filled with the chromatographic column of D100 type macroporous absorbent resin, wash away sugar and other water-solubility impurities with pure water after, re-use concentration of volume percent and be 10～100% ethanol water and carry out gradient elution.The collected volume percent concentration is 70% eluent, concentrate, the pH value of using sodium carbonate liquor to regulate concentrate eluant is 8, the ethyl acetate extraction of 1 times of volume of use 2 times, it is 3 that the sodium carbonate liquor part is adjusted to the pH value with phosphoric acid, and then with the extracting n-butyl alcohol of 2 times of volumes 3 times, wash with water to neutrality, after reduction vaporization concentrates then, freeze drying, through high-performance liquid chromatogram determination, calculate acquisition general flavone amount and count 1.3mg/g based on sugarcane raw material (the moisture sugarcane toppers after the squeezing).The collected volume percent concentration is 10% eluent, re-uses the ethyl acetate extraction 3 times of 2 times of volumes, concentrates, freeze drying, through high-performance liquid chromatogram determination, promptly get the anthocyanidin amount and count 0.60mg/g based on sugarcane raw material (moisture sugarcane toppers), purity is 60%.
Embodiment 8
Bagasse raw material 100g after squeezing used 80% ethanol extract each 1 hour 3 times with the solid-liquid ratio percolation of 1:10 (mass volume ratio).Then with the raw material extract by being filled with the chromatographic column of AB-8 type macroporous absorbent resin, wash away sugar and other water-solubility impurities with pure water after, re-use concentration of volume percent and be 10～100% ethanol water and carry out gradient elution.The collected volume percent concentration is 80% eluent, concentrate, the pH value of using sodium bicarbonate solution to regulate concentrate eluant is 9, the ethyl acetate extraction of 2 times of volumes of use 1 time, it is 4 that the sodium bicarbonate solution part is adjusted to the pH value with formic acid, and then with the ethyl acetate extraction of 3 times of volumes 4 times, wash with water to neutrality, after reduction vaporization concentrates then, freeze drying, through high-performance liquid chromatogram determination, calculate acquisition general flavone amount and count 0.31mg/g based on sugarcane raw material (the moisture bagasse after the squeezing).The collected volume percent concentration is 20% eluent, re-uses the ethyl acetate extraction 1 time of 3 times of volumes, concentrates, freeze drying, through high-performance liquid chromatogram determination, promptly get the anthocyanidin amount and count 0.056mg/g based on sugarcane raw material (moisture bagasse), purity is 70%.
Embodiment 9
Use 70% methyl alcohol with the ultrasonic lixiviate of the solid-liquid ratio of 1:7 (mass volume ratio) 4 times, each 1 hour the sugarcane toppers raw material 100g after the chopping.Then with the raw material extract by being filled with the chromatographic column of D301 type macroporous absorbent resin, wash away sugar and other water-solubility impurities with pure water after, re-use concentration of volume percent and be 10～100% ethanol water and carry out gradient elution.The collected volume percent concentration is 90% eluent, concentrate, the pH value of using sodium hydroxide solution to regulate concentrate eluant is 9, the ethyl acetate extraction of 3 times of volumes of use 3 times, it is 5 that the sodium hydroxide solution part is adjusted to the pH value with acetic acid, and then with the ethyl acetate extraction of 1 times of volume 2 times, wash with water to neutrality, after reduction vaporization concentrates then, freeze drying, through high-performance liquid chromatogram determination, calculate acquisition general flavone amount and count 1.0mg/g based on sugarcane raw material (the moisture sugarcane toppers after the squeezing).The collected volume percent concentration is 30% eluent, re-uses the ethyl acetate extraction 2 times of 1 times of volume, concentrates, freeze drying, through high-performance liquid chromatogram determination, promptly get the anthocyanidin amount and count 0.61mg/g based on sugarcane raw material (moisture sugarcane toppers), purity is 80%.
Embodiment 10
The methyl alcohol of the use of the bagasse raw material 100g after squeezing 95% is extracted each 2 hours 2 times with the solid-liquid ratio infusion process of 1:5 (mass volume ratio).Then with the raw material extract by being filled with the chromatographic column of D101 type macroporous absorbent resin, wash away sugar and other water-solubility impurities with pure water after, re-use concentration of volume percent and be 10～100% ethanol water and carry out gradient elution.The collected volume percent concentration is 100% eluent, concentrate, the pH value of using potassium hydroxide solution to regulate concentrate eluant is 10, the extracting n-butyl alcohol of 1 times of volume of use 2 times, it is 6 that the potassium hydroxide solution part is adjusted to the pH value with hydrochloric acid, and then with the ethyl acetate extraction of 2 times of volumes 3 times, wash with water to neutrality, after reduction vaporization concentrates then, freeze drying, through high-performance liquid chromatogram determination, calculate acquisition general flavone amount and count 0.29mg/g based on sugarcane raw material (the moisture bagasse after the squeezing).The collected volume percent concentration is 40% eluent, re-uses the ethyl acetate extraction 3 times of 2 times of volumes, concentrates, freeze drying, through high-performance liquid chromatogram determination, promptly get the anthocyanidin amount and count 0.053mg/g based on sugarcane raw material (moisture bagasse), purity is 65%.
Embodiment 11
Sugarcane toppers raw material 100g after the chopping used 60% ethanol extract each 1 hour 4 times with the solid-liquid ratio percolation of 1:14 (mass volume ratio).Then with the raw material extract by being filled with the chromatographic column of D301 type macroporous absorbent resin, wash away sugar and other water-solubility impurities with pure water after, re-use concentration of volume percent and be 10～100% ethanol water and carry out gradient elution.The collected volume percent concentration is 60% eluent, concentrate, the pH value of using sodium hydroxide solution to regulate concentrate eluant is 8, the ethyl acetate extraction of 2 times of volumes of use 3 times, it is 5 that the sodium hydroxide solution part is adjusted to the pH value with acetic acid, and then with the ethyl acetate extraction of 2 times of volumes 2 times, wash with water to neutrality, after reduction vaporization concentrates then, freeze drying, through high-performance liquid chromatogram determination, calculate acquisition general flavone amount and count 1.2mg/g based on sugarcane raw material (the moisture sugarcane toppers after the squeezing).The collected volume percent concentration is 20% eluent, re-uses the ethyl acetate extraction 1 time of 3 times of volumes, concentrates, freeze drying, through high-performance liquid chromatogram determination, promptly get the anthocyanidin amount and count 0.62mg/g based on sugarcane raw material (moisture sugarcane toppers), purity is 75%.
Embodiment 12
Bagasse raw material 100g after squeezing used 90% ethanol extract each 2 hours 3 times with the solid-liquid ratio percolation of 1:5 (mass volume ratio).Then with the raw material extract by being filled with the chromatographic column of D101 type macroporous absorbent resin, wash away sugar and other water-solubility impurities with pure water after, re-use concentration of volume percent and be 10～100% ethanol water and carry out gradient elution.The collected volume percent concentration is 100% eluent, concentrate, the pH value of using potassium hydroxide solution to regulate concentrate eluant is 12, the extracting n-butyl alcohol of 3 times of volumes of use 2 times, it is 4 that the potassium hydroxide solution part is adjusted to the pH value with hydrochloric acid, and then with the ethyl acetate extraction of 2 times of volumes 3 times, wash with water to neutrality, after reduction vaporization concentrates then, freeze drying, through high-performance liquid chromatogram determination, calculate acquisition general flavone amount and count 0.28mg/g based on sugarcane raw material (the moisture bagasse after the squeezing).The collected volume percent concentration is 30% eluent, re-uses the ethyl acetate extraction 2 times of 1 times of volume, concentrates, freeze drying, through high-performance liquid chromatogram determination, promptly get the anthocyanidin amount and count 0.054mg/g based on sugarcane raw material (moisture bagasse), purity is 85%.
Claims (9)
1, anti-oxidation active substance (general flavone in a kind of comprehensive extraction separation of sugarcane tip or the bagasse, anthocyanidin) method, it is characterized in that this method is earlier with sugarcane toppers or bagasse raw material pulverizing, lixiviate, then with leaching liquor by being filled with the chromatographic column of macroporous absorbent resin, with pure water wash away sugar and other water-solubility impurities after, re-use concentration of volume percent and be 10～100% ethanol-water solution and carry out gradient elution, the ethanol water elution liquid of collecting the high concentration section concentrates the crude extract that obtains being rich in flavones, the ethanol water elution liquid of collecting the low concentration section concentrates the crude extract that obtains being rich in anthocyanidin, again above two kinds of crude extracts are adopted soda acid facture and the further enrichment of solvent extraction respectively, purifying, concentrate, after the vacuum drying, obtain general flavone and anthocyanidin respectively.
2. raw material extracting method according to claim 1, it is characterized in that in this method that with sugar industry discarded object sugarcane toppers or bagasse after pulverizing be raw material, to use concentration of volume percent be 60～95% solvent extracts 2～4 times with the solid-liquid ratio of 1:5～1:15 (mass volume ratio), each 1～3 hour, extract merges, and (pressure＜0.09MPa) concentrates and obtains the raw material extract in decompression.
3, method according to claim 1, the concrete grammar that it is characterized in that the extract column chromatography is by being filled with the chromatographic column of macroporous absorbent resin with leaching liquor, with pure water wash away sugar and other water-solubility impurities after, re-use concentration of volume percent and be 10～100% ethanol water and carry out gradient elution, the collected volume percent concentration is 10～40% eluent, slowly use the ethyl acetate extraction 1～3 time of 1～3 times of volume, (pressure＜0.09MPa) concentrate gets anthocyanidin after the freeze drying in decompression.
4, method according to claim 1, the concrete grammar that it is characterized in that the extract column chromatography is by being filled with the chromatographic column of macroporous absorbent resin with leaching liquor, with pure water wash away sugar and other water-solubility impurities after, re-use concentration of volume percent and be 10～100% ethanol water and carry out gradient elution, the collected volume percent concentration is 50～100% eluent, through decompression (after pressure＜0.09MPa) concentrates, the pH value of using aqueous slkali to regulate concentrate eluant is 8～12, extractant with 1～3 times of volume extracts 1～4 time again, collect the buck layer, regulating aqueous slkali pH value with the pH conditioning agent then is 3～6, extractant with 1～3 times of volume extracts acid solution 2～4 times at last, merges repeatedly extract, washes with water to neutrality again, concentrate, get general flavone after the vacuum drying.
5, method according to claim 2 is characterized in that used solvent is ethanol-water solution or methanol-water solution, and extracting mode is that ultrasonic extraction or infusion process are extracted or percolation extracts.
6, method according to claim 3 is characterized in that macroporous absorbent resin used in this method is D101 type or D301 type or AB-8 type or D100 type or D141 type macroporous absorbent resin.
7, method according to claim 4, it is characterized in that used extractant is ethyl acetate or n-butanol in this method, aqueous slkali is NaOH or potassium hydroxide or sodium carbonate or sodium bicarbonate solution, and the pH conditioning agent is hydrochloric acid or acetic acid or sulfuric acid or formic acid or phosphoric acid.
8, method according to claim 3 is characterized in that the productive rate in moisture sugarcane toppers or slag weight anthocyanidin is 0.053～0.63mg/g, and purity is 60～85%.
9, method according to claim 4 is characterized in that the productive rate in sugarcane toppers or slag weight general flavone is 0.28～1.3mg/g.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102409572A (en) * | 2011-09-14 | 2012-04-11 | 四川大学 | New environmentally-friendly process for synthetically separating lignocellulose from bagasse |
| CN103149282A (en) * | 2013-01-16 | 2013-06-12 | 广西中医药大学 | Sugarcane top qualitative identification high performance liquid chromatography (HPLC) fingerprint spectrum detection method |
| CN104957602A (en) * | 2015-05-22 | 2015-10-07 | 长沙普源生物科技有限公司 | Sugarcane bioactive component composition, functional health food, and preparation method of sugarcane bioactive component composition and functional health food |
| WO2018133600A1 (en) * | 2017-01-19 | 2018-07-26 | 华南理工大学 | Method for preparing high-activity sugarcane anthocyanin |
| CN109705081A (en) * | 2019-01-20 | 2019-05-03 | 林燕 | A method of extracting anthocyanidin from sugarcane pericarp |
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| CN1814695A (en) * | 2006-01-13 | 2006-08-09 | 暨南大学 | Method fox extracting sugar-cane-leaf oxidation-resisting matter and use thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102409572A (en) * | 2011-09-14 | 2012-04-11 | 四川大学 | New environmentally-friendly process for synthetically separating lignocellulose from bagasse |
| CN102409572B (en) * | 2011-09-14 | 2014-08-13 | 四川大学 | New environmentally-friendly process for synthetically separating lignocellulose from bagasse |
| CN103149282A (en) * | 2013-01-16 | 2013-06-12 | 广西中医药大学 | Sugarcane top qualitative identification high performance liquid chromatography (HPLC) fingerprint spectrum detection method |
| CN104957602A (en) * | 2015-05-22 | 2015-10-07 | 长沙普源生物科技有限公司 | Sugarcane bioactive component composition, functional health food, and preparation method of sugarcane bioactive component composition and functional health food |
| CN104957602B (en) * | 2015-05-22 | 2018-06-19 | 长沙普源生物科技有限公司 | Sugarcane active component composition and functional health-care food and preparation method thereof |
| WO2018133600A1 (en) * | 2017-01-19 | 2018-07-26 | 华南理工大学 | Method for preparing high-activity sugarcane anthocyanin |
| CN109705081A (en) * | 2019-01-20 | 2019-05-03 | 林燕 | A method of extracting anthocyanidin from sugarcane pericarp |
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