CN106568856B - A kind of fingerprint atlas detection method of Pasania cuspidata leaf effective-part - Google Patents
A kind of fingerprint atlas detection method of Pasania cuspidata leaf effective-part Download PDFInfo
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Abstract
The invention discloses a kind of fingerprint atlas detection methods of Pasania cuspidata leaf effective-part.It is related to traditional Chinese medicine quality control method.Fingerprint atlas detection method the following steps are included: reference substance solution preparation；The preparation of test solution；Chromatographic column is using octadecyl silane as filler；Using gradient elution, mobile phase is the gradient eluent that methanol and 0.1% formic acid form, and column temperature is 25 DEG C；Ultraviolet detection wavelength is 285nm；Time is 140min；High performance liquid chromatography measures finger-print.This method can be efficiently used for the quality control of Pasania cuspidata leaf.
Description
Technical field
The present invention relates to Chinese medical extract and its method of quality control, and in particular to the fingerprint image of Pasania cuspidata leaf effective-part
The foundation of spectrum detection method.
Background technique
Pasania cuspidata derives from Fagaceae Lithocarpus Lithocarpus polystachyus (Wall.) Rehd., You Mingduo
Fringe Shi Ke, multiple ear lithocarpus；Because leaf chew it is pleasantly sweet, it is therefore named be Sweet tea, be known as hydrangeae dulcis folium in Guizhou, it is thick to be known as great Ye in Guangdong
Son.Each provinces and regions are distributed on the south China the Changjiang river, especially with Wuyi Mountain be distributed it is most wide, in addition, the resource-savings such as osmanthus, Hunan, Anhui most
It is abundant, wherein the about hundreds of tons of resource storage in Guangxi (osmanthus).In Guangdong, cloud, river, Fujian etc., resource-savings amount is taken second place.India, it is safe
Also there is a little distribution in state.
Pasania cuspidata be it is a kind of have both medicine, tea, sugared three kinds of functions medical and edible dual purpose plant, civil that its tender leaf is often taken to make tea, tea
Coloured gold Huang is bright-coloured, and slightly bitterness, persistent aftertaste, ancients are usually used in clear heat and quench one's thirst in taste sweet tea.Containing up in Pasania cuspidata leaf
10% high sugariness, non-sugar sweetener low in calories, sweet ingredient is mainly dihydrochalcone-type phloridzin, 3- hydroxyl root skin
Glycosides, trifloroside etc..
Pasania cuspidata leaf has the functions such as hypoglycemic, lipid-loweringing, anti-oxidant, modern research shows that its flavonoids abundant for being rich in
Ingredient is its principle active component.For the quality standard for further improving Pasania cuspidata, at the same it is unstable to explore pharmacological evaluation early period
The research to the finger-print of its effective component is unfolded in fixed reason, this experiment.
Summary of the invention
The purpose of the present invention is establish the detection method of Pasania cuspidata leaf effective-part HPLC finger-print.
Used technical solution to achieve the object of the present invention: the effective portion of Pasania cuspidata leaf is established with high performance liquid chromatography
The fingerprint atlas detection method of position, specifically comprises the following steps:
1. the preparation of reference substance solution: precision weighs 3-OH phloridzin reference substance, and 50% ethyl alcohol is added and is dissolved, is made into
Concentration is the solution of 0.50mg/mL, as reference substance solution；
2. the preparation of test solution: taking Pasania cuspidata leaf medicinal material, beat powder, and cross No. two sieves, accurately weigh 5.00g, place
In 125mL stuffed conical flask, the ethyl alcohol for measuring 40mL50% is added thereto, and is placed in thermostat water bath, and 80 DEG C are heated back
Stream extracts 60min, continuous to extract three times, extracting solution will finally be uniformly mixed, and let cool three times, filters, by filtrate constant volume in 250mL
In measuring bottle, take appropriate, cross 0.45 μm of miillpore filter, subsequent filtrate be placed in liquid phase bottle to get；
3. chromatographic condition: chromatographic column is using octadecylsilane chemically bonded silica as filler, and using gradient elution, mobile phase is first
The gradient eluent of alcohol and formic acid composition, column temperature is 20~30 DEG C；Ultraviolet detection wavelength: 200~400nm；
4. measurement: precision is drawn test solution injection high performance liquid chromatograph and is obtained according to high effective liquid chromatography for measuring
Finger-print.
Further preferred method can be implemented by following step:
1. the preparation of reference substance solution: precision weighs 3-OH phloridzin 10.05mg, and 50% ethyl alcohol is added and is dissolved, fixed
It is dissolved in 10mL volumetric flask, precision pipettes the above-mentioned solution of 1mL, and in 10mL volumetric flask, be made into concentration is 50% ethyl alcohol constant volume
The solution of 0.1005mg/mL；Precision weighs phloridzin 5.00mg, and 50% ethyl alcohol is added and is dissolved, constant volume is in 10mL volumetric flask
In, be made into concentration be 0.50mg/mL solution to get；
2. the preparation of test solution: taking lot number is 20140815 Pasania cuspidata leaf medicinal material, beats powder, and crosses No. two sieves, quasi-
5.00g really is weighed, is placed in 125mL stuffed conical flask, the ethyl alcohol for measuring 40mL50% is added thereto, and is placed in water bath with thermostatic control
In pot, 80 DEG C of heating and refluxing extraction 60min are continuous to extract three times, extracting solution will finally be uniformly mixed, and let cool three times, filter, will
Filtrate constant volume takes appropriate in 250mL measuring bottle, crosses 0.45 μm of miillpore filter, subsequent filtrate be placed in liquid phase bottle to get；
3. chromatographic condition: chromatographic column is using octadecylsilane chemically bonded silica as filler；Using gradient elution, mobile phase is first
The gradient eluent of alcohol and 0.1%~2.0% aqueous formic acid composition, column temperature is 20~30 DEG C；Ultraviolet detection wavelength be 200~
400nm；
4. measurement: precision is drawn test solution injection high performance liquid chromatograph and is obtained according to high effective liquid chromatography for measuring
Finger-print.
The optimal detection method of the present invention can be implemented by following step:
Step 3. in chromatographic condition mobile phase be methanol and 0.1% aqueous formic acid composition gradient eluent, column temperature is
25 DEG C, Detection wavelength 254nm, flow velocity 0.8mL/min；Analysis time is 140min.
3. gradient elution described in chromatographic condition, gradient elution program are configured with following volumetric concentration and are carried out step:
At 0 minute, the methanol solution that mobile phase A is 18%, 0.1% aqueous formic acid that Mobile phase B is 82%；
At 20 minutes, the methanol solution that mobile phase A is 35%, 0.1% aqueous formic acid that Mobile phase B is 65%；
At 60 minutes, the methanol solution that mobile phase A is 35%, 0.1% aqueous formic acid that Mobile phase B is 65%；
At 120 minutes, the methanol solution that mobile phase A is 60%, 0.1% aqueous formic acid that Mobile phase B is 40%；
At 140 minutes, the methanol solution that mobile phase A is 60%, 0.1% aqueous formic acid that Mobile phase B is 40%.
Specifically it see the table below:
The detection method of Pasania cuspidata leaf effective-part finger-print, specifically comprises the following steps:
1. the preparation of reference substance solution: precision weighs 3-OH phloridzin 10.05mg, and 50% ethyl alcohol is added and is dissolved, fixed
It is dissolved in 10mL volumetric flask, precision pipettes the above-mentioned solution of 1mL, and in 10mL volumetric flask, be made into concentration is 50% ethyl alcohol constant volume
The solution of 0.1005mg/mL；Precision weighs phloridzin 5.00mg, and 50% ethyl alcohol is added and is dissolved, constant volume is in 10mL volumetric flask
In, be made into concentration be 0.50mg/mL solution to get；
2. the preparation of test solution: taking lot number is 20140815 Pasania cuspidata leaf medicinal material, beats powder, and crosses No. two sieves, quasi-
5.00g really is weighed, is placed in 125mL stuffed conical flask, the ethyl alcohol for measuring 40mL50% is added thereto, and is placed in water bath with thermostatic control
In pot, 80 DEG C of heating and refluxing extraction 60min are continuous to extract three times, extracting solution will finally be uniformly mixed, and let cool three times, filter, will
Filtrate constant volume takes appropriate in 250mL measuring bottle, crosses 0.45 μm of miillpore filter, subsequent filtrate be placed in liquid phase bottle to get；
3. chromatographic condition: chromatographic column is using octadecylsilane chemically bonded silica as filler；Using gradient elution, mobile phase is first
The gradient eluent of alcohol and 0.1%~2.0% aqueous formic acid composition, column temperature is 20~30 DEG C；Ultraviolet detection wavelength be 200~
400nm；
4. measurement: precision is drawn test solution injection high performance liquid chromatograph and is obtained according to high effective liquid chromatography for measuring
Finger-print.
There are 10 features to share peak in the finger-print, wherein No. 3 chromatographic peaks are 3-OH phloridzin, highest peak is No. 6
Chromatographic peak, and referring to peak phloridzin, map total length is 140min, it is specific as follows:
According to thering are 10 features to share peak in Pasania cuspidata leaf effective-part finger-print obtained by the present invention, wherein No. 3 chromatographies
Peak is 3-OH phloridzin, and highest peak is No. 6 chromatographic peaks, and referring to peak phloridzin, map total length is 140min, wherein unimodal
The super total peak area 2% of area has 7, they are 1,3,5,6,7,8, No. 9 peaks, wherein the super total peak area 10% of unimodal area
There is 1, they are No. 6 chromatographic peaks, wherein the super total peak area 15% of unimodal area has 1, they are No. 6 chromatographic peaks, wherein
The unimodal super total peak area 20% of area has 1, they are No. 6 chromatographic peaks.
It is specific as follows:
No. 1 peak, Average residence time RT are 33.20min, and RSD 0.41%, peak area 292467.2, RSD is
34.25%；
No. 2 peaks, Average residence time RT are 38.35min, and RSD 0.35%, peak area 159295.1, RSD is
48.19%；
No. 3 peaks, Average residence time RT are 40.84min, and RSD 0.90%, peak area 551159.5, RSD is
26.29%；
No. 4 peaks, Average residence time RT are 46.65min, and RSD 0.92%, peak area 166383.2, RSD is
24.90%；
No. 5 peaks, Average residence time RT are 48.64min, and RSD 0.65%, peak area 669754.3, RSD is
43.54%；
No. 6 peaks, Average residence time RT are 61.09min, and RSD 0.76%, peak area 6032428.7, RSD is
34.22%；
No. 7 peaks, Average residence time RT are 68.70min, and RSD 0.65%, peak area 555096.1, RSD is
32.46%；
No. 8 peaks, Average residence time RT are 72.24min, and RSD 0.66%, peak area 212800.3, RSD is
44.16%；
No. 9 peaks, Average residence time RT are 90.31min, and RSD 0.45%, peak area 503140.4, RSD is
32.30%；
No. 10 peaks, Average residence time RT are 98.52min, and RSD 0.32%, peak area 105901.2, RSD is
34.59%.
The peak that RT occurs before being 5min is solvent peak.
The principle of the present invention is found from the composition Study of Pasania cuspidata leaf effective-part, and the effective component of Pasania cuspidata leaf is main
For dihydrochalcone glycosides compound, such compound has various bioactivity.Establish Pasania cuspidata leaf effective-part
HPLC fingerprint atlas detection method, it is effective that the finger-print of active component can show Pasania cuspidata leaf from the whole looks upper body of chromatography
Component content situation.Identical, similar fingerprint image can be obtained by being measured with this method from the Pasania cuspidata leaf medicinal material collected on the market
Spectrum.
Beneficial effects of the present invention are as follows:
(1) method provided by the present invention can provide reference to carry out further pharmacology pharmacodynamic experiment, be further
It develops and uses Pasania cuspidata resource and scientific basis is provided.
(2) finger-print focuses on each tandem correlation for constituting fingerprint characteristic peak, focuses on whole facial feature,
Not only it had avoided and has determined the one-sidedness of Pasania cuspidata leaf effective-part ingredient total quality because measuring individualized Xuecheng point, but also reduced
A possibility that processing is thought for requisite quality.
(3) present invention has method simplicity, stablizes, precision height, high repeatability and other advantages.
(4) this method can quickly and accurately identify the true and false superiority and inferiority of product.
Detailed description of the invention
The HPLC finger-print of Fig. 1 Pasania cuspidata leaf effective-part.
The active component characteristic fingerprint pattern of 10 batches of Pasania cuspidata leaves of Fig. 2.
The finger-print of Fig. 3 Pasania cuspidata leaf effective-part HPLC common pattern.
Specific embodiment
In order to further appreciate that feature of the invention, technological means and specific purposes achieved, function, parsing is originally
The advantages of invention and spirit.Detailed description of the invention is further understood by below in conjunction with attached drawing and concrete mode.
Embodiment one: the finger-print of detection Pasania cuspidata leaf effective-part
1. instrument and reagent
1.1 instrument FZ-230 type Universalpulverizers (herding the happy machine tool plant of III and hundred in Wenling city)；A ten thousandth
SartoriusBP110s analyzes electronic balance (German sartorius company)；Ten a ten thousandth Sartorius CP225D analysis
Electronic balance (German sartorius company)；HWS24 type electric-heated thermostatic water bath (the permanent Science and Technology Ltd. in Shanghai one)；DK-
8AD electric-heated thermostatic water bath (Shanghai precision instrumentation Co., Ltd)；SHZ-D (III) circulating water type vacuum pump (Henan Gongyi
Yu Hua instrument plant, city)；Japanese Shimadzu Shimadzu high performance liquid chromatograph (LC-20AT efficient liquid phase pump, SIL-20A automatically into
Sample device, SPD-20A diode array detector, CTO-20A column oven)；Performance liquid chromatographic column: Phenomenex luna
C18 chromatographic column (250mm × 4.6mm, 5 μm), Dikma Diamonsil C18 chromatographic column (250mm × 4.6mm, 5 μm),
Thermo Hypersil Gold C18 chromatographic column (250mm × 4.6mm, 5 μm), Kromasil (C18 250mm × 4.6mm, 5 μ
M) column；
1.2 reagent analysis methanol, acetonitrile (chromatographic grade, Merck KGaA company), (analysis level, Tianjin are big for formic acid, acetic acid
Luxuriant chemical reagent factory), phosphoric acid (analysis level, the huge chemical reagent factory of new east station of Guangzhou), happy treasured pure water.
2. high performance liquid chromatography
2.1 C18 reverse-phase chromatographic column Kromasil (C18 250mm × 4.6mm, 5 μm)；Flow phase system is methanol-
0.1% formic acid system, specific gradient condition such as following table；Column temperature is 25 DEG C,；Flow velocity is 0.8mL/min；Detection wavelength is 254nm,
Sampling volume is 25 μ L；Acquisition time is 140min；
Gradient elution program is as follows:
Condition of gradient elution
The preparation of 2.2 reference substance solutions: precision weighs 3-OH phloridzin 10.05mg, and 50% ethyl alcohol is added and is dissolved, fixed
It is dissolved in 10mL volumetric flask, precision pipettes the above-mentioned solution of 1mL, and in 10mL volumetric flask, be made into concentration is 50% ethyl alcohol constant volume
The solution of 0.1005mg/mL；Precision weighs phloridzin 5.00mg, and 50% ethyl alcohol is added and is dissolved, constant volume is in 10mL volumetric flask
In, be made into concentration be 0.50mg/mL solution to get；
The preparation of 2.3 test solutions: taking lot number is 20140815 Pasania cuspidata leaf medicinal material, beats powder, and crosses No. two sieves, quasi-
5.00g really is weighed, is placed in 125mL stuffed conical flask, the ethyl alcohol for measuring 40mL50% is added thereto, and is placed in water bath with thermostatic control
In pot, 80 DEG C of heating and refluxing extraction 60min are continuous to extract three times, extracting solution will finally be uniformly mixed, and let cool three times, filter, will
Filtrate constant volume takes appropriate in 250mL measuring bottle, crosses 0.45 μm of miillpore filter, subsequent filtrate be placed in liquid phase bottle to get；
2.4 measurements: precision is drawn test solution injection high performance liquid chromatograph and is obtained according to high effective liquid chromatography for measuring
To finger-print, such as Fig. 1.
The finger-print of the active component of two: 10 batches of Pasania cuspidata leaves of embodiment
10 batch of Pasania cuspidata medicinal material is taken, prepares Pasania cuspidata leaf effective-part by one method of embodiment and by one condition of embodiment
It is detected, obtains the HPLC map of 10 batches of samples.By the comparison of 10 batches of HPLC maps, similarity evaluation is carried out, determines its spy
Levy shared peak:
There are 10 features to share peak in finger-print, now by the retention time of map, the average value and total peak of peak area
Area summing, specific as follows:
No. 1 peak, Average residence time RT are 33.20min, and RSD 0.41%, peak area 292467.2, RSD is
34.25%；
No. 2 peaks, Average residence time RT are 38.35min, and RSD 0.35%, peak area 159295.1, RSD is
48.19%；
No. 3 peaks, Average residence time RT are 40.84min, and RSD 0.90%, peak area 551159.5, RSD is
26.29%；
No. 4 peaks, Average residence time RT are 46.65min, and RSD 0.92%, peak area 166383.2, RSD is
24.90%；
No. 5 peaks, Average residence time RT are 48.64min, and RSD 0.65%, peak area 669754.3, RSD is
43.54%；
No. 6 peaks, Average residence time RT are 61.09min, and RSD 0.76%, peak area 6032428.7, RSD is
34.22%；
No. 7 peaks, Average residence time RT are 68.70min, and RSD 0.65%, peak area 555096.1, RSD is
32.46%；
No. 8 peaks, Average residence time RT are 72.24min, and RSD 0.66%, peak area 212800.3, RSD is
44.16%；
No. 9 peaks, Average residence time RT are 90.31min, and RSD 0.45%, peak area 503140.4, RSD is
32.30%；
No. 10 peaks, Average residence time RT are 98.52min, and RSD 0.32%, peak area 105901.2, RSD is
34.59%.
The peak that RT occurs before being 5min is solvent peak.
There are 10 features to share peak in the finger-print of the Pasania cuspidata leaf effective-part, wherein No. 3 chromatographic peaks are 3-OH
Phloridzin, highest peak are No. 6 chromatographic peaks, and referring to peak phloridzin, map total length is 140min, wherein unimodal area is super total
Peak area 2% has 7, they are 1,3,5,6,7,8, No. 9 peaks, wherein the super total peak area 10% of unimodal area has 1, it
Be No. 6 chromatographic peaks, wherein the super total peak area 15% of unimodal area has 1, they are No. 6 chromatographic peaks, wherein unimodal area
Super total peak area 20% has 1, they are No. 6 chromatographic peaks.
Similarity evaluation: the chromatogram of 10 batches of Pasania cuspidata leaf effective-parts is imported into " chromatographic fingerprints of Chinese materia medica similarity
Evaluation system (Chinese Pharmacopoeia committee 2004A editions) ", numerical selection peak (phloridzin) is as referring to peak, such as Fig. 2, it is determined that 10 altogether
There is peak.Control map R is automatically generated using median method Auto-matching, obtains each medicinal material similarity.10 batch Pasania cuspidatas it is similar
Degree is greater than 0.90.It is shown in Table 1.
The similarity of the HPLC finger-print of 1 10 batches of Pasania cuspidata leaf medicinal material active components of table
The finger-print for the Pasania cuspidata leaf effective-part HPLC common pattern established by the above method is as shown in Figure 3.
Some embodiments of the invention above described embodiment only expresses, in this revealed embodiment and all sights
Point should be considered as to illustrate the present invention, and the description thereof is more specific and detailed, and but it cannot be understood as to model of the present invention
The limitation enclosed.It should be pointed out that for those of ordinary skill in the art, in the premise for not departing from present inventive concept
Under, several modifications and improvements can also be gone out, these are all within the scope of protection of the present invention.Therefore protection scope of the present invention should be with
Subject to claim, and cover legal equivalents.
Claims (2)
1. a kind of fingerprint atlas detection method of Pasania cuspidata leaf effective-part comprising following steps:
(1) preparation of reference substance solution: precision weighs 3-OH phloridzin 10.05mg, and 50% ethyl alcohol is added and is dissolved, constant volume in
In 10mL volumetric flask, precision pipettes the above-mentioned solution of 1mL, and in 10mL volumetric flask, be made into concentration is 50% ethyl alcohol constant volume
The solution of 0.1005mg/mL；Precision weighs phloridzin 5.00mg, and 50% ethyl alcohol is added and is dissolved, constant volume is in 10mL volumetric flask
In, be made into concentration be 0.50mg/mL solution to get；
(2) preparation of test solution: taking Pasania cuspidata leaf medicinal material, beats powder, and crosses No. two sieves, accurately weighs 5.00g, is placed in
In 125mL stuffed conical flask, the ethyl alcohol for measuring 40mL 50% is added thereto, and is placed in thermostat water bath, 80 DEG C are heated to reflux
60min is extracted, it is continuous to extract three times, it extracting solution will finally be uniformly mixed, let cool three times, filter, by filtrate constant volume in 250mL amount
In bottle, take appropriate, cross 0.45 μm of miillpore filter, subsequent filtrate be placed in liquid phase bottle to get；
(3) chromatographic condition: chromatographic column is using octadecylsilane chemically bonded silica as filler, and using gradient elution, mobile phase is methanol
With the gradient eluent of 0.1% formic acid composition, column temperature is 25 DEG C；Ultraviolet detection wavelength is 254nm；
The gradient elution, gradient elution program are configured with following volumetric concentration and are carried out:
At 0 minute, the methanol solution that mobile phase A is 18%, 0.1% aqueous formic acid that Mobile phase B is 82%；
At 20 minutes, the methanol solution that mobile phase A is 35%, 0.1% aqueous formic acid that Mobile phase B is 65%；
At 60 minutes, the methanol solution that mobile phase A is 35%, 0.1% aqueous formic acid that Mobile phase B is 65%；
At 120 minutes, the methanol solution that mobile phase A is 60%, 0.1% aqueous formic acid that Mobile phase B is 40%；
At 140 minutes, the methanol solution that mobile phase A is 60%, 0.1% aqueous formic acid that Mobile phase B is 40%；
(4) measure: precision is drawn test solution injection high performance liquid chromatograph and is referred to according to high effective liquid chromatography for measuring
Line map；
There are 10 features to share peak in the finger-print, wherein No. 3 chromatographic peaks are 3-OH phloridzin, highest peak is No. 6 chromatographies
Peak is phloridzin referring to peak, and map total length is 140min, specific as follows:
No. 1 peak, Average residence time RT are 33.20min, RSD 0.41%, peak area 292467.2, RSD 34.25%；
No. 2 peaks, Average residence time RT are 38.35min, RSD 0.35%, peak area 159295.1, RSD 48.19%；
No. 3 peaks, Average residence time RT are 40.84min, RSD 0.90%, peak area 551159.5, RSD 26.29%；
No. 4 peaks, Average residence time RT are 46.65min, RSD 0.92%, peak area 166383.2, RSD 24.90%；
No. 5 peaks, Average residence time RT are 48.64min, RSD 0.65%, peak area 669754.3, RSD 43.54%；
No. 6 peaks, Average residence time RT are 61.09min, and RSD 0.76%, peak area 6032428.7, RSD is
34.22%；
No. 7 peaks, Average residence time RT are 68.70min, RSD 0.65%, peak area 555096.1, RSD 32.46%；
No. 8 peaks, Average residence time RT are 72.24min, RSD 0.66%, peak area 212800.3, RSD 44.16%；
No. 9 peaks, Average residence time RT are 90.31min, RSD 0.45%, peak area 503140.4, RSD 32.30%；
No. 10 peaks, Average residence time RT are 98.52min, and RSD 0.32%, peak area 105901.2, RSD is
34.59%.
2. a kind of fingerprint atlas detection method of Pasania cuspidata leaf effective-part according to claim 1, it is characterised in that:
Step (3) chromatographic condition: flow velocity: 0.8mL/min；Time: 140min；
Step (4) measurement: high performance liquid chromatograph is injected using the accurate 25 μ L of test solution that draws, according to high-efficient liquid phase color
Spectrometry measurement, obtains finger-print.
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| CN2301203Y (en) * | 1997-05-29 | 1998-12-23 | 张传斗 | Pill device |
| CN2494197Y (en) * | 2001-04-05 | 2002-06-05 | 丹东金丸集团有限公司 | Microcapsule filling device |
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| US3535795A (en) * | 1968-09-06 | 1970-10-27 | Varian Associates | Process of drying lithocarpus densiflora rehd. (tanoak) wood with radio wave energy |
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| CN103169782B (en) * | 2013-04-10 | 2015-09-09 | 康美药业股份有限公司 | A kind of tune stomach CHENGQI TANG granule and preparation method thereof and detection method |
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| CN2301203Y (en) * | 1997-05-29 | 1998-12-23 | 张传斗 | Pill device |
| CN2494197Y (en) * | 2001-04-05 | 2002-06-05 | 丹东金丸集团有限公司 | Microcapsule filling device |
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