CN1566137A - Production process for platycodin - Google Patents

Production process for platycodin Download PDF

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Publication number
CN1566137A
CN1566137A CN 03139761 CN03139761A CN1566137A CN 1566137 A CN1566137 A CN 1566137A CN 03139761 CN03139761 CN 03139761 CN 03139761 A CN03139761 A CN 03139761A CN 1566137 A CN1566137 A CN 1566137A
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CN
China
Prior art keywords
resin bed
hour
flow rate
total saponins
balloonflower root
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN 03139761
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Chinese (zh)
Inventor
王炜
何勤
陈平
黄礼杰
颜胜利
王明军
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SHENZHEN YISHENG PHARMACEUTICAL SCIENCE AND TECHNOLOGY DEV Co Ltd
Original Assignee
SHENZHEN YISHENG PHARMACEUTICAL SCIENCE AND TECHNOLOGY DEV Co Ltd
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Priority to CN 03139761 priority Critical patent/CN1566137A/en
Publication of CN1566137A publication Critical patent/CN1566137A/en
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Abstract

A production process for platycodin comprises, (1) charging water into balloonflower root coarse grains, boiling, extracting three times, combining the extract liquid and concentrating, (2) isolating through absorption resin bed, (3) rinsing the resin bed with deionized water, (3) rinsing the resin bed with 70% of alcohol, (5) gathering alcohol eluent, reclaiming alcohol through decompression, concentrating, spray drying to obtain the end product.

Description

The Radix Platycodi total saponins production technique
Technical field
The present invention relates to extracting technique of Chinese medicine, particularly from balloonflower root, extract the platycodin correlation technique.
Background technology
From tcm theory, the basic pathogenesis of acute and chronic bronchitis illness is outer evil lung, impairment of dispersing and descending function of the lung, the deficiency of yang phlegm and retained fluid violated, and then causes cough, and gas is not returned and will then cannot do not breathed hard continuously.Its performance is that cough is prolonged, the often deficiency syndrome of the lung and spleen, insufficiency of the spleen-yang damage, water-damp not being transformed constantly grows phlegm and retained fluid, on store in lung, and root for showing effect repeatedly, chronic cough for many years must reach kidney, kidney yang thoroughly and lose emptyly, loses in taking the photograph and receives, gas is not returned unit, just forms disease such as do not breathe hard continuous.The above-mentioned illness of Chinese traditional treatment balloonflower root commonly used is used as medicine, and its Chinese patent medicine has platycodinin, Platycodi Pill, sheet etc.Also have Radix Platycodonis extract liquid technology to use, but it is numerous and diverse to have technology comparatively speaking, purity is not enough, the effective ingredient extraction yield is low wait not enough.
Technology contents
It is simple to the purpose of this invention is to provide a kind of method, the production technique that the platycodin extraction yield is high.
The present invention can be achieved through the following technical solutions.
The Radix Platycodi total saponins production technique, described process using following steps:
1. get the balloonflower root coarse particles, add 10~15 times of water gagings, soaked 1~3 hour, heated and boiled is extracted 3 times, add 8~12,6~10 times of water gagings respectively the 2nd time, extraction time was respectively 1~2,0.5~1.5,0.5~1.5 hour, filtered, merge three times soup, being concentrated into relative density is 1.0~1.2 (50 ℃ of heat are surveyed).
2. treat the soup cooling, behind high speed centrifugation (16000r/min), press Radix Platycodi total saponins content: HPD100 type macroporous adsorbent resin bed (blade diameter length ratio 1: 5) on dried resin=1: 15~20, last column flow rate is 3BV/h.
3. washed resin bed 3~5 hours with deionized water, elution flow rate is 3BV/h, discards water lotion.
4. washed resin bed 1~3 hour with 70% ethanol, elution flow rate is 3BV/h, collects ethanol eluate.
5. decompression recycling ethanol, being concentrated into relative density is 1.1~1.25 (50 ℃ of heat are surveyed), spraying drying (180 ℃ of inlet temperature, 100 ℃ of temperature of outgoing airs), the Radix Platycodi total saponins extract.
Also the Radix Platycodi total saponins extract can be made various formulations:
A, Radix Platycodi total saponins is added appropriate amount of starch and dextrin mix spoon, use 90% alcohol granulation, 16 orders sieve, and particle is after 60~80 ℃ of dryings, and compacting is wrapped film-coat, promptly in flakes.
B, above-mentioned Radix Platycodi total saponins is added an amount of Celluloasun Microcrystallisatum, mixing, after 60~80 ℃ of dryings, filled capsules promptly gets capsule formulation.
C, above-mentioned Radix Platycodi total saponins is added appropriate amount of starch and dextrin, mixing is used 90% alcohol granulation, and 12 orders sieve, and particle is in 60~80 ℃ of dryings, and packing promptly gets granule.
The present technique advantage is that the method for extracting total saponins in the balloonflower root is simple, the extraction yield height.
Specific implementation method
The Radix Platycodi total saponins production technique, described process using following steps:
1. get balloonflower powder and be broken to coarse particles 10kg about diameter 3mm, add 12 times of water gagings, soaked 2 hours, heated and boiled is extracted 3 times, 2nd, add 10,8 times of water gagings for 3 times respectively, extraction time was respectively 1.5,1,1 hours, filtered, merge three times soup, being concentrated into relative density is 1.05-1.08 (50 ℃ of heat are surveyed).
2. treat the soup cooling, behind high speed centrifugation (16000r/min), press Radix Platycodi total saponins content: dried resin=HPD100 type macroporous adsorbent resin bed (blade diameter length ratio 1: 5) on 1: 17.7, last column flow rate is 3BV/h.
3. washed resin bed 4 hours with deionized water, elution flow rate is 3BV/h, discards water lotion.
4. washed resin bed 2 hours with 70% ethanol, elution flow rate is 3BV/h, collects ethanol eluate.
5. decompression recycling ethanol, being concentrated into relative density is 1.15~1.18 (50 ℃ of heat are surveyed), spraying drying (inlet temperature 180, temperature of outgoing air 100), the Radix Platycodi total saponins extract.
6. above-mentioned total saponins is added appropriate amount of starch and dextrin, use 90% alcohol granulation, 16 orders sieve, and are pressed into 1000, and the bag film-coat promptly gets tablet.
Experimentation:
Control drug: pentoxiverin (antibechic), ammonium chloride (eliminating the phlegm)
Blank product: physiological saline
Laboratory animal: small white mouse, KM kind, ♀ ♂ half and half, body weight 20 ± 2g.Purchase in Traditional Chinese Medicine University Of Guangzhou's Experimental Animal Center (Guangdong probatio inspectionem pecuoarem word: 2001A054 number)
Other medicine: ammoniacal liquor, phenol red, physiological saline, sodium bicarbonate
Utensil: 10ml Erlenmeyer flask, 10ml test tube, measuring cup (5-100ml), 5ml syringe, 1ml syringe, irritate stomach pin, syringe needle (various model), stopwatch, tweezers, medical gloves, plastic film gloves, draw and cough device (500ml beaker, cotton balls or lens, air pump), glue head dropper, beaker (10-100ml), glass stick, transfer pipet (1-10ml), punch tool, operating scissors, electronic balance, torsion(type)balance, UV-730 trace stream dynamic formula spectrophotometer
Experimental technique and result
Determining of dosage
Be equivalent to people's routine clinical dosage (reduction factor 0.0026) administration for reagent thing, positive control drug with mouse, wherein the Radix Platycodi total saponins extract divides three dosage groups (2 times of routine dose, routine dose, routine dose 1/2).
Animal grouping and dosage
Balloonflower root crude drug aqueous extract group is (in the crude drug amount, 20g/kg)
Balloonflower root water extract group is (in the crude drug amount, 20g/kg)
The balloonflower root n-butyl alcohol extract is total saponin extracts group (high, medium and low dosage is respectively 0.4g/kg, 0.1g/kg)
Positive controls (pentoxiverin 10mg/kg, ammonia chloride 0.5g/kg)
Blank group (physiological saline group)
The animal random packet, 10 every group.
Method and result
Mouse ammoniacal liquor draws the method for coughing
Get the animal of random packet, the difference gastric infusion, the blank combination gives distilled water 0.15ml/10g.Behind the administration 1hr mouse is placed in the 2L bell glass, (about 400mmHg) begins to accept spraying under constant voltage.Stop spraying behind the spraying 20s, in bell jar, place 20s, take out mouse immediately.Cough number of times in record mouse cough latent period and the 2min carries out statistical treatment with the gained data and makes comparisons with the blank group, carries out the t inspection statistics and analyzes (table 1).
Table 1GJO to ammoniacal liquor cause the influence of coughing mouse (X ± S, n=10)
The group dosage number of times of coughing latent period
(g/kg) (s) (/2min)
Physiological saline-32.8 ± 14.2 57.6 ± 7.9
Pentoxiverin group 0.01 59.6 ± 17.8 *33.9 ± 8.2 * *
Balloonflower root crude drug water carries 20 35.2 ± 18.9 43.8 ± 16.9
The thing group
Balloonflower root water extract group 20 38.7 ± 12.8 57.9 ± 10.8
GJO group 0.1 47.4 ± 12.9 * *42.4 ± 17.2 *
Group 0.2 49.1 ± 17.9 among the GJO *40.3 ± 16.9 *
Big group 0.4 55.5 ± 15.4 of GJO *40.0 ± 8.0 * *
Annotate: compare with the physiological saline group, * represents P<0.05, and * * represents P<0.01, and * * * represents P<0.001
The result shows that (0.1g/kg, 0.2g/kg's pentoxiverin (10mg/kg) 0.4g/kg) experimentize behind the administration mouse, have the effect of shortening cough latent period, reduce the cough number of times in 2min, show that GJO has antitussive effect with GJO.
The phenol red expelling phlegm method of mouse
Get the animal of random packet, respectively at first the sky, afternoon each gastric infusion once, the blank group gives distilled water 0.15ml/10g, behind administration in the morning next day 1/2hr, difference abdominal injection 2.5% phenol red solution 0.1ml/10g, put to death mouse behind the 1/2hr, peel off the tracheae surrounding tissue, cut one section tracheae down to the tracheae bifurcation from thyroid cartilage, put into the test tube that fills 2ml physiological saline, add 1-2 again and drip 5% sodium hydrogen carbonate solution, supersound process, centrifugation (3000rpm) 3min.Get supernatant liquor and measure its optical density in ultraviolet-visible spectrophotometer 545nm place, try to achieve the phenol red content of excretion, the gained data are carried out statistical treatment, and make comparisons, carry out the t inspection statistics and analyze (table 2) with the blank group
Table 2GJO to the phenol red influence that causes the phlegm mouse (X ± S, n=10)
Group dosage colorimetric result
(g/kg) (g/ml)
Blank group-3.38 ± 1.72
Ammonia chloride group 0.5 5.47 ± 1.86 *
GJO group 0.1 5.21 ± 1.95 *
Group 0.2 5.15 ± 1.48 among the GJO *
Big group 0.4 5.34 ± 1.74 of GJO *
Annotate: compare with the physiological saline group, * represents P<0.05
The result shows that (0.1g/kg, 0.2g/kg's ammonia chloride (0.5g/kg) 0.4g/kg) experimentize behind the administration mouse, have the effect that promotes phenol red excretion, show that GJO has phlegm-dispelling functions with GJO.

Claims (1)

1, the Radix Platycodi total saponins production technique is characterized in that, described process using following steps:
1. get the balloonflower root coarse particles, add 10~15 times of water gagings, soaked 1~3 hour, heated and boiled is extracted 3 times, 2nd, add 8~12,6~10 times of water gagings for 3 times respectively, extraction time was respectively 1~2,0.5~1.5,0.5~1.5 hour, filtered, merge three times soup, being concentrated into relative density is 1.0-1.2 (50 ℃ of heat are surveyed).
2. treat the soup cooling, behind high speed centrifugation (16000r/min), press balloonflower root medicinal material total saponin content: HPD100 type macroporous adsorbent resin bed (blade diameter length ratio 1: 5) on dried resin=1: 15~20, last column flow rate is 3BV/h.
3. washed resin bed 3-5 hour with deionized water, elution flow rate is 3BV/h, discards water lotion.
4. washed resin bed 1-3 hour with 70% ethanol, elution flow rate is 3BV/h, collects ethanol eluate.
5. decompression recycling ethanol, being concentrated into relative density is 1.1~1.25 (50 ℃ of heat are surveyed), spraying drying (180 ℃ of inlet temperature, 100 ℃ of temperature of outgoing airs), the Radix Platycodi total saponins extract.
CN 03139761 2003-07-04 2003-07-04 Production process for platycodin Pending CN1566137A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100406467C (en) * 2006-05-24 2008-07-30 浙江大学 Method for preparing total saponins from theroots of platycodon grandiflorum utilizing weak polarity macroreticular resin and its use
CN101856382A (en) * 2010-07-02 2010-10-13 安徽济人药业有限公司 Novel method for extracting and separating platycodin effective ingredients
CN101904890A (en) * 2009-06-02 2010-12-08 中国医学科学院药用植物研究所 Preparation method, application and QC (Quality Control) detection method of platycodon grandiflorum active site
CN101084971B (en) * 2006-06-08 2011-06-08 天津天士力之骄药业有限公司 Method for preparing total saponins of platycodon grandiflorum
CN102264378A (en) * 2009-01-23 2011-11-30 B&C生物制药株式会社 Pharmaceutical composition for preventing or treating hepatitis c, comprising the roots extract of platycodon grandiflorum or platycodon grandiflorum saponin components
CN102327310A (en) * 2011-11-04 2012-01-25 安徽中医学院 Preparation method of high-purity platycodon root total saponin
CN102423334A (en) * 2011-09-30 2012-04-25 淮南联合大学 Comprehensive extraction method of platycodin and platycodon polysaccharide
CN106994180A (en) * 2016-01-23 2017-08-01 卡拉玛(长沙)生物科技有限公司 A kind of traditional Chinese medical science medicine composition with foot health-care function
CN108497302A (en) * 2018-03-23 2018-09-07 广东日可威富硒食品有限公司 A kind of selenium-enriched cordceps militaris noodles and preparation method thereof
CN110028545A (en) * 2019-05-28 2019-07-19 南开大学 A kind of preparation method for the secondary saponin(e of campanulaceae that can improve permeability of cell membrane

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100406467C (en) * 2006-05-24 2008-07-30 浙江大学 Method for preparing total saponins from theroots of platycodon grandiflorum utilizing weak polarity macroreticular resin and its use
CN101084971B (en) * 2006-06-08 2011-06-08 天津天士力之骄药业有限公司 Method for preparing total saponins of platycodon grandiflorum
CN102264378A (en) * 2009-01-23 2011-11-30 B&C生物制药株式会社 Pharmaceutical composition for preventing or treating hepatitis c, comprising the roots extract of platycodon grandiflorum or platycodon grandiflorum saponin components
CN101904890A (en) * 2009-06-02 2010-12-08 中国医学科学院药用植物研究所 Preparation method, application and QC (Quality Control) detection method of platycodon grandiflorum active site
CN101856382A (en) * 2010-07-02 2010-10-13 安徽济人药业有限公司 Novel method for extracting and separating platycodin effective ingredients
CN102423334A (en) * 2011-09-30 2012-04-25 淮南联合大学 Comprehensive extraction method of platycodin and platycodon polysaccharide
CN102327310A (en) * 2011-11-04 2012-01-25 安徽中医学院 Preparation method of high-purity platycodon root total saponin
CN102327310B (en) * 2011-11-04 2014-03-19 安徽中医学院 Preparation method of high-purity platycodon root total saponin
CN106994180A (en) * 2016-01-23 2017-08-01 卡拉玛(长沙)生物科技有限公司 A kind of traditional Chinese medical science medicine composition with foot health-care function
CN108497302A (en) * 2018-03-23 2018-09-07 广东日可威富硒食品有限公司 A kind of selenium-enriched cordceps militaris noodles and preparation method thereof
CN110028545A (en) * 2019-05-28 2019-07-19 南开大学 A kind of preparation method for the secondary saponin(e of campanulaceae that can improve permeability of cell membrane
CN110028545B (en) * 2019-05-28 2021-09-14 南开大学 Preparation method of platycodon secondary saponin capable of improving cell membrane permeability

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