CN108164541A - The method that dendrobine is extracted in dendrobium candidum - Google Patents
The method that dendrobine is extracted in dendrobium candidum Download PDFInfo
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- CN108164541A CN108164541A CN201810049833.5A CN201810049833A CN108164541A CN 108164541 A CN108164541 A CN 108164541A CN 201810049833 A CN201810049833 A CN 201810049833A CN 108164541 A CN108164541 A CN 108164541A
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- dendrobium candidum
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D491/00—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00
- C07D491/02—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00 in which the condensed system contains two hetero rings
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Abstract
The invention discloses a kind of methods that dendrobine is extracted in dendrobium candidum:Including:1. taking dendrobium candidum, crush, be 1 by solid-liquid ratio:10 14 add in water into dendrobium candidum, obtain A product;2. A product adjust pH=9 with saturated limewater;3. Microwave Extraction 3 times in the case where power is 300 320W of B product, extract 15 20min, extracting solution merges, and obtains C product every time;4. C product filter, filter vacuum concentration obtains D product;5. adding in 34 times of amount ethyl alcohol in D product, 10 12h are placed at 14 DEG C, obtain E product;6. E product filter, precipitation washed 34 times with ethyl alcohol, it is dry to constant weight to get.When present invention process extracts dendrobium candidum, dendrobine recovery rate is high, promotes the utilization to dendrobium candidum dendrobine.
Description
Technical field
The present invention relates to a kind of extracting method of dendrobium candidum, the side of dendrobine is extracted in particularly a kind of dendrobium candidum
Method.
Background technology
Dendrobium candidum nickname iron sheet orchid, bracketplant, Yunnan iron sheet, iron sheet bracketplant are orchid family Dendrobium herbaceos perennials,
Dendrobium candidum is the top grade of Shihu " medicinal materials, is known as the laudatory title of " gold in Chinese celestial grass-medicine ", is used as medicine with stem, containing dendrobine,
The active ingredients such as dendrobine, alkaloid, with nourishing Yin and clearing heat, the beneficial stomach that promotes the production of body fluid, wet one's whistle improving eyesight and other effects, in antitumor, raising people
Body immunity, anti-aging, anti-oxidant, platelet aggregation-against, reduces blood glucose, treatment cataract etc. at treatment enterogastric diseases
There is good efficacy.
Modern pharmacology research shows that dendrobium candidum has humidification to non-specific and specific immunity, anti-swollen
Knurl, treatment that is anti-oxidant, reducing blood glucose and cataract etc., pharmacological action is notable.The drug action of dendrobium candidum is main
It is because it contains a variety of active ingredients, such as alkaloid, dendrobine, amino acid, but the effect of various active constituents not to the utmost
It is identical.And dendrobium candidum clinically application mainly by taking and working dendrobium candidum medicinal material tanning decoction of medicinal ingredients, each activity into
The effect of dividing is not applied targetedly, so the utilization of dendrobium candidum mainly also rests on the primary stage of low side,
Medical value also needs further to develop.Research shows that dendrobine has the works such as immunological regulation, anti-inflammatory, expansion blood vessel in dendrobium candidum
With with good potential Development volue.If further opening to dendrobium candidum is recycled after its dendrobine is extracted
Hair is of great significance.
There is certain limitation to the extraction of dendrobine at present so that dendrobine recovery rate is low, limits dendrobium candidum
The utilization of dendrobine active constituent.
Invention content
The purpose of the present invention is to provide a kind of method that dendrobine is extracted in dendrobium candidum, and present invention process is to iron sheet stone
When dry measure used in former times extracts, dendrobine recovery rate is high, promotes the utilization to dendrobium candidum dendrobine.
The invention is realized in this way:The method that dendrobine is extracted in dendrobium candidum, including:
1. taking dendrobium candidum, crush, be 1 by solid-liquid ratio:10-14 adds in water into dendrobium candidum, obtains A product;
2. A product adjust pH=9 with saturated limewater, B product are obtained;
3. Microwave Extraction 3 times in the case where power is 300-320W of B product, extract 15-20min, extracting solution merges, and obtains C product every time;
4. C product filter, filter vacuum concentration obtains D product;
5. adding in 3-4 times in D product measures ethyl alcohol, 10-12h is placed at 1-4 DEG C, obtains E product;
6. E product filter, precipitation wash 3-4 times with ethyl alcohol, dry to constant weight to get.
In aforementioned dendrobium candidum extract dendrobine method in, step 3. in:The power is 310W.
In aforementioned dendrobium candidum extract dendrobine method in, step 3. in, each extraction time be 18min.
In aforementioned dendrobium candidum extract dendrobine method in, step 4. in, the filter vacuum concentration is;It is divided to two
Secondary to be concentrated, the first secondary control vacuum degree is 0.07-0.08MPa, and the second secondary control vacuum degree is 0.08-0.09MPa, twice
It is 5-10min to be concentrated in vacuo the time.
In the method that dendrobine is extracted in aforementioned dendrobium candidum, filter vacuum concentration is;It carries out in two times dense
Contracting, the first secondary control vacuum degree are 0.07-0.08MPa, and the second secondary control vacuum degree is 0.08-0.09MPa, is concentrated in vacuo twice
Time is 8min.
In the method that dendrobine is extracted in aforementioned dendrobium candidum, 5. the step is;3 times of amount ethyl alcohol are added in D product,
11h is placed at 1-4 DEG C, obtains E product.
Applicant has carried out a large amount of experimental study to the present invention, and part Experiment is as follows:
1 dendrobine recovery rate of experimental example is investigated
1 material
3 parts of the dendrobium candidum that weight is identical is taken, extract 1, extract 2 and extract 3 is made as follows respectively.
Extract 1:It is extracted by embodiment 1.
Extract 2:Extracting method and embodiment 1 the difference lies in:
(1)1. middle solid-liquid ratio is 1 to step:20;
(2)Step 4. middle concentration when, first time vacuum degree is 0.06MPa, and second vacuum degree is 0.07MPa.
2 methods and result.
Obtained extract 1 and extract 2 are weighed, recovery rate is calculated according to result, recovery rate calculation formula is,
Recovery rate(%)=(Dendrobium candidum fresh weight-extract weight)* 100%/iron sheet tree fresh weight.Final result is:
Recovery rate=21.38% of extract 1
Recovery rate=15.01% of extract 2
Recovery rate=16.02% of extract 3.
It follows that extraction process recovery rate highest of the present invention.
2 purity of experimental example is investigated
1 materials and methods
1.1 material
1.1.1 dendrobium candidum 1:It is extracted by embodiment 1.
1.1.2 dendrobium candidum 2:Extracting method is the same as extract 2.
1.2 instruments and reagent
Dendrobine standard items:Chengdu Man Site Bioisystech Co., Ltd, MUST-12080608.A E240 electronic balances:It is auspicious
Scholar MEITLER;HH-s digital control constant temperature water-baths:Jinhua Wenhua science and education laboratory apparatus factory;510 Rotary Evaporators of BM:Japan
YAM ATO companies;6890N gas chromatographs:Pacify in the U.S.
Jie Lun companies;UV-2450 ultraviolet specrophotometers:Japanese Shimadzu Corporation;Methanol (chromatographically pure):Tianjin section is close europeanized
Learn reagent Co., Ltd;Remaining reagent is that analysis is pure;Phenol:Shanghai Ling Feng chemical reagent Co., Ltd;Sulfuric acid:Shanghai Ling Feng
Chemical reagent Co., Ltd.
2 methods
The preparation of 2.1 test solutions
2.1.1 the preparation of test solution 1:
1 powder 3.34g of dendrobium candidum is taken, adds 90% ethyl alcohol of 200mL, is flowed back 1 hour, filtering pours out supernatant, then adds
100mL90% ethyl alcohol flows back 1 hour, pours out supernatant, merges above-mentioned 2 supernatants, puts Rotary Evaporators concentration, water-bath
50 DEG C are evaporated, and dry product adds methanol to dissolve, and are settled to 25m L to get test solution 1.
2.1.2 the preparation of test solution 2
2 powder 3.34g of dendrobium candidum is taken, adds 90% ethyl alcohol of 200mL, is flowed back 1 hour, filtering pours out supernatant, then adds
100mL90% ethyl alcohol flows back 1 hour, pours out supernatant, merges above-mentioned 2 supernatants, puts Rotary Evaporators concentration, water-bath
50 DEG C are evaporated, and dry product adds methanol to dissolve, and are settled to 25m L to get test solution 2.
The preparation of 2.2 reference substance solutions
Precision is weighed in dendrobine reference substance 50.01lmg to 100mL measuring bottles, and methanol constant volume is added to shake up to scale, obtain 500.1m
G/L dendrobine reference substance mother liquors.50.01m g/L solution, it is spare as reference substance solution.
2.3 chromatographic condition
Chromatographic column:D B-1 capillary columns (30mm × 0.25mm, 0.25um);Temperature programming:Initial temperature is 80 DEG C, with
The rate of 10 DEG C/min is warming up to 250 DEG C, is kept for 5 minutes;Injector temperature is 250 DEG C, and detector temperature is 250 DEG C, into
Sample amount 10uL, theoretical cam curve is based on dendrobine, not less than 10000.
It is prepared by 2.4 standard curves
Precision measurement reference substance solution 0.2,0.5,0.8,1.0,2.0,4.0m L are respectively placed in 10m L measuring bottles, add first
Alcohol shakes up to scale.It is measured by above-mentioned chromatographic condition.Using integrating peak areas as ordinate, reference substance sample size for abscissa into
Row linear regression, regression equation are A=0.7522C -0.0252, and r=0.9997 shows dendrobine in 0.10-2.00ug models
There is good linear relationship in enclosing.
2.5 precision test
Precision draws dendrobine reference substance solution l0ul, and continuous 6 sample introductions record peak area, and the RSD of dendrobine peak area is
1.58%, show that instrument precision is good.
2.6 repetitive test
6 parts of test solutions 1 and test solution 2 are prepared as stated above, are measured by above-mentioned chromatographic condition.Dendrobine peak
The RSD of area is respectively 2.05% and 2.06%.
2.7 stability test
Take same test solution 1, place at room temperature, respectively at 0,2,4,6,8, l2 hours sample introductions, record dendrobine
Peak area, RSD 2.88%.The result shows that test solution 1 was stablized in 12 hours.
Take same test solution 2, place at room temperature, respectively at 0,2,4,6,8, l2 hours sample introductions, record stone
Dry measure used in former times alkali peak area, RSD 2.89%.The result shows that test solution 2 was stablized in 12 hours.
2.8 recovery test
Take known content 0.46mg/g) 6 parts of dendrobium candidum powder, every part of about 1.65g is accurately weighed.It is accurate to add in dendrobine
2 mL of reference substance mother liquor, prepares test solution 1 and test solution 2 as stated above, is surveyed under above-mentioned chromatographic condition
It is fixed, calculate the rate of recovery.As a result average recovery rate is 97.1% and 96.8%, RSD are respectively 2.5% and 2.6%.
2.9 sample sizes measure
The preparation method and determination condition of above-mentioned test solution 1, test solution 2 and test solution 3 measure 6 parts of extractions
The content of dendrobine in 1 sample of object and 6 parts of 2 samples of dendrobium candidum, record the results are shown in Table 1 as a result, results are averaged.
As seen from table, present invention process to dendrobium candidum into during extraction, dendrobine containing 910.23g in every gram of extract, stone
Dry measure used in former times alkali purity is 91.0%, and the dendrobine purity in extract 2 is 71.0%.
Compared with prior art, when present invention process extracts dendrobium candidum, recovery rate is high, and dendrobine purity is high
Up to 91.0%.
Specific embodiment
Embodiment 1.
The method that dendrobine is extracted in dendrobium candidum, includes the following steps:
1. taking dendrobium candidum, crush, be 1 by solid-liquid ratio:12 add in water into dendrobium candidum, obtain A product;
2. A product adjust pH=9 with saturated limewater;
3. Microwave Extraction 3 times in the case where power is 310W of B product, extract 18min, extracting solution merges, and obtains C product every time;
4. C product filter, filtrate is concentrated in two times, and the first secondary control vacuum degree is 0.07-0.08MPa, and the second secondary control is true
Reciprocal of duty cycle is 0.08-0.09MPa, and it is 8min to be concentrated in vacuo the time twice, obtains D product;
5. adding in 3 times of amount ethyl alcohol in D product, 11h is placed at 1-4 DEG C, obtains E product;
6. E product filter, precipitation wash 3-4 times with ethyl alcohol, dry to constant weight to get.
Embodiment 2.
The method that dendrobine is extracted in dendrobium candidum, includes the following steps:
1. taking dendrobium candidum, crush, be 1 by solid-liquid ratio:10 add in water into dendrobium candidum, obtain A product;
2. A product adjust pH=9 with saturated limewater;
3. Microwave Extraction 3 times in the case where power is 320W of B product, extract 20min, extracting solution merges, and obtains C product every time;
4. C product filter, filtrate is concentrated in two times, and the first secondary control vacuum degree is 0.07-0.08MPa, and the second secondary control is true
Reciprocal of duty cycle is 0.08-0.09MPa, and it is that 10min obtains D product to be concentrated in vacuo the time twice;
5. adding in 4 times of amount ethyl alcohol in D product, 12h is placed at 1-4 DEG C, obtains E product;
6. E product filter, precipitation wash 4 times with ethyl alcohol, dry to constant weight to get.
Embodiment 3.
The method that dendrobine is extracted in dendrobium candidum, includes the following steps:
1. taking dendrobium candidum, crush, be 1 by solid-liquid ratio:14 add in water into dendrobium candidum, obtain A product;
2. A product adjust pH=9 with saturated limewater;
3. Microwave Extraction 3 times in the case where power is 300W of B product, extract 15min, extracting solution merges, and obtains C product every time;
4. C product filter, filtrate is concentrated in two times, and the first secondary control vacuum degree is 0.07-0.08MPa, and the second secondary control is true
Reciprocal of duty cycle is 0.08-0.09MPa, and it is that 5min obtains D product to be concentrated in vacuo the time twice;
5. adding in 3 times of amount ethyl alcohol in D product, 10h is placed at 1-4 DEG C, obtains E product;
6. E product filter, precipitation wash 3 times with ethyl alcohol, dry to constant weight to get.
Claims (6)
1. the method for dendrobine is extracted in dendrobium candidum, it is characterised in that:Including:
1. taking dendrobium candidum, crush, be 1 by solid-liquid ratio:10-14 adds in water into dendrobium candidum, obtains A product;
2. A product adjust pH=9 with saturated limewater;
3. Microwave Extraction 3 times in the case where power is 300-320W of B product, extract 15-20min, extracting solution merges, and obtains C product every time;
4. C product filter, filter vacuum concentration obtains D product;
5. adding in 3-4 times in D product measures ethyl alcohol, 10-12h is placed at 1-4 DEG C, obtains E product;
6. E product filter, precipitation wash 3-4 times with ethyl alcohol, dry to constant weight to get.
2. the method for dendrobine is extracted in dendrobium candidum as described in claim 1, it is characterised in that:Step 3. in:Described
Power is 310W.
3. the method for dendrobine is extracted in dendrobium candidum as described in claim 1, it is characterised in that:Step 3. in, carry every time
It is 18min to take the time.
4. the method for dendrobine is extracted in dendrobium candidum as described in claim 1, it is characterised in that:Step 4. in, it is described
Filter vacuum concentrates;Concentrated in two times, the first secondary control vacuum degree be 0.07-0.08MPa, the second secondary control vacuum degree
For 0.08-0.09MPa, it is 5-10min to be concentrated in vacuo the time twice.
5. the method for dendrobine is extracted in dendrobium candidum as claimed in claim 4, it is characterised in that:The filter vacuum is dense
Contracting is;It is concentrated in two times, the first secondary control vacuum degree is 0.07-0.08MPa, and the second secondary control vacuum degree is 0.08-
0.09MPa, it is 8min to be concentrated in vacuo the time twice.
6. the method for dendrobine is extracted in dendrobium candidum as described in claim 1, it is characterised in that:5. the step is;D
3 times of amount ethyl alcohol are added in product, 11h is placed at 1-4 DEG C, obtains E product.
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CN113332383A (en) * | 2021-03-05 | 2021-09-03 | 杭州蚕宝生物技术有限公司 | Method for efficiently extracting alkaloid from dendrobium officinale |
CN113425694A (en) * | 2021-07-02 | 2021-09-24 | 杭州蚕宝生物技术有限公司 | Dendrobium alkaloid orally disintegrating tablet and preparation method thereof |
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