CN1839939A - Method for extracting alpha- glucosidase inhibitor from traditional Chinese cinnamomum cassia - Google Patents

Method for extracting alpha- glucosidase inhibitor from traditional Chinese cinnamomum cassia Download PDF

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Publication number
CN1839939A
CN1839939A CN 200610023280 CN200610023280A CN1839939A CN 1839939 A CN1839939 A CN 1839939A CN 200610023280 CN200610023280 CN 200610023280 CN 200610023280 A CN200610023280 A CN 200610023280A CN 1839939 A CN1839939 A CN 1839939A
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extraction
separation reactor
supercritical
alpha
temperature
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CN100408054C (en
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雍克岚
吕敬慈
张忠
陈旭
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University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Abstract

The invention relates to a process for preparing alpha- glucosidase depressant from Cinnamomum cassia, which comprises removing low-polarity constituents with no inhibiting activity to alpha-glucosidase from Cinnamomum cassia by means of fluid extraction technique, and carrying out solid-liquid oscillation extraction to the residual of extracting with anhydrous alcohol. The extracted effective portion has rather strong inhibiting activity to alpha-glucosidase.

Description

From Chinese medicine cinnamon, extract the method for alpha-glucosidase inhibitor
Technical field
The present invention relates to a kind of method of from Chinese medicine cinnamon, extracting alpha-glucosidase inhibitor, belong to Chinese herbal medicine preparation and technical field of chemistry and chemical engineering.
Background technology
Cortex Cinnamomi has another name called beautiful osmanthus, Cortex cinnamomi japonici (Ramulus Cinnamomi) etc., is a kind of conventional Chinese medicine and food adjuvant, and health is had no side effect.Chinese medicine cinnamon derives from the cinnamomic dry bark of canella.Cortex Cinnamomi have mend that fire is supporing yang, the effect of let the fire back to its origin, dispersing cold for relieving pain, promoting blood circulation to restore menstrual flow.In recent years, find that Cortex Cinnamomi also has the effect of prevent diabetes, but do not see the report that from Cortex Cinnamomi, extracts alpha-glucosidase inhibitor and carry out the research aspect of hypoglycemic activity.
Once there was at present the scholar to adopt supercritical liquid extraction technique in Chinese medicine cinnamon, to extract the research report of cinnamon essential oil.
Summary of the invention
The purpose of this invention is to provide a kind of method of from Chinese medicine cinnamon, extracting alpha-glucosidase inhibitor.
The main points of the inventive method are: at first adopt supercritical liquid extraction technique to remove from Chinese medicine cinnamon the active low-polarity constituents of alpha-glucosidase unrestraint, the reuse dehydrated alcohol carries out liquid-solid extraction to raffinate, extracts alpha-glucosidase is had the very effective site of strong inhibitory activity.
The present invention relates to a kind of method of from Chinese medicine cinnamon, extracting alpha-glucosidase inhibitor, it is characterized in that having following technical process and step:
A. the raw material Chinese medicine cinnamon is pulverized, and sieved, make by 40~80 mesh sieves; Then this powder material is put into supercritical CO 2Extract supercritical CO in the extraction kettle of fluid extraction device 2Fluid flows into extraction kettle with the flow of 25~30kg per hour, and the pressure in the extraction kettle remains 20~30MPa, and temperature remains 35~45 ℃;
B.CO 2Fluid enters separation reactor I and separation reactor I I; The pressure of separation reactor I is 6~8MPa, and temperature is 55~65 ℃; The pressure of separation reactor I I is 6~7MPa, and temperature is 35~45 ℃; Under these conditions, supercritical CO 2Fluid extraction 2~3 hours, finally the material that stays in separation reactor I and separation reactor I I is the active component of unrestraint, other deals with; And the raffinate that stays in the extraction kettle is further handled;
C. in above-mentioned raffinate, add dehydrated alcohol and under 40~60 ℃ of temperature, carry out solid-liquid concussion extraction, concussion extraction 60~80 minutes, repeat again once, merge alcohol extraction liquid twice, reclaim alcohol solvent with rotary evaporator, obtain alpha-glucosidase is had the effective site of strong inhibitory activity at last.
The inventive method adopts the process integration of supercritical fluid extraction and ethanol extraction, and the alpha-glucosidase inhibitor that finally obtains can be used for the exploitation of hypoglycemic drug.Technology of the present invention is simple, and is easy to operate, and product do not contain harmful dissolvent residual, also pollution-free to environment.
The specific embodiment
After now embodiments of the invention being described in.
Embodiment 1
Alpha-glucosidase inhibitor extracts in the present embodiment process and step are as follows:
(1) at first 300g raw material Chinese medicine cinnamon is pulverized, and sieved, make by 80 mesh sieves; Then this powder material is put into supercritical CO 2Extract supercritical CO in the extraction kettle of fluid extraction device 2Fluid flows into extraction kettle with the flow of 25kg per hour, and the pressure in the extraction kettle remains 25MPa, and temperature remains 40 ℃;
(2) CO 2Fluid enters separation reactor I and separation reactor I I; The pressure of separation reactor I is 6MPa, and temperature is 55 ℃; The pressure of separation reactor I I is 6MPa, and temperature is 35 ℃; Under these conditions, supercritical CO 2Fluid extraction 2 hours, finally the material that stays in separation reactor I and separation reactor I I is the active component of unrestraint, in respect of 15g, other deals with; And the raffinate 285g that stays in original extraction kettle is further handled;
(3) in above-mentioned raffinate, add the 1000ml dehydrated alcohol, under 40 ℃ of temperature, carry out solid-liquid concussion extraction, concussion extraction 60 minutes, repeat again once, amount to 2 hours, merge alcohol extraction liquid twice, reclaim alcohol solvent with rotary evaporator, obtain alpha-glucosidase is had the effective site of strong inhibitory activity at last, in respect of 13.1g.
Embodiment 2
The leaching process of present embodiment and step and the foregoing description 1 are identical.Its step is as follows:
(1) at first 300g raw material Chinese medicine cinnamon is pulverized, and sieved, make by 60 mesh sieves; Then this powder material is put into supercritical CO 2Extract supercritical CO in the extraction kettle of fluid extraction device 2Fluid flows into extraction kettle with the flow of 30kg per hour, and the pressure in the extraction kettle remains 30MPa, and temperature remains 45 ℃;
(2) CO 2Fluid enters separation reactor I and separation reactor I I; The pressure of separation reactor I is 8MPa, and temperature is 65 ℃; The pressure of separation reactor I I is 7MPa, and temperature is 45 ℃; Under these conditions, supercritical CO 2Fluid extraction 3 hours, finally the material that stays in separation reactor I and separation reactor I I is the active component of unrestraint, in respect of 16g, other deals with; And the raffinate 284g that stays in the extraction kettle is further handled;
(3) in above-mentioned raffinate, add the 1000ml dehydrated alcohol, under 60 ℃ of temperature, carry out solid-liquid concussion extraction, concussion extraction 75 minutes, repeat again once, amount to 2.5 hours, merge the secondary alcohol extraction liquid, reclaim alcohol solvent with rotary evaporator, obtain alpha-glucosidase is had the effective site of strong inhibitory activity at last, in respect of 15.1g.
Chinese medicine cinnamon extract by gained in the foregoing description is described below in external inhibition test to alpha-glucosidase:
In test tube, successively add pH and be 6.8 kaliumphosphate buffer 1.2ml, the sweet peptide of each Guang (1mg/ml) 50 μ l, a certain amount of Cortex Cinnamomi extract inhibitor, alpha-glucosidase 2 μ l, 4-Nitrobenzol-alpha-d-galactopy Fructus Vitis viniferae benzene (0.116mol/L) 50 μ l and add mixing in vitro, in 37 ℃ the insulation 10 minutes after, add 10ml sodium carbonate (0.1mol/L) stop buffer, test method is tested in accordance with regulations.End product is as shown in table 1 below:
Table 1 Chinese medicine cinnamon supercritical prepared product suppresses active to alpha-glucosidase
Inhibitor Suppress dosage (μ g) Suppression ratio (%) IC 50(μg/ml)
Cortex Cinnamomi supercritical prepared product 1 22.56 1.637
2 41.43
3 71.53
4 88.47
5 98.57
The Cortex Cinnamomi supercritical extract is described in down the influence test of the inductive blood glucose in diabetic mice value of alloxan Alloxan:
Get Kunming mouse, body weight 20~22g, fasting 12h, lumbar injection Alloxan 200mg/kg normally raises fasting 12h after 3 days, and the venous sinus eye socket is got blood, and centrifuging and taking determination of serum blood glucose value is chosen blood glucose value and is experimentized greater than the above person of 11.1mmol/L.Mice is pressed blood glucose value uniform distribution grouping, and mice is divided into 5 groups, i.e. negative control group, positive controls, Cortex Cinnamomi supercritical extract high dose group, middle dosage group and low dose group.Negative control group is irritated stomach with normal saline, positive controls is irritated stomach acarbose 20mg/kg, high dose group is irritated stomach Cortex Cinnamomi supercritical extract 1g/kg, middle dosage group is irritated stomach Cortex Cinnamomi supercritical extract 0.5g/kg, and low dosage is carefully irritated stomach Cortex Cinnamomi supercritical extract 0.25g/kg, successive administration 10 days, fasting 12h after the last administration, the eye socket venous sinus is got blood, and centrifuging and taking serum is used the determination of glucose oxidase blood glucose value.The results are shown in Table 2.
Table 2 Cortex Cinnamomi supercritical extract is to the inductive diabetic mice of Alloxan
Group Dosage (mg/kg) Sample number (N) Blood glucose value (mmol/L)
Negative control group 0 12 31.74±11.82
Positive controls 20 13 16.68±6.23 *
Cortex Cinnamomi supercritical extract low dose group 250 12 13.26±7.99 *
Dosage group in the Cortex Cinnamomi supercritical extract 500 12 13.30±8.04 *
Cortex Cinnamomi supercritical extract high dose group 1000 12 13.06±3.75 *
Can find out obviously that from table 2 the Cortex Cinnamomi supercritical extract has tangible reduction effect to the blood glucose value of the inductive diabetic mice of Alloxan.This illustrates that it can be used for the exploitation of hypoglycemic medicine.

Claims (1)

1. method of extracting alpha-glucosidase inhibitor from Chinese medicine cinnamon is characterized in that having following technical process and step:
A. the raw material Chinese medicine cinnamon is pulverized, and by 40~80 mesh sieves; Then this powder material is put into supercritical CO 2Extract supercritical CO in the extraction kettle of fluid extraction device 2Fluid flows into extraction kettle with the flow of 25~30kg per hour, and the pressure in the extraction kettle remains 20~30MPa, and temperature remains 35~45 ℃;
B.CO 2Fluid enters separation reactor I and separation reactor I I; The pressure of separation reactor I is 6~8MPa, and temperature is 55~65 ℃; The pressure of separation reactor I I is 6~7MPa, and temperature is 35~45 ℃; Under these conditions, supercritical CO 2Fluid extraction 2~3 hours, finally the material that stays in separation reactor I and separation reactor I I is the active component of unrestraint, other deals with; And the raffinate that stays in original extraction kettle is further handled;
C. in above-mentioned raffinate, add dehydrated alcohol and under 40~60 ℃ of temperature, carry out solid-liquid concussion extraction, concussion extraction 60~80 minutes, repeat again once, merge alcohol extraction liquid twice, reclaim alcohol solvent with rotary evaporator, obtain alpha-glucosidase is had the effective site of strong inhibitory activity at last.
CNB2006100232803A 2006-01-12 2006-01-12 Method for extracting alpha- glucosidase inhibitor from traditional Chinese cinnamomum cassia Expired - Fee Related CN100408054C (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101167802B (en) * 2006-10-25 2011-04-20 中国科学院上海生命科学研究院 Method for preparing cinnamon extraction, cinnamon extraction and its composition and use
CN101530469B (en) * 2009-04-20 2011-10-05 孙益民 Method for preparing effective component group of water soluble Chinese cassia tree
CN101785802B (en) * 2009-01-22 2011-11-23 上海中医药大学 Cinnamomum japonicum phenolic compound and preparation method and application thereof
CN102274244A (en) * 2011-07-14 2011-12-14 中国药科大学 Cassia bark polyphenol extract and preparation method and application thereof
CN103221059A (en) * 2010-11-23 2013-07-24 地塞医药有限公司 Substantially coumarin-free extract of cinnamon and its production method
CN106361994A (en) * 2016-10-25 2017-02-01 四川大学 Alpha-glucosidase activity inhibition component in habenaria ciliolaris kranzl, and preparation method and application of alpha-glucosidase activity inhibition component
CN110384729A (en) * 2019-09-02 2019-10-29 江西省科学院生物资源研究所 Lignum cinnamomi camphorae extract is inhibiting the application in glycohydrolase activity
CN113142579A (en) * 2020-01-22 2021-07-23 广涵科技有限公司 Method for preparing cinnamon extraction powder and cinnamon extraction powder

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000306311A (en) * 1999-04-19 2000-11-02 Pioneer Electronic Corp Reproduction apparatus

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101167802B (en) * 2006-10-25 2011-04-20 中国科学院上海生命科学研究院 Method for preparing cinnamon extraction, cinnamon extraction and its composition and use
CN101785802B (en) * 2009-01-22 2011-11-23 上海中医药大学 Cinnamomum japonicum phenolic compound and preparation method and application thereof
CN101530469B (en) * 2009-04-20 2011-10-05 孙益民 Method for preparing effective component group of water soluble Chinese cassia tree
CN103221059A (en) * 2010-11-23 2013-07-24 地塞医药有限公司 Substantially coumarin-free extract of cinnamon and its production method
CN102274244A (en) * 2011-07-14 2011-12-14 中国药科大学 Cassia bark polyphenol extract and preparation method and application thereof
CN102274244B (en) * 2011-07-14 2012-11-28 中国药科大学 Cassia bark polyphenol extract and preparation method and application thereof
CN106361994A (en) * 2016-10-25 2017-02-01 四川大学 Alpha-glucosidase activity inhibition component in habenaria ciliolaris kranzl, and preparation method and application of alpha-glucosidase activity inhibition component
CN106361994B (en) * 2016-10-25 2019-07-05 四川大学 Alpha-glucosidase activity constituents for suppressing in Habenaria Ciliolaris Kranzl and its preparation method and application
CN110384729A (en) * 2019-09-02 2019-10-29 江西省科学院生物资源研究所 Lignum cinnamomi camphorae extract is inhibiting the application in glycohydrolase activity
CN113142579A (en) * 2020-01-22 2021-07-23 广涵科技有限公司 Method for preparing cinnamon extraction powder and cinnamon extraction powder

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