CN103041175B - One extracts alkaloidal method from Radix seu Herba Spiranthis Lanceae - Google Patents
One extracts alkaloidal method from Radix seu Herba Spiranthis Lanceae Download PDFInfo
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Abstract
The invention belongs to field of natural organic chemistry, relate to a kind of alkaloidal purification process, particularly relate to one and utilize the alkaloidal method of Radix seu Herba Spiranthis Lanceae in cellulase degradation and ultrasonic extraction and membrane separation technique coupling enriching and purifying Radix seu Herba Spiranthis Lanceae.The present invention adds the accessibility that zymolysis technique can increase enzyme-to-substrate, improves enzymatic hydrolyzation, utilizes ultrasonic extraction to accelerate rate of extraction, binding film isolation technics improves alkaloidal purity, combining of several technology greatly reduces extraction time, improves rate of extraction, shortens extracting cycle, safe and reliable, pollution-free, separating effect is obvious, and DNA purity is high, the alkaloid finished product of content more than 90% can be obtained, overcome the shortcoming that traditional extraction rate is relatively low, DNA purity is low.
Description
Technical field:
The invention belongs to field of natural organic chemistry, relate to a kind of alkaloidal purification process, particularly relate to one and utilize the alkaloidal method of Radix seu Herba Spiranthis Lanceae in cellulase degradation and ultrasonic extraction and membrane separation technique coupling enriching and purifying Radix seu Herba Spiranthis Lanceae.
Background technology:
Radix seu Herba Spiranthis Lanceae: Lu Shenglan is high 15 ~ 30 centimetres.Stem is upright, and base portion clusters, and several are slightly thick, the root of meat, raw 2 ~ 4 pieces of leaves of nearly base portion.Leaf wire falls lanceolar or linear, long 10 ~ 20 centimetres, wide 4 ~ 10 millimeters.Inflorescence top is raw, long 10 ~ 20 centimetres, and the little Hua of the most close life of tool, like spike; Floral white or pale red, arrange in the shape of a spiral; Petal sheet is avette, long gradually point; Middle sepal is linear, blunt, long 5 millimeters, wide 1.3 millimeters; Side sepal is isometric, but narrower; Petal and middle sepal isometric but thinner, top is extremely blunt; The nearly Long Circle of lip, long 4 ~ 5 millimeters, wide 2.5 millimeters, top is stretched, base portion to the full edge of center edge portion, the crisp grinding tooth that on middle part, tool is strong, the surperficial tool ripple shape more than middle part and long bristle, base portion slightly caves in, in shallow cryptomere, tool 2 pieces of projections in capsule.Flower, really 6 ~ August of phase.Aerial parts is containing coumarin glycoside and alkaloid.
Radix seu Herba Spiranthis Lanceae alkaloid is a kind of natural active matter human health being had to remarkable health-care effect, has caused the common concern of international community.Prove through scientific research and clinical practice, Radix seu Herba Spiranthis Lanceae alkaloid has anti-inflammatory analgetic, antibacterial, antiviral, anticancer, spasmolytic and improves Cardiovascular System, is a large class medicine of determined curative effect; It is found that containing a large amount of Radix seu Herba Spiranthis Lanceae alkaloids in natural plants Radix seu Herba Spiranthis Lanceae, because its raw material Radix seu Herba Spiranthis Lanceae is distributed more widely, therefrom extract Radix seu Herba Spiranthis Lanceae alkaloid and achieve encouraging progress.The alkaloidal method of current domestic extraction is water extraction method and organic solvent extraction mostly, leaching process is complicated, extraction time is long, Radix seu Herba Spiranthis Lanceae extract extraction process in patent of the present invention is mainly after acid soak, add cellulase, be aided with ultrasonic extraction again, obtain the effect be separated through membrane filtration process.
The invention has the advantages that application cellulase degradation and ultrasonic extraction and membrane separation technique coupling separation and purification Radix seu Herba Spiranthis Lanceae alkaloid, add the accessibility that zymolysis technique can increase enzyme-to-substrate, improve enzymatic hydrolyzation, ultrasonic extraction is utilized to accelerate rate of extraction, binding film isolation technics improves alkaloidal purity, combining of several technology greatly reduces extraction time, improve rate of extraction, shorten extracting cycle, safe and reliable, pollution-free, separating effect is obvious, DNA purity is high, the alkaloid finished product of content more than 90% can be obtained, overcome traditional extraction rate relatively low, the shortcoming that DNA purity is low.
Summary of the invention: the object of the invention is to overcome the shortcomings such as routine techniques extraction ratio is relatively low, DNA purity is low, provides one to utilize the alkaloidal method of Radix seu Herba Spiranthis Lanceae in cellulase degradation and ultrasonic extraction and membrane separation technique coupling enriching and purifying Radix seu Herba Spiranthis Lanceae.
For achieving the above object, the technical solution used in the present invention is:
One utilizes the alkaloidal method of Radix seu Herba Spiranthis Lanceae in cellulase degradation and ultrasonic extraction and membrane separation technique coupling enriching and purifying Radix seu Herba Spiranthis Lanceae, and its step is as follows:
(1) will do after Radix seu Herba Spiranthis Lanceae is pulverized and cross 40 ~ 80 mesh sieves, be the acid soak 30min of 1% by concentration, adjust ph is between 4.0 ~ 5.0, and enzyme addition is 2 ~ 4mg/g, enzymolysis time 1 ~ 2 hour, hydrolysis temperature 40 ~ 50 DEG C;
(2) material after (1) process is carried out ultrasonic extraction, solid-liquid ratio is 8 ~ 10 times that pulverize volume, and Extracting temperature is 40 ~ 60 DEG C, extract frequency 80 ~ 120Hz, extraction time 60min ~ 100min, extracts 2 times, merges extracted twice liquid;
(3) extracting solution 1mol/L hydrochloric acid is regulated pH value to 3.4 ~ 3.5, filtrate concentration is the alkali adjust ph to 11 of 50% by sucking filtration after 5 DEG C of cold preservation 48h, with the chloroform extraction 2 times with filtrate equivalent, combined chloroform liquid, reclaims chloroform, obtains alkaloid crude extract;
(4) extracting solution is retained relative molecular weight through ultrafiltration, temperature controls at 40 ~ 60 DEG C, and Stress control is at 0.6 ~ 2.2MPa;
(5) gained filtrate carries out nanofiltration operation again and retains relative molecular weight, and operative temperature controls at 40 ~ 60 DEG C, and Stress control is at 0.6 ~ 2.2MPa;
(6) concentrated under vacuum by filtering solution, concentrated Stress control is at 0.02 ~ 0.04MPa, and temperature controls at 50 ~ 60 DEG C, and proportion is 1.12 ~ 1.20, obtains alkaloid concentrated solution;
(7) dissolved through chloroform by gained alkaloid concentrated solution, by sodium hydroxide adjust ph to 11, be concentrated into 1/4 of original volume, leave standstill, crystallization obtains alkaloid crude product, and so repeatedly twice, obtain alkaloid finished product, its purity is more than 90%.
Detailed description of the invention:
Case study on implementation 1: one utilizes the alkaloidal method of Radix seu Herba Spiranthis Lanceae in cellulase degradation and ultrasonic extraction and membrane separation technique coupling enriching and purifying Radix seu Herba Spiranthis Lanceae, and its step is as follows:
(1) done by 100g after Radix seu Herba Spiranthis Lanceae is pulverized and cross 40 mesh sieves, soak 30min with the dilute hydrochloric acid that concentration is 1%, adjust ph is 4.0, adds cellulase, and addition is 2mg/g, enzymolysis time 1 hour, hydrolysis temperature 40 DEG C;
(2) material after (1) process is carried out ultrasonic extraction, solid-liquid ratio is 8 times that pulverize volume, and Extracting temperature is 40 DEG C, extracts frequency 80Hz, extraction time 60minmin, extracts 2 times, merges extracted twice liquid;
(3) extracting solution 1mol/L hydrochloric acid is regulated pH value to 3.4, sucking filtration after 5 DEG C of cold preservation 48h, by filtrate by 50% sodium hydroxide adjust ph to 11, with the chloroform extraction 2 times with filtrate equivalent, combined chloroform liquid, recovery chloroform, obtains alkaloid crude extract;
(4) by extracting solution through ultrafiltration, retain relative molecular weight 3000 ~ 10000, temperature controls at 40 DEG C, and Stress control is at 0.6MPa;
(5) gained filtrate carries out nanofiltration operation again, retains relative molecular weight 20000 ~ 30000, and operative temperature controls at 40 DEG C, and Stress control is at 0.6MPa;
(6) concentrated under vacuum by filtering solution, concentrated Stress control is at 0.02MPa, and temperature controls at 50 DEG C, and proportion is 1.17, obtains alkaloid concentrated solution;
(7) dissolved through chloroform by gained alkaloid concentrated solution, the amount adding chloroform is 5 times of concentrated solution volume, by sodium hydroxide adjust ph to 11, be concentrated into 1/4 of original volume, leave standstill, crystallization obtains alkaloid crude product, so repeatedly twice, obtain alkaloid finished product, its purity is 90.4%.
Case study on implementation 2: one utilizes the alkaloidal method of Radix seu Herba Spiranthis Lanceae in cellulase degradation and ultrasonic extraction and membrane separation technique coupling enriching and purifying Radix seu Herba Spiranthis Lanceae, and its step is as follows:
(1) done by 100g after Radix seu Herba Spiranthis Lanceae is pulverized and cross 60 mesh sieves, soak 30min with the dilute hydrochloric acid that concentration is 1%, adjust ph is 4.5, adds cellulase, and addition is 2.5mg/g, enzymolysis time 1.5 hours, hydrolysis temperature 45 DEG C;
(2) material after (1) process is carried out ultrasonic extraction, solid-liquid ratio is 9 times that pulverize volume, and Extracting temperature is 45 DEG C, extracts frequency 100Hz, extraction time 80min, extracts 2 times, merges extracted twice liquid;
(3) extracting solution 1mol/L hydrochloric acid is regulated pH value to 3.4, sucking filtration after 5 DEG C of cold preservation 48h, by filtrate by 50% sodium hydroxide adjust ph to 11, with the chloroform extraction 2 times with filtrate equivalent, combined chloroform liquid, recovery chloroform, obtains alkaloid crude extract;
(4) by extracting solution through ultrafiltration, retain relative molecular weight 3000 ~ 10000, temperature controls at 50 DEG C, and Stress control is at 0.8MPa;
(5) gained filtrate carries out nanofiltration operation again, retains relative molecular weight 20000 ~ 30000, and operative temperature controls at 50 DEG C, and Stress control is at 0.8MPa;
(6) concentrated under vacuum by filtering solution, concentrated Stress control is at 0.03MPa, and temperature controls at 55 DEG C, and proportion is 1.12, obtains alkaloid concentrated solution;
(7) dissolved through chloroform by gained alkaloid concentrated solution, the amount adding chloroform is 7 times of concentrated solution volume, by sodium hydroxide adjust ph to 11, be concentrated into 1/4 of original volume, leave standstill, crystallization obtains alkaloid crude product, so repeatedly twice, obtain alkaloid finished product, its purity is 91.3%.
Case study on implementation 3: one utilizes the alkaloidal method of Radix seu Herba Spiranthis Lanceae in cellulase degradation and ultrasonic extraction and membrane separation technique coupling enriching and purifying Radix seu Herba Spiranthis Lanceae, and its step is as follows:
(1) done by 100g after Radix seu Herba Spiranthis Lanceae is pulverized and cross 50 mesh sieves, soak 30min with the dilute hydrochloric acid that concentration is 1%, adjust ph, 5.0, adds cellulase, and addition is 3mg/g, enzymolysis time 2 hours, hydrolysis temperature 45 DEG C;
(2) material after (1) process is carried out ultrasonic extraction, solid-liquid ratio is 8 times that pulverize volume, and Extracting temperature is 60 DEG C, extracts frequency 90Hz, extraction time 80min, extracts 2 times, merges extracted twice liquid;
(3) extracting solution 1mol/L hydrochloric acid is regulated pH value to 3.5, sucking filtration after 5 DEG C of cold preservation 48h, by filtrate by 50% sodium hydroxide adjust ph to 11, with the chloroform extraction 2 times with filtrate equivalent, combined chloroform liquid, recovery chloroform, obtains alkaloid crude extract;
(4) by extracting solution through ultrafiltration, retain relative molecular weight 3000 ~ 10000, temperature controls at 60 DEG C, and Stress control is at 2.0MPa;
(5) gained filtrate carries out nanofiltration operation again, retains relative molecular weight 20000 ~ 30000, and operative temperature controls at 60 DEG C, and Stress control is at 2.0MPa;
(6) concentrated under vacuum by filtering solution, concentrated Stress control is at 0.04MPa, and temperature controls at 60 DEG C, and proportion is 1.20, obtains alkaloid concentrated solution;
(7) dissolved through chloroform by gained alkaloid concentrated solution, the amount adding chloroform is 8 times of concentrated solution volume, by sodium hydroxide adjust ph to 11, be concentrated into 1/4 of original volume, leave standstill, crystallization obtains alkaloid crude product, so repeatedly twice, obtain alkaloid finished product, its purity is 91.7%.
Case study on implementation 4: one utilizes the alkaloidal method of Radix seu Herba Spiranthis Lanceae in cellulase degradation and ultrasonic extraction and membrane separation technique coupling enriching and purifying Radix seu Herba Spiranthis Lanceae, and its step is as follows:
(1) done by 100g after Radix seu Herba Spiranthis Lanceae is pulverized and cross 80 mesh sieves, soak 30min with the dilute hydrochloric acid that concentration is 1%, adjust ph, between 5.0, adds cellulase, and addition is 4mg/g, enzymolysis time 1.5 hours, hydrolysis temperature 50 DEG C;
(2) material after (1) process is carried out ultrasonic extraction, solid-liquid ratio is 10 times that pulverize volume, and Extracting temperature is 55 DEG C, extracts frequency 120Hz, extraction time 100min, extracts 2 times, merges extracted twice liquid;
(3) extracting solution 1mol/L hydrochloric acid is regulated pH value to 3.5, sucking filtration after 5 DEG C of cold preservation 48h, by filtrate by 50% sodium hydroxide adjust ph to 11, with the chloroform extraction 2 times with filtrate equivalent, combined chloroform liquid, recovery chloroform, obtains alkaloid crude extract;
(4) by extracting solution through ultrafiltration, retain relative molecular weight 3000 ~ 10000, temperature controls at 55 DEG C, and Stress control is at 2.2MPa;
(5) gained filtrate carries out nanofiltration operation again, retains relative molecular weight 20000 ~ 30000, and operative temperature controls at 55 DEG C, and Stress control is at 2.2MPa;
(6) concentrated under vacuum by filtering solution, concentrated Stress control is at 0.04MPa, and temperature controls at 60 DEG C, and proportion is 1.20, obtains alkaloid concentrated solution;
(7) dissolved through chloroform by gained alkaloid concentrated solution, the amount adding chloroform is 8 times of concentrated solution volume, by sodium hydroxide adjust ph to 11, be concentrated into 1/4 of original volume, leave standstill, crystallization obtains alkaloid crude product, so repeatedly twice, obtain alkaloid finished product, its purity is 92.6%.
Claims (5)
1. from Radix seu Herba Spiranthis Lanceae, extract an alkaloidal method, its step is as follows:
(1) will do after Radix seu Herba Spiranthis Lanceae is pulverized and cross 40 ~ 80 mesh sieves, be the acid soak 30min of 1% by concentration, add cellulase, enzyme addition is 2 ~ 4mg/g, and adjust ph is between 4.0 ~ 5.0, and enzymolysis time is 1 ~ 2 hour, and hydrolysis temperature is 40 ~ 50 DEG C;
(2) material after step (1) process is carried out ultrasonic extraction, solid-liquid ratio is 1:8 ~ 10, and Extracting temperature is 40 ~ 60 DEG C, extraction frequency is 80 ~ 120Hz, extraction time is 60min ~ 100min, extracts 2 times, merges extracted twice liquid;
(3) by extracting solution 1mol/L salt acid for adjusting pH value to 3.4 ~ 3.5, filtrate concentration is the alkali adjust ph to 11 of 50% by sucking filtration after cold preservation 48h at 5 DEG C, with the chloroform extraction 2 times with filtrate equivalent, combined chloroform liquid, reclaims chloroform, obtains alkaloid crude extract;
(4) by extracting solution through ultrafiltration molecular cut off, temperature controls at 40 ~ 60 DEG C, and Stress control is at 0.6 ~ 2.2MPa;
(5) gained filtrate carries out nanofiltration operation molecular cut off again, and operative temperature controls at 40 ~ 60 DEG C, and Stress control is at 0.6 ~ 2.2MPa;
(6) concentrated under vacuum by filtering solution, concentrated Stress control is at 0.02 ~ 0.04MPa, and temperature controls at 50 ~ 60 DEG C, and proportion is 1.12 ~ 1.20, obtains alkaloid concentrated solution;
(7) dissolved through chloroform by gained alkaloid concentrated solution, by sodium hydroxide adjust ph to 11, be concentrated into 1/4 of original volume, leave standstill, crystallization obtains alkaloid crude product, and so repeatedly twice, obtain alkaloid finished product, its purity is more than 90%.
2. according to claim 1ly from Radix seu Herba Spiranthis Lanceae, extract alkaloidal method, wherein, in described step (2), the acid solution of extraction is dilute hydrochloric acid.
3. according to claim 2ly from Radix seu Herba Spiranthis Lanceae, extract alkaloidal method, wherein, in described step (3), the alkali of adjust ph is sodium hydroxide.
4. according to claim 3ly from Radix seu Herba Spiranthis Lanceae, extract alkaloidal method, wherein, in described step (4) and (5), ultrafiltration retains relative molecular weight and retains relative molecular weight 20000 ~ 30000 in 3000 ~ 10000 and nanofiltration.
5. according to claim 4ly from Radix seu Herba Spiranthis Lanceae, extract alkaloidal method, wherein, in described step (7), the amount adding chloroform is 5 ~ 8 times of concentrated solution volume.
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| CN116656865B (en) * | 2023-07-03 | 2024-01-23 | 海南医学院 | Detection method and kit for rapidly identifying spiranthes sinensis and application of detection method and kit |
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| CN101358224A (en) * | 2008-09-04 | 2009-02-04 | 浙江益圣菌物发展有限公司 | Extraction method of hericium erinaceus polysaccharide |
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| CN101358224A (en) * | 2008-09-04 | 2009-02-04 | 浙江益圣菌物发展有限公司 | Extraction method of hericium erinaceus polysaccharide |
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| 不同产地绶草中总黄酮的含量测定;李家敏;《湖北农业科学》;20120531;第51卷(第9期);1866-1867、1871 * |
| 响应面法优化盘龙参多酚微波辅助提取工艺;吴道宏等;《吉首大学学报》;20120531;第33卷(第3期);81-85、99 * |
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