CN103159810A - Method for preparing polysaccharide saponins by taking synurus deltoides as raw material - Google Patents
Method for preparing polysaccharide saponins by taking synurus deltoides as raw material Download PDFInfo
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Abstract
The invention relates to a preparation method of polysaccharide saponins, and concretely relates to a method for preparing polysaccharide saponins by taking synurus deltoides as a raw material through steps of biotransformation, polysaccharide saponins extraction and membrane filtration, the preparation method comprises four phases: a raw material processing phase, a biotransformation and extraction phase, a separation phase and a chromatogram separating phase; an air-flow crushing technology is selected to prepare the synurus deltoides super fine micro powder, the crushing technology parameter can be determined, the minimum average particle size of the micro powder can be processed to less than 0.2 micrometers; synurus deltoides polysaccharide is performed with crude separation, a supersonic wave water extraction method is used for a preliminary research of polysaccharide extraction, the recovery rate of the effective composition can be increased by about 10%, the purity can reach more than 65%; the high efficiency liquid phase detection method and thin layer detection method suitable for industrial chromatogram separation of the synurus deltoides saponins monomer compounds can be established, and the batch preparation of the products can be realized.
Description
Technical field
The present invention relates to a kind of preparation method of polysaccharide saponin, specifically relate to a kind of method for preparing polysaccharide saponin take Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) as raw material.
Background technology
Along with the raising of people's living standard, people are also become increasingly abundant to the pursuit of nutritive value, health care and the pharmaceutical use of product, so the space, consumption market that safe and reliable vegetable food product nutrition is taken in is extremely huge.The effective ingredient of extracting from the natural product Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae)---polysaccharide, saponin fine chemicals, medicine, healthcare products raw material had both been can be used as, can be used for medicine, the healthcare products production of antifatigue, anti-ageing and brain tonic, as Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) polysaccharide and saponin capsule, tablet or oral liquid etc.; Also can be applicable to the cosmetics industry, can be mixed with the makeup of nti-freckle, minimizing wrinkle, activation skin cells, enhancing skin elasticity; Can also be used as the luxury food additive, of many uses, so market outlook are wide.At present, China's Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) product also only rests on the simple preliminary working level such as salt marsh, chopping, and added value of product is not high, has seriously restricted the development of Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) plant husbandry.
Summary of the invention
Problem in view of prior art exists the objective of the invention is to provide a kind of take Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) as raw material, prepares the method for polysaccharide saponin by steps such as bio-transformation, polysaccharide saponin lixiviate and membrane filtrations.
To achieve these goals, the technical solution adopted in the present invention is a kind of method for preparing polysaccharide take Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) as raw material, and it comprises four-stage, is respectively: the treatment stage of raw material, bio-transformation and extraction stage, separation phase and chromatographic separation stage;
The process treatment stage of described raw material is:
1) Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) of choosing is cleaned with clear water;
2) the Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) micronizing after cleaning: utilize planet ball shredder that Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) is pulverized, and adopt airflow pulverization; Described planet ball shredder rotating speed is 270 ~ 280r/min, and milling time is 80 ~ 90min, and charge ratio of media is 10 ~ 15%, is 10 ~ 15% by the comminuting matter filling ratio;
Described bio-transformation and extraction stage adopt enzyme that the raw material after processing is transformed; Adopt the ultrasonic wave water extraction; Described bio-transformation and extraction stage adopt enzyme that the raw material after processing is transformed; Adopt the ultrasonic wave water extraction; The condition of described ultrasonic extraction is: solid-liquid ratio is 1:15, and the time is 10 ~ 20min, and temperature is 50 ~ 70 ℃, power 400 ~ 450W;
The process of described separation phase is:
1), membrane filtration, remove impurity;
2), to select macroporous resin be 6 ~ 7 in the pH value, temperature is to carry out under 30 ~ 40 conditions separating on post;
Described chromatographic separation stage it adopt industrial chromatography to separate, it is take Arctiin, aretigenin as testing index, measured the content of Arctiin and aretigenin in the extract; Chromatographic column is KromasilC18100A (150mm * 4.6mm, 5 μ m); Moving phase: methanol-water (employing gradient elution mode: 0～7min, 35%～45% methyl alcohol; 7～9min, 45%～48% methyl alcohol; 9～15min, 48%～53% methyl alcohol; 15～24min, 53%～80% methyl alcohol; 24～30min, 80%～100% methyl alcohol); The detection wavelength is 280nm, and the average recovery rate of Arctiin and aretigenin is respectively 97.7%, 96.9%; RSD is respectively 1.3%, 0.9% (n=5); Linear equation is respectively:
Y=782.6X-64.11(r=0.9998)，Y=1220.217X-35.26(r=0.9998)。
A kind of method for preparing saponin take Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) as raw material, its process comprises four-stage for it, is respectively: the treatment stage of raw material, bio-transformation and extraction stage, separation phase and chromatographic separation stage;
The process treatment stage of described raw material is:
1) the Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) raw material of select;
2) Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) of choosing is cleaned with clear water;
3) the Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) micronizing after cleaning: utilize planet ball shredder that Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) is pulverized, and adopt airflow pulverization; Described planet ball shredder rotating speed is 270 ~ 280r/min, and milling time is 80 ~ 90min, and charge ratio of media is 10 ~ 15%, is 10 ~ 15% by the comminuting matter filling ratio;
Described bio-transformation and extraction stage adopt enzyme that the raw material after processing is transformed; Adopt the ultrasonic wave water extraction; Described ultrasonic extraction is starved condition: solid-liquid ratio is 1:15, and the time is 10 ~ 20min, and temperature is 50 ~ 70 ℃, power 400 ~ 450W;
Described chromatographic separation stage it adopt industrial chromatography to separate, it is take Arctiin, aretigenin as testing index, measured the content of Arctiin and aretigenin in the extract; Chromatographic column is KromasilC18100A (150mm * 4.6mm, 5 μ m); Moving phase: methanol-water (employing gradient elution mode: 0～7min, 35%～45% methyl alcohol; 7～9min, 45%～48% methyl alcohol; 9～15min, 48%～53% methyl alcohol; 15～24min, 53%～80% methyl alcohol; 24～30min, 80%～100% methyl alcohol); The detection wavelength is 280nm, and the average recovery rate of Arctiin and aretigenin is respectively 97.7%, 96.9%.RSD is respectively 1.3%, 0.9% (n=5); Linear equation is respectively:
Y=782.6X-64.11(r=0.9998)，Y=1220.217X-35.26(r=0.9998；
It is characterized in that: the process of described separation phase is:
1), membrane filtration, remove impurity;
2), to select silica gel, C18, sephedax be filler, is 6 ~ 7 in the pH value, temperature is to carry out under 30 ~ 40 conditions separating on post.
The invention has the advantages that: the choice for use airflow pulverization has been made the Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) ultra-fine micropowder, has determined the crushing technology parameter, and the micro mist minimum average particle diameters can be processed less than 0.2 micron; The roughing out of Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) polysaccharide: utilize the ultrasonic wave water extraction method to do preliminary study to the extraction of polysaccharide, the extraction yield of effective ingredient can improve approximately 10%, and purity reaches more than 65%; Set up and be applicable to industrial chromatography and separate the high performance liquid phase detection method of Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) saponin class monomeric compound and the detection method of thin layer, realized that product is carried out batch to be prepared.
Embodiment
Embodiment 1
A kind of method for preparing polysaccharide take Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) as raw material, it comprises four-stage, is respectively: the treatment stage of raw material, bio-transformation and extraction stage, separation phase and chromatographic separation stage;
The process treatment stage of described raw material is:
3) Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) of choosing is cleaned with clear water;
4) the Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) micronizing after cleaning: utilize planet ball shredder that Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) is pulverized, and adopt airflow pulverization; Described planet ball shredder rotating speed is 272r/min, and milling time is 85min, and charge ratio of media is 12%, is 13% by the comminuting matter filling ratio;
Described bio-transformation and extraction stage adopt enzyme that the raw material after processing is transformed; Adopt the ultrasonic wave water extraction; Described bio-transformation and extraction stage adopt enzyme that the raw material after processing is transformed; Adopt the ultrasonic wave water extraction; Described ultrasonic extraction is starved condition: solid-liquid ratio is 1:15, and the time is 15min, and temperature is 60 ℃, power 420W;
The process of described separation phase is:
3), membrane filtration, remove impurity;
4), to select macroporous resin be 6.5 in the pH value, temperature is to carry out under 35 conditions separating on post;
Described chromatographic separation stage it adopt industrial chromatography to separate, it is take Arctiin, aretigenin as testing index, measured the content of Arctiin and aretigenin in the extract; Chromatographic column is KromasilC18100A (150mm * 4.6mm, 5 μ m); Moving phase: methanol-water (employing gradient elution mode: 0～7min, 35%～45% methyl alcohol; 7～9min, 45%～48% methyl alcohol; 9～15min, 48%～53% methyl alcohol; 15～24min, 53%～80% methyl alcohol; 24～30min, 80%～100% methyl alcohol); The detection wavelength is 280nm, and the average recovery rate of Arctiin and aretigenin is respectively 97.7%, 96.9%; RSD is respectively 1.3%, 0.9% (n=5); Linear equation is respectively:
Y=782.6X-64.11(r=0.9998)，Y=1220.217X-35.26(r=0.9998)。
Embodiment 2
A kind of method for preparing saponin take Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) as raw material, its process comprises four-stage, is respectively: the treatment stage of raw material, bio-transformation and extraction stage, separation phase and chromatographic separation stage;
The process treatment stage of described raw material is:
1) the Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) raw material of select;
2) Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) of choosing is cleaned with clear water;
3) the Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) micronizing after cleaning: utilize planet ball shredder that Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) is pulverized, and adopt airflow pulverization; Described planet ball shredder rotating speed is 272r/min, and milling time is 85min, and charge ratio of media is 12%, is 13% by the comminuting matter filling ratio;
Described bio-transformation and extraction stage adopt enzyme that the raw material after processing is transformed; Adopt the ultrasonic wave water extraction; The condition of described ultrasonic extraction is: solid-liquid ratio is 1:15, and the time is 18min, and temperature is 65 ℃, power 430W;
Described chromatographic separation stage it adopt industrial chromatography to separate, it is take Arctiin, aretigenin as testing index, measured the content of Arctiin and aretigenin in the extract; Chromatographic column is KromasilC18100A (150mm * 4.6mm, 5 μ m); Moving phase: methanol-water (employing gradient elution mode: 0～7min, 35%～45% methyl alcohol; 7～9min, 45%～48% methyl alcohol; 9～15min, 48%～53% methyl alcohol; 15～24min, 53%～80% methyl alcohol; 24～30min, 80%～100% methyl alcohol); The detection wavelength is 280nm, and the average recovery rate of Arctiin and aretigenin is respectively 97.7%, 96.9%.RSD is respectively 1.3%, 0.9% (n=5); Linear equation is respectively:
Y=782.6X-64.11(r=0.9998)，Y=1220.217X-35.26(r=0.9998）；
It is characterized in that: the process of described separation phase is:
1), membrane filtration, remove impurity;
2), to select silica gel, C18, sephedax be filler, is 6.5 in the pH value, temperature is to carry out separating on post under 35 ℃ of conditions.
Claims (2)
1. method for preparing polysaccharide take Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) as raw material, it comprises four-stage, is respectively: the treatment stage of raw material, bio-transformation and extraction stage, separation phase and chromatographic separation stage;
The process treatment stage of described raw material is:
1) Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) of choosing is cleaned with clear water;
2) the Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) micronizing after cleaning: utilize planet ball shredder that Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) is pulverized, and adopt airflow pulverization; Described planet ball shredder rotating speed is 270 ~ 280r/min, and milling time is 80 ~ 90min, and charge ratio of media is 10 ~ 15%, is 10 ~ 15% by the comminuting matter filling ratio;
Described bio-transformation and extraction stage adopt enzyme that the raw material after processing is transformed; Adopt the ultrasonic wave water extraction; Described bio-transformation and extraction stage adopt enzyme that the raw material after processing is transformed; Adopt the ultrasonic wave water extraction; The condition of described ultrasonic extraction is: solid-liquid ratio is 1:15, and the time is 10 ~ 20min, and temperature is 50 ~ 70 ℃, power 400 ~ 450W;
The process of described separation phase is:
1), membrane filtration, remove impurity;
2), to select macroporous resin be 6 ~ 7 in the pH value, temperature is to carry out under 30 ~ 40 conditions separating on post;
Described chromatographic separation stage it adopt industrial chromatography to separate, it is take Arctiin, aretigenin as testing index, measured the content of Arctiin and aretigenin in the extract; Chromatographic column is KromasilC18100A (150mm * 4.6mm, 5 μ m); Moving phase: methanol-water (employing gradient elution mode: 0～7min, 35%～45% methyl alcohol; 7～9min, 45%～48% methyl alcohol; 9～15min, 48%～53% methyl alcohol; 15～24min, 53%～80% methyl alcohol; 24～30min, 80%～100% methyl alcohol); The detection wavelength is 280nm, and the average recovery rate of Arctiin and aretigenin is respectively 97.7%, 96.9%; RSD is respectively 1.3%, 0.9% (n=5).
2. method for preparing saponin take Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) as raw material, its process comprises four-stage for it, is respectively: the treatment stage of raw material, bio-transformation and extraction stage, separation phase and chromatographic separation stage;
The process treatment stage of described raw material is:
1) the Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) raw material of select;
2) Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) of choosing is cleaned with clear water;
3) the Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) micronizing after cleaning: utilize planet ball shredder that Herba seu Radix Cirsii Japonici (Radix Saussureae cordifoliae) is pulverized, and adopt airflow pulverization; Described planet ball shredder rotating speed is 270 ~ 280r/min, and milling time is 80 ~ 90min, and charge ratio of media is 10 ~ 15%, is 10 ~ 15% by the comminuting matter filling ratio;
Described bio-transformation and extraction stage adopt enzyme that the raw material after processing is transformed; Adopt the ultrasonic wave water extraction; Described ultrasonic extraction is starved condition: solid-liquid ratio is 1:15, and the time is 10 ~ 20min, and temperature is 50 ~ 70 ℃, power 400 ~ 450W;
Described chromatographic separation stage it adopt industrial chromatography to separate, it is take Arctiin, aretigenin as testing index, measured the content of Arctiin and aretigenin in the extract; Chromatographic column is KromasilC18100A (150mm * 4.6mm, 5 μ m); Moving phase: methanol-water (employing gradient elution mode: 0～7min, 35%～45% methyl alcohol; 7～9min, 45%～48% methyl alcohol; 9～15min, 48%～53% methyl alcohol; 15～24min, 53%～80% methyl alcohol; 24～30min, 80%～100% methyl alcohol); The detection wavelength is 280nm, and the average recovery rate of Arctiin and aretigenin is respectively 97.7%, 96.9%.RSD is respectively 1.3%, 0.9% (n=5);
It is characterized in that: the process of described separation phase is:
1), membrane filtration, remove impurity;
2), to select silica gel, C18, sephedax be filler, is 6 ~ 7 in the pH value, temperature is to carry out under 30 ~ 40 conditions separating on post.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008290995A (en) * | 2007-05-28 | 2008-12-04 | Otaka Koso Kk | New oligosaccharide and its manufacturing method |
| CN101433568A (en) * | 2008-12-19 | 2009-05-20 | 陈靠山 | Extraction of burdock root aqueous extract and use |
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- 2013-03-07 CN CN2013100724935A patent/CN103159810A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008290995A (en) * | 2007-05-28 | 2008-12-04 | Otaka Koso Kk | New oligosaccharide and its manufacturing method |
| CN101433568A (en) * | 2008-12-19 | 2009-05-20 | 陈靠山 | Extraction of burdock root aqueous extract and use |
Non-Patent Citations (3)
| Title |
|---|
| 唐仕荣，等: "牛蒡多糖的超声波提取工艺及抗氧化性研究", 《食品工程》 * |
| 季志红，等: "大孔吸附树脂分离纯化毛头牛蒡子多糖的工艺研究", 《环球中医药》 * |
| 苗敬芝，等: "超声结合酶法提取牛蒡根多糖及抗氧化活性研究", 《食品工程》 * |
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Application publication date: 20130619 |