CN101804087B - Burdock concocting method and concocting product thereof - Google Patents
Burdock concocting method and concocting product thereof Download PDFInfo
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- CN101804087B CN101804087B CN2010101427203A CN201010142720A CN101804087B CN 101804087 B CN101804087 B CN 101804087B CN 2010101427203 A CN2010101427203 A CN 2010101427203A CN 201010142720 A CN201010142720 A CN 201010142720A CN 101804087 B CN101804087 B CN 101804087B
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Abstract
The invention relates to a burdock concocting method and a concocting product thereof. The method comprises the following steps: a) taking burdock raw materials with the properties, the microscopic features and the arctiin content conforming to the requirements of Chinese Pharmacopoeia, removing impurities and dust, cleaning the materials, and then drying the materials to obtain clean materials; b) transferring the clean materials into a medicine frying machine to be fried; and (c) discharging the materials after the frying is completed, and sieving the dust. The initial temperature of the medicine frying machine in the frying step is 100 DEG C, the temperature is uniformly improved to the frying temperature of 200 to 300 DEG C in 1 minute, the rotating speed of the medicine frying machine in the temperature rising process is 16 r/min, the rotating speed of the medicine frying machine after the frying temperature is reached is 32 r/min, and the total frying time is between 2 and 8 minutes. The properties of herbal pieces of burdock concocting products prepared by the method of the invention conform to the specification, the content of active ingredients does not have obvious difference from that of raw materials, in addition, the content of cold and cool ingredients after the heating and frying is reduced, and the medicine property is moderate. In addition, the content of fatty oil in the burdock concocting products prepared by the method of the invention is reduced, so the lubricating effect is inhabited.
Description
Technical field:
The present invention relates to the field of Chinese medicines, specifically, the present invention relates to a kind of Fructus Arctii concocting method and processed product thereof.
Background technology:
In recent years, along with the continuous propelling of the modernization of Chinese medicine, the research of Chinese medicine, exploitation and production have obtained development rapidly.Plantation at Chinese crude drug has been promoted " Chinese crude drug quality of production management regulation " (GAP); Complete GMP authentication and control measures have been set up in important production aspect; The research of chemical composition of Chinese materia medica and material base has obtained the development of advancing by leaps and bounds, and from Chinese medicine, find and develop new drug is hot research both domestic and external field always.But be in the state that relatively lags behind as the processing procedure of the decoction pieces of Chinese medicine preparation production important intermediate and the research of quality standard; And the process of preparing Chinese medicine of Chinese medicine is the important critical process that embodies the Chinese medicine characteristic, will have influence on the modernization with Chinese medicine that further develops of Chinese medicine to the ignorance of prepared slice quality.Though " Chinese medicine processing standard " issued in national each province and city in succession; Because of the difference of medical material kind, the place of production, process of preparing Chinese medicine season, processing procedure condition; And do not have unified processing standard, and can cause obscuring of medical material kind and decoction pieces kind, the quality of decoction pieces can't be guaranteed.Although the current prepared slices of Chinese crude drugs have been set up some standards; But because technical conditions fall behind; Also there is sizable gap with current international practice standard and market demands; Especially kind is chaotic, the concocting method variation, and no standard or standard backwardnesss are the main causes that restricts prepared slices of Chinese crude drugs industry and even Chinese medicine industry health, sustainable development at present.On prepared slices of Chinese crude drugs concocted specification, national standard and provincial standard disunity, standard also lacks restraining forces and authority, has caused managerial confusion, is unfavorable for very much the production of Chinese medicine, even causes influence treatment, the serious consequence of curative effect.Therefore, must accelerate to set up the production standard and the quality standard of the high-quality prepared slices of Chinese crude drugs.
Fructus Arctii is the dry mature fruit of feverfew Fructus Arctii Arctium lappa L., has dispelling wind and heat pathogens, lung qi dispersing rash, the effect of resolving toxin and disinhibiting the throat; Be used for anemopyretic cold, cough with copious phlegm, measles, rubella; Laryngopharynx swelling and pain, the mumps erysipelas, carbuncle sore tumefacting virus all has distribution throughout the country.
Modern age, pharmacological research found that Fructus Arctii had effects such as antibiotic, antiviral, raise immunity, blood sugar lowering, changes of anti-nephropathy, anti-tumor mutation, and bibliographical information Arctiin and aretigenin are arranged is its main active.The document of comprehensive nearly recent decades can be found out; Puppet article to the research of Fructus Arctii mainly concentrates on Fructus Arctii are differentiated, in the Fructus Arctii medical material pharmacological research and the Fructus Arctii Decoction of active component in the discussion aspect the clinical practice; Constantly find with its new chemical constituent and pharmacologically active, with further researching and developing foundation is provided for clinical practice.But relevant Fructus Arctii processing procedure, prepared slice quality standard criterion, plurality of active ingredients are extracted, the research report of separation method is few.China's Fructus Arctii aboundresources, Fructus Arctii should obtain effective development and utilization.
Summary of the invention:
First technical problem to be solved by this invention is to provide a kind of Fructus Arctii concocting method, to improve the quality of existing Fructus Arctii processed product.
Second technical problem to be solved by this invention is to provide a kind of Fructus Arctii processed product, to improve the quality and the curative effect of Chinese medicine finished product.
Technical problem to be solved by this invention can be able to solve through following technical scheme:
As first aspect present invention, a kind of Fructus Arctii concocting method, said method comprises the steps:
A) get character, microscopic features, Arctiin content and meet that " the raw material Fructus Arctii that Chinese pharmacopoeia requires is removed impurity and ash bits, cleans, and drying is totally expected then;
B) will totally expect to be transferred in the medicine roasting machine, fry; With
C) fry and finish the back discharging and sieve the dedust bits.
It is characterized in that: said initial temperature of frying medicine roasting machine in the step is 100 ℃; At the uniform velocity be warming up in 1 minute and fry temperature 200-300 ℃; The reversal rate of medicine roasting machine is 16r/min in the temperature-rise period; Reach and fry that the reversal rate of medicine roasting machine is 32r/min after the temperature, always the time of frying is 2-8 minute.
The preferred said temperature of frying of frying in the step is 300 ℃, and always the time of frying is 3-5 minute.
Used term " is always fried the time " to the heating-up time and is added constant temperature time in this civilization.
As second aspect present invention, a kind of Fructus Arctii processed product, said processed product adopt Fructus Arctii concocting method of the present invention to concoct and form.
The decoction pieces character of the Fructus Arctii processed product through the inventive method preparation is up to specification, and content of effective has significant difference and fry its cold and cool composition of back through heating not reduce to some extent than raw material, has relaxed the property of medicine.In addition, reduce, thereby suppressed the property of sliding profit through the fatty oil content in the Fructus Arctii processed product of the inventive method preparation.The present invention is through setting a temperature-rise period and an isothermal process in the process of frying; Avoided the inhomogeneous and hot-spot of being heated of Fructus Arctii, through when heating up, lower reversal rate being set higher reversal rate has been set in isothermal process simultaneously and further guarantees being heated evenly of Fructus Arctii.
Description of drawings
Fig. 1 is the HPLC chromatogram of Arctiin reference substance;
Fig. 2 is the HPLC chromatogram of aretigenin reference substance;
Fig. 3 is the HPLC chromatogram of Fructus Arctii processed product in the embodiment of the invention 6.
The specific embodiment
For technological means, creation characteristic that the present invention is realized, reach purpose and effect and be easy to understand and understand, below in conjunction with concrete example, further set forth the present invention.
According to " the following requirement to the raw material Fructus Arctii in the Chinese pharmacopoeia is screened:
Character: long inverted ovoid, slightly flat, microbend, long 5-7mm, wide 2-3mm.The surface taupe, band atropurpureus speckle has several vertical ribs, and usually middle 1-2 bar is more obvious.The blunt circle in top, wide slightly, end face has annulus, middle tool point-like style vestiges; Base portion is slightly narrow, and the areloe color is lighter.Peel is harder, cotyledon yellowish white, rich oil property.Feeble QI, little bitter little suffering in back and numb tongue.The powder taupe.The endocarp stone cell is slightly flat, and the surface is seen and is sharp fusiformis, oblong or sharp oval, inlays closely; Norma lateralis rectangle like or strip, curved slightly partially, long 70-224 μ m, wide 13-70 μ m, wall thickness be approximately to 20 μ m, lignify, pit is grown crosswise.A type polygon is seen in mesocarp reticulated cell transverse section, and anticlinal wall tool choice refreshments shape thickens: vertical section is seen cell elongation, the reticular texture of the fine and closely woven intersection of wall tool.Prism of calcium oxalate diameter 3-9 μ m is present in the xanchromatic mesocarp parenchyma cell crystal cell boundary fuzzy in flakes.Cotyledon cell is full of aleurone grain, and tiny cluster crystal and fatty oil droplet are arranged in the aleurone grain that has.
Total ash: according to " inspection of an appendix IX of Chinese pharmacopoeia version in 2005 K-method must not cross 7.0%.
Acid-insoluble ash: according to " inspection of an appendix IX of Chinese pharmacopoeia version in 2005 K-method must not cross 2.0%.
Arctiin content: measure Arctiin (C according to HPLC (Chinese Pharmacopoeia version appendix in 2005 VID)
27H
340
11) must not be less than 5.0%, wherein the test of chromatographic condition and system suitability is according to carrying out as follows:
With the octadecyl silane is filler; Second eyeball one water (27: 73) is mobile phase; The detection wavelength is 280nm, and number of theoretical plate calculates by the Arctiin peak and is not less than 1500.
The preparation of reference substance solution: precision weighing Arctiin 6.5mg puts in the 10ml measuring bottle, adds dissolve with methanol and is diluted to scale, shakes up, and promptly gets.
The preparation of need testing solution: sample thief powder (crossing 40 mesh sieves) 0.5g, the accurate title, decide, and places the 50ml measuring bottle; Add methanol 50ml, supersound process (power 150W, frequency 20kHz) 30min adds methanol to scale, shakes up, and filters, and gets subsequent filtrate, and filtering with microporous membrane promptly gets.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly get.
Embodiment 2
(place of production: Zhejiang, total ash are 5.36% weight, and sour ash is 1.10% with the raw material Fructus Arctii; The sweet content of Fructus Arctii is 7.56% weight) remove impurity and ash bits, wash in a pan only, take out; Drying is transferred in 100 ℃ the medicine roasting machine then, at the uniform velocity is warming up in 1 minute and fries 200 ℃ of temperature; The reversal rate of medicine roasting machine is 16r/min in the temperature-rise period, reaches to fry that the reversal rate of medicine roasting machine is 32r/min after the temperature, and always the time of frying is 3 minutes.After finishing to fry, take out and sieve dedust bits, obtain the Fructus Arctii processed product.Take a sample and seal and test in order to the road, back.
Embodiment 3-10
Fry step parameter reference implementation example 2 according to listed in the table 1 and carry out embodiment 3-10 and prepare the Fructus Arctii processed product, and sampling and testing, test result is seen table 8.
Fry step parameter among the table 1 embodiment 2-10
Embodiment | Fry temperature (℃) | Always fry the time (min) |
2 | 200 | 3 |
3 | 200 | 5 |
4 | 200 | 8 |
5 | 300 | 3 |
6 | 300 | 5 |
7 | 300 | 8 |
8 | 400 | 3 |
9 | 400 | 5 |
10 | 400 | 8 |
According to the Fructus Arctii processed product that obtains among the embodiment 2-10 is carried out the analysis of property of medicine component content.
1, instrument and reagent
Agillent1100serie: high performance liquid chromatograph comprises modular pump, UV-detector, Agillent chromatographic work station (U.S. Agillent company limited); BP211D type electronic balance (100,000/, German Sartorius company).SK5200LH type Ultrasound Instrument (Shanghai High Kudos Science Instrument Co., Ltd.).
Arctiin reference substance (819-9401) is provided by Nat'l Pharmaceutical & Biological Products Control Institute.The aretigenin reference substance is 99.11% for self-control through the HPLC purity check.Agents useful for same is chromatographically pure, and water is redistilled water.
2, chromatographic condition
Chromatographic column: Hypersil BDS C18 (4.6mm * 250mm, 5 μ m); Mobile phase: methanol: water (1: 1.2); Flow velocity: 1.0ml/min; Detect wavelength: 280nm; Column temperature: 25 ℃.Theoretical cam curve must not be lower than 3000 in Arctiin.
With this understanding, other compositions in the sample can obtain baseline separation with other chromatographic peaks to Arctiin and aretigenin peak, and other compositions in the sample do not disturb the mensuration of Arctiin and aretigenin.
3, the preparation of reference substance solution
Accurately respectively take by weighing Arctiin reference substance 6.17mg and the arctigenin reference substance 4.7mg that is dried to constant weight, put respectively in 10ml and the 50ml volumetric flask, add dissolve with methanol and fixed moltenly get final product to scale.
4, the preparation of need testing solution
Get the Fructus Arctii processed product, pulverize, cross 60 mesh sieves, get about 0.5 gram, accurate title is fixed, adds the about 45ml of methanol, and supersound process 25 minutes is taken out, and filters, and filtrating deciding dissolves to the 50ml measuring bottle, adds methanol to scale, shakes up, and promptly gets.
5, linear relationship is investigated
Accurate each 2ul of absorption Arctiin reference substance solution (0.617mg/ml), 4ul, 6ul, 8ul, 10ul, 12ul inject high performance liquid chromatograph respectively, by above-mentioned chromatographic condition, measure peak area.With the sample size is abscissa, and peak area is a vertical coordinate, calculates regression equation to be: Y=588.4153X-25.1997, r=0.9998 sees table 2.
The table 2 Arctiin range of linearity is investigated
Sample size (μ g) | 1.234 | 2.468 | 3.702 | 4.936 | 6.170 | 7.404 |
Peak area | 703.96 | 1432.10 | 2135.68 | 2886.61 | 3607.22 | 4216.97 |
The result shows: the Arctiin sample size is in 1.234-7.404 μ g scope, and linear relationship is good.
Accurate each 2ul of absorption aretigenin reference substance solution (0.094mg/ml), 4ul, 6ul, 8ul, 10ul, 12ul inject high performance liquid chromatograph respectively, by above-mentioned chromatographic condition, measure peak area.With the sample size is abscissa, and peak area is a vertical coordinate, calculates regression equation to be: Y=85.6527X-13.3329, r=0.9999.Measure the result and see table 3.
The table 3 aretigenin range of linearity is investigated
Sample size (μ g) | 0.188 | 0.376 | 0.564 | 0.752 | 0.940 | 1.128 |
Peak area | 162.00 | 329.07 | 495.72 | 669.27 | 847.96 | 989.53 |
The result shows: the aretigenin sample size is in 0.188-1.128 μ g scope, and linear relationship is good.
6, precision test
Under the above-mentioned chromatographic condition, get need testing solution, continuous sample introduction 5 times, each 5ul, with the quadrat method deal with data, the RSD of Arctiin peak area is 0.78% as a result, the RSD of aglycon peak area is 0.27%, sees table 4, shows that the precision of this method is good.
The precision test of table 4 Arctiin and aretigenin
|
1 | 2 | 3 | 4 | 5 | RSD(%) |
The Arctiin peak area | 2365.52 | 2408.25 | 2410.53 | 2406.99 | 2395.46 | 0.78 |
The aretigenin peak area | 102.56 | 102.54 | 101.98 | 102.24 | 102.68 | 0.27 |
7, repeatability test
Get same confession test agent, press the content assaying method operation, carry out 5 parallel laboratory tests, the result shows that the RSD of Arctiin and aretigenin peak area is respectively 0.79% and 1.0%, sees table 5, shows that repeatability is good.
The repeatability test of table 5 Arctiin and aretigenin
|
1 | 2 | 3 | 4 | 5 | RSD(%) |
The Arctiin peak area | 2077.28 | 2068.63 | 2038.37 | 2045.54 | 2056.48 | 0.79 |
The aretigenin peak area | 158.59 | 160.60 | 157.68 | 161.59 | 158.46 | 1.0 |
8, stability test
At ambient temperature, the same need testing solution of accurate absorption is pressed the sample determination method respectively 0,2, measures peak area in 4,6,8,10 hours.The result shows that chromatographic peak did not have significant change in 10 hours, explains that Arctiin and aretigenin are stable in 10h, and the result sees table 6.
The stability test of table 6 sample solution
Time (h) | 0 | 2 | 4 | 6 | 8 | 10 | RSD(%) |
The Arctiin peak area | 2349.58 | 2346.55 | 2369.56 | 2353.12 | 2335.52 | 2341.61 | 0.49 |
The aretigenin peak area | 145.90 | 144.46 | 146.35 | 145.06 | 146.84 | 147.56 | 0.78 |
9, average recovery test
Adopt the application of sample absorption method; Precision takes by weighing the Fructus Arctii sample (containing Arctiin 8.10%, aretigenin 0.38%) of known content, adds Arctiin 10ml (1.72mg/ml) and aglycon reference substance 2ml (0.365mg/ml) respectively; Measure by the sample determination method; Calculate recovery rate, the average recovery rate of Arctiin is 98.74% as a result, RSD is 0.42% (n=5); The average recovery rate of aretigenin is 98.54%, and RSD is 1.95% (n=5), sees table 7, shows that the response rate of this method is good.
The average recovery result of the test of table 7 Arctiin and aretigenin
10, sample size is measured
Get need testing solution through 0.45 μ m filtering with microporous membrane, the accurate 5ul that draws injects high performance liquid chromatograph, by above-mentioned chromatographic condition analysis, measures the chromatographic peak area of Arctiin and aretigenin, calculates content, and test result is seen table 8 and Fig. 1-9.
Fry property of medicine component content in technological parameter and the processed product among each embodiment of table 8
Embodiment | Fry temperature (℃) | Always fry the time (min) | Arctiin content (%) | Aretigenin content (%) | Total content (%) |
2 | 200 | 3 | 6.02 | 0.49 | 6.51 |
3 | 200 | 5 | 6.16 | 0.44 | 6.6 |
4 | 200 | 8 | 6.17 | 0.53 | 6.7 |
5 | 300 | 3 | 5.79 | 0.68 | 6.47 |
6 | 300 | 5 | 5.41 | 0.76 | 6.17 |
7 | 300 | 8 | 3.77 | 0.95 | 4.72 |
8 | 400 | 3 | 4.73 | 0.7 | 5.43 |
9 | 400 | 5 | 1.75 | 0.81 | 2.56 |
10 | 400 | 8 | 0 | 0.74 | 0.74 |
Can find out that from table 7 compare with the raw material Fructus Arctii, the content of Arctiin all has reduction; Explain that the parch heating can make Arctiin receive destruction in various degree, frying temperature when being 400 ℃ especially, the content loss of Arctiin is very big; And in the time of 200-300 ℃, the loss of Arctiin is less.Arctiin is the main effective ingredient that Fructus Arctii plays cold and cool effect, through concocting, suitably reduces its content, relaxes the property of medicine, thus outstanding others.And all corresponding increase of the content of aretigenin, this is because heating is ruptured the glycosidic bond of part Arctiin, sloughs the cause that sugar becomes aretigenin.
Find also during embodiment of the present invention that the character of the Fructus Arctii processed product that when frying for 200 ℃, obtains is not as the character of the Fructus Arctii processed product of acquisition in the time of 300 ℃.
More than show and described ultimate principle of the present invention, principal character and advantage of the present invention.The technical staff of the industry should understand; The present invention is not restricted to the described embodiments; That describes in the foregoing description and the description just explains principle of the present invention; The present invention also has various changes and modifications under the prerequisite that does not break away from spirit and scope of the invention, and these variations and improvement all fall in the scope of the invention that requires protection.The present invention requires protection domain to be defined by appending claims and equivalent thereof.
Claims (3)
1. Fructus Arctii concocting method, said method comprises the steps:
A) get character, microscopic features, Arctiin content and meet that " the raw material Fructus Arctii that Chinese pharmacopoeia requires is removed impurity and ash bits, cleans, and drying is totally expected then;
B) will totally expect to be transferred in the medicine roasting machine, fry; With
C) fry and finish the back discharging and sieve the dedust bits;
It is characterized in that: said initial temperature of frying medicine roasting machine in the step is 100 ℃; At the uniform velocity be warming up in 1 minute and fry temperature 200-300 ℃; The reversal rate of medicine roasting machine is 16r/min in the temperature-rise period; Reach and fry that the reversal rate of medicine roasting machine is 32r/min after the temperature, always the time of frying is 2-8 minute;
The said time of frying always is the heating-up time to add constant temperature time.
2. Fructus Arctii concocting method according to claim 1 is characterized in that:
The said temperature of frying of frying in the step is 300 ℃, and always the time of frying is 3-5 minute.
3. a Fructus Arctii processed product is characterized in that said Fructus Arctii processed product adopts each described Fructus Arctii concocting method preparation among the claim 1-2.
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CN1569138A (en) * | 2004-05-13 | 2005-01-26 | 上海交通大学 | Preparation method of arctium fruit extract for decreasing blood sugar |
CN201044820Y (en) * | 2006-12-29 | 2008-04-09 | 成都中医药大学 | Apparatus for detecting duration of Chinese medicine process |
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CN1569138A (en) * | 2004-05-13 | 2005-01-26 | 上海交通大学 | Preparation method of arctium fruit extract for decreasing blood sugar |
CN201044820Y (en) * | 2006-12-29 | 2008-04-09 | 成都中医药大学 | Apparatus for detecting duration of Chinese medicine process |
Non-Patent Citations (2)
Title |
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刘彬彬等.牛蒡子炮制的历史沿革及现况研究.《山西医药杂志》.2005,第34卷(第6期),443-445. * |
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