CN105628834B - Anaesthetic Radix Rhapontici seu Radix Echinopsis spends fingerprint and quality evaluating method - Google Patents
Anaesthetic Radix Rhapontici seu Radix Echinopsis spends fingerprint and quality evaluating method Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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Abstract
The present invention relates to the method for building up that a kind of anaesthetic Radix Rhapontici seu Radix Echinopsis spends finger-print, including:1) preparation of need testing solution:Medicinal powder is taken, in putting 100mL conical flask with cover, plus 70% methyl alcohol, ultrasonic extraction, after being placed into room temperature, then weighed weight, the weight of less loss is supplied with solvent, filter, take filtrate and filtered with 0.45 μm of miillpore filter;2) will need testing solution inject high performance liquid chromatograph in, obtain finger-print, the chromatographic condition for using for:Chromatographic column:Octadecylsilane chemically bonded silica chromatographic column;Mobile phase:The phosphate aqueous solution (B) of acetonitrile (A) 0.2%, using gradient elution 85%B (0min)~78%B (12min)~74%B (13min)~60%B (60min);Testing conditions:DAD detectors, 230~400nm of Detection wavelength;Column temperature:20~40 DEG C;Sample size:5~30 μ L.The present invention also provides a kind of utilization finger-print and evaluates the method that anaesthetic Radix Rhapontici seu Radix Echinopsis spends quality, and the method sensitivity is high, favorable reproducibility;The standard finger-print for being obtained can more comprehensively reflect chemical composition species and quantity contained in Radix Rhapontici seu Radix Echinopsis flower anaesthetic material.
Description
Technical field
The present invention relates to Pharmaceutical Analysis field, and in particular to Fingerprint of Chinese medicine materia method for building up and evaluation of medical materials' quality side
Method.
Background technology
With the fast development of anaesthetic industry, the wild resource day that the reason such as resource irrational utilization and the change of circumstances is brought
The problem that benefit is reduced is highlighted, and seriously constrains the sound development of anaesthetic industry.Picking up from certainly for anaesthetic material uses also very universal, current city
There is the special road native drug of some Mongolian medicines not commodity circulation on field, what is had has the commodity medicinal material of market circulation, but kind
Confusion, infective use is unclear, and this is just rationally effectively caused very big puzzlement using anaesthetic material.Radix Rhapontici seu Radix Echinopsis flower is exactly wherein one
Kind, its homonym phenomenon is very universal, and misapplied equal other plant capitulum is used as medicine more.So selection is a kind of can be fast
Speed, the means that efficiently, comprehensively quality of medicinal material information is covered in reflection are very necessary and important, and fingerprint pattern technology is exactly to accord with
The technological means of these features is closed, and chemical component fingerprint can also differentiate the quality of medicine materical crude slice, can also aid in cultivar identification,
Chinese medicine overall picture can substantially be reflected, the control to Chinese medicine inherent quality is realized.
Anaesthetic Radix Rhapontici seu Radix Echinopsis flower is the drying of composite family Radix Rhapontici seu Radix Echinopsis platymiscium centaurea monanthos Georgi Rhaponticum uniflorum (L.) DC.
Flower.Anaesthetic name:Big vast Gu Er-Zhu Er, are distributed in China Inner Mongol, northeast, Hebei, Shaanxi, Gansu, Qinghai, Shanxi, Henan, four
The ground such as river, Shandong.Entering anaesthetic can kill " viscous ", only shouting pain, heat-clearing, removing toxic substances, inducing diaphoresis etc., cure mainly flu, heart hot dysentery disease, blood-head and biography
Metachromia heat symptom-complex etc..Radix Rhapontici seu Radix Echinopsis flower for Mongolian medicine clinic common medicine, record in《Drug Standard of Ministry of Public Health of the Peoples Republic of China》(anaesthetic point
Volume), but without discriminating, inspection, assay,《Chinese Pharmacopoeia》Only with respect to Radix Rhapontici (root of centaurea monanthos Georgi) in 2015 editions
Method of quality control, but be not particularly suited for Radix Rhapontici seu Radix Echinopsis flower.This not only constrains effective utilization that Radix Rhapontici seu Radix Echinopsis spends resource, cannot also ensure
The security and validity of medication.
The present invention establishes anaesthetic Radix Rhapontici seu Radix Echinopsis flower finger-print first, identifies 8 peaks in 13 total peaks.Research institute uses
HPLC methods it is simple to operate, separating degree is high, favorable reproducibility.The standard finger-print of foundation is typical, comprehensive, representative, can be true
In fact, objectively reflection Radix Rhapontici seu Radix Echinopsis spends type, quantity and the relative amount of contained chemical composition.
The content of the invention
The present invention proposes that a kind of Radix Rhapontici seu Radix Echinopsis spends the method for building up of finger-print, comprises the following steps:
1) preparation of need testing solution:Medicinal powder is taken, in putting 100mL conical flask with cover, plus 70% methyl alcohol, ultrasound is carried
Take, after being placed into room temperature, then weighed weight, the weight of less loss is supplied with solvent, filter, take filtrate and filtered with 0.45 μm of miillpore filter
Cross, it is standby;
2) will need testing solution inject high performance liquid chromatograph in, obtain finger-print, the chromatographic condition for using for:Chromatogram
Post:Octadecylsilane chemically bonded silica chromatographic column;Mobile phase:The phosphate aqueous solution (B) of acetonitrile (A) -0.2%, using gradient elution
85%B (0min)~78%B (12min)~74%B (13min)~60%B (60min);Testing conditions:DAD detectors, detection
230~400nm of wavelength;Column temperature:20~40 DEG C;Sample size:5~30 μ L.
Preferably, it is 250mm × 4.6mm, 5 μm of YMC-Pack ODS-A chromatographic columns or island that chromatographic column uses specification
Tianjin Inertsil ODS-SP HPLC chromatogram posts.
It is further to be preferably, step 1) in, medicinal powder about 0.2g, accurately weighed, 70% methyl alcohol 25mL of addition are taken, surpass
Sound extracts 40min, after being placed into room temperature, then weighed weight, the weight of less loss is supplied with solvent, filter, filtrate is taken with 0.45 μm
Miillpore filter is filtered.
It is highly preferred that flow velocity is 1.2ml/min;Using DAD detectors, Detection wavelength 254nm;25 DEG C of column temperature;Sample size
10μL。
The present invention also provides a kind of method that utilization finger-print evaluates orobanche pycnostachya Hance quality of medicinal material, comprises the following steps:
Step one:Standard finger-print is set up, including:A) preparation of need testing solution:11 Radix Rhapontici seu Radix Echinopsis flowers of different batches are prepared respectively
Sample need testing solution, takes sample powder, in putting 100mL conical flask with cover, plus 70% methyl alcohol, ultrasonic extraction, it is placed into room temperature
Afterwards, then weighed weight, the weight of less loss is supplied with solvent, is filtered, taken filtrate and filtered with 0.45 μm of miillpore filter, it is standby;B) it is right
According to the preparation of product solution:Weigh 1) ecdysterone, 2) Quercetin -3-O- alpha-L-rhamnosides, 3) apigenin-7-O-beta-D-grape
Glycuronide, 4) Kaempferol -3-O- alpha-L-rhamnosides, 5) Ni Hu lignanoids B glycosides, 6) cyanidenon, 7) apiolin, 8) 5,7,
4 '-trihydroxy -3 '-methoxy flavone totally 8 kinds of reference substances, constant volume is dissolved with methyl alcohol, certain density single contrast solution is made,
0.45 μm of filtration of miillpore filter, it is standby;C) successively each need testing solution and reference substance solution are injected in high performance liquid chromatograph,
Finger-print is obtained respectively, and chromatographic condition is:Chromatographic column:Octadecylsilane chemically bonded silica chromatographic column;Mobile phase:Acetonitrile (A)-
0.2% phosphate aqueous solution (B), using gradient elution 85%B (0min)~78%B (12min)~74%B (13min)~60%B
(60min);Testing conditions:DAD detectors, 230~400nm of Detection wavelength;Column temperature:20~40 DEG C;Sample size:5~30 μ L;d)
11 similarities of sample are calculated with similarity evaluation software, therefrom determines a similarity highest as standard fingerprint figure
Spectrum.Step 2:A finger-print for sample to be evaluated is obtained with above-mentioned identical mode;Step 3:Commented with foregoing similarity
The similarity of sample finger-print to be evaluated and the standard finger-print described in valency software evaluation, similarity is sentenced more than 0.9
The fixed sample quality to be evaluated meets the requirements.
Further, the standard finger-print includes following 13 total peaks, and the relative retention time at each peak is respectively:
5.40,11.24,16.47,17.46,18.53,18.91,20.92,22.62,23.01,25.43,27.66,33.59,35.22.
Further, wherein, the relative peak area at 13 total peaks is respectively 0.164,1.280,0.378,
0.115,0.061,0.617,0.056,0.251,0.446,0.491,0.268,0.038.
Further, with the peak area at the 8 reference substances correspondence peak identified in the total peak, with testing sample pair
The peak area answered is compared, and the latter's peak area is bigger, illustrates that sample quality is better.
Need testing solution preparation method working solution of the invention, with precision higher, stability and reproduction
Property, system suitability by force, is applicable to the making of the category medicinal material.The Radix Rhapontici seu Radix Echinopsis flower fingerprint analysis method sensitivity set up
Height, favorable reproducibility;The standard finger-print for being obtained has typicalness, representativeness, can more comprehensively reflect in Radix Rhapontici seu Radix Echinopsis flower pesticide material
Contained chemical composition species and quantity, and then the overall evaluation to medicinal material and description provide a more comprehensively foundation.This
The Radix Rhapontici seu Radix Echinopsis flower pesticide material high-efficiency liquid-phase fingerprint technology set up is invented, compensate for still belonging to now the Radix Rhapontici seu Radix Echinopsis flower quality of medicinal material control of blank
The method of system, makes the Quality Control Technology more science of Radix Rhapontici seu Radix Echinopsis flower pesticide material comprehensive.
Brief description of the drawings
Fig. 1 is the standard finger-print that the method according to the invention is obtained;
What Fig. 2 and Fig. 3 showed 8 single reference substances and standard finger-print compares collection of illustrative plates;
Fig. 4 is 11 careless mistake reed catkins HPLC-FPS stacking charts.
Specific embodiment
The preparation of need testing solution
In the link, it is broken to take dry Radix Rhapontici seu Radix Echinopsis pollen, takes medicinal powder, and precision adds the methanol solution of amount of calculation, ultrasound
Treatment, places to room temperature, and solvent supplies weightlessness, shakes up, and filtration takes subsequent filtrate, crosses 0.45 μm of miillpore filter, molten as test sample
Liquid.
In the present invention, using methanol aqueous solution as test sample solvent, the concentration range of methanol solution can 50~
Between 100%, preferably between 60~80%, most preferably 70% methanol solution.
It is preferred that Radix Rhapontici seu Radix Echinopsis is crushed, 65 mesh sieves are crossed when using, extracting method can be backflow or ultrasonically treated, preferably pass through
Ultrasonic extraction, extraction time can be 30~60min, preferably extract 40min.
In the present invention, the amount of sampling can in the scope of 0.1~0.4g, in the case of using above-mentioned most preferably mode,
It is preferred that 0.2g is sampled, plus 70% methyl alcohol 25ml, weighed weight, ultrasonically treated 40min, after being placed into room temperature, then weighed weight, use
Solvent supplies the weight of less loss, filtration, takes subsequent filtrate and is filtered with 0.45 μm of miillpore filter, obtains need testing solution.
Therefore, the preparation method of the present invention most preferably Radix Rhapontici seu Radix Echinopsis flower need testing solution is:Medicinal powder about 0.2g is taken, it is accurate
It is weighed, to put in 100mL conical flask with cover, precision adds 70% methyl alcohol 25mL, ultrasonic extraction 40min, after being placed into room temperature, then claims
Determine weight, the weight of less loss is supplied with solvent, filter, take filtrate and filtered with 0.45 μm of miillpore filter, obtain final product.Using this most preferably
Preparation method, put up the best performance in terms of the peak number, peak height, peak area and separating degree in chromatogram.
The preparation of reference substance solution
Precision weighs each reference substance about 0.5mg, and in putting 5mL volumetric flasks respectively, plus methyl alcohol dissolves and is diluted to scale, shakes
It is even, reference substance solution is made, filtered with 0.45 μm of miillpore filter before sample introduction.Reference substance is obtained in being Radix Rhapontici seu Radix Echinopsis flower chemical constitution study
To and through spectrum resolution identification structure.Following 8 kinds:
1) ecdysterone
2) Quercetin -3-O- alpha-L-rhamnosides
3) apigenin-7-O-β-D-glucuronide
4) Kaempferol -3-O- alpha-L-rhamnosides
5) Ni Hu lignanoids B glycosides
6) cyanidenon
7) apiolin
8) 5,7,4 '-trihydroxy -3 '-methoxy flavone
Chromatographic condition
The chromatographic condition used in the present invention is preferably:Chromatographic column is octadecylsilane chemically bonded silica chromatographic column;Flowing
It is mutually the phosphate aqueous solution (B) of acetonitrile (A) -0.2%, using gradient elution 85%B (0min)~78%B (12min)~74%B
(13min)~60%B (60min);Using DAD detectors, 230~400nm of Detection wavelength;20~40 DEG C of column temperature;Sample size 5~
30μL。
In highly preferred embodiment of the present invention, the optimal chromatographic condition for determining Radix Rhapontici seu Radix Echinopsis flower HPLC fingerprint map analyzings is:Color
Spectrum post:YMC-Pack ODS-A chromatographic columns (250mm × 4.6mm, 5 μm) or Shimadzu Inertsil ODS-SP HPLC chromatograms
Post;Mobile phase:The phosphate aqueous solution of acetonitrile -0.2%, gradient elution:85%B (0min)~78%B (12min)~74%B
(13min)~60%B (60min);Flow velocity:1.2mL/min;Detection wavelength 254nm;25 DEG C of column temperature;The μ L of sample size 20.Using this
Optimal flow phase system and wash-out ratio, comprehensively, peak shape is good, and baseline is steady for peak information in chromatogram.Using the detection ripple of 254nm
Length can obtain peak number in optimal each chromatogram, peak height, peak area and separating degree.Chromatogram when flow velocity is 1.2mL/min
Separating degree is preferable, and elution time is shorter in the case where separating degree and peak number is not influenceed.
The demarcation at total peak
11 careless mistake reed catkins medicinal material samples of different sources collection are taken, sample introduction is distinguished according to the above-mentioned operating method having built up
Analysis, obtains the HPLC finger-prints of each batch medicinal material.In 11 sample finger-prints, it may be determined that 13 total peaks, formed
Common pattern.Wherein No. 2 peaks (S) are that its relative retention time and relative peak area are 1.00, and other peaks are in contrast with reference to peak
Relative retention time and relative peak area are relatively calculated, 1 is shown in Table:
Peak relative retention time and peak area are had in the Radix Rhapontici seu Radix Echinopsis of table 1 flower standard finger-print
The foundation of standard finger-print
11 parts of sample finger-prints of above-mentioned acquisition are imported in similarity evaluation software, similarity is calculated with average method.
Selected from result of calculation similarity it is maximum finger-print --- S7 medicinal materials fingerprints are used as standard finger-print
(Fig. 1).Reference substance points out comparing such as Fig. 2 and Fig. 3 of collection of illustrative plates (being obtained by foregoing reference substance) and S7 medicinal material collection of illustrative plates, wherein Fig. 1
In identify 2,4,6,12, No. 13 peaks, 3,7, No. 10 peaks are identified in Fig. 2.
Using foregoing most preferred parameters and chromatographic condition, 13 total peaks that the standard finger-print is included, its
Retention time and relative peak area are respectively:5.40,0.164;11.24,1.0000;16.47,1.280;17.46,0.3782;
18.53,0.115;18.91,0.061;20.92,0.617;22.62,0.056;23.01,0.251;25.43,0.446;
27.66,0.491;33.59,0.268;35.22,0.038.The reference substance solution sample introduction that will be prepared simultaneously, can point out 13 altogether
There are 8 in peak, this 8 peaks are corresponding with peak number in standard finger-print as follows:
No. 2:Ecdysterone
No. 3:Quercetin -3-O- alpha-L-rhamnosides
No. 4:Apigenin-7-O-β-D-glucuronide
No. 6:Kaempferol -3-O- alpha-L-rhamnosides
No. 7:Ni Hu lignanoids B glycosides
No. 10:Cyanidenon
No. 12:Apiolin
No. 13:5,7,4 '-trihydroxy -3 '-methoxy flavone
The 11 careless mistake reed catkins information in following source in this invention
The careless mistake reed catkins medicinal material of table 2.11
Radix Rhapontici seu Radix Echinopsis spends evaluation of medical materials' quality
According to the present invention it is possible to the finger-print of sample to be evaluated is obtained using the condition that above-mentioned finger-print is set up, so
It is compared with aforesaid standards finger-print afterwards, is evaluated using similarity evaluation software, investigate its similitude, it is similar
Degree judges samples met requirement more than 0.90.The evaluation software used in exemplary embodiments of the invention is NF committee member
The similarity evaluation (2004A editions) that can recommend.Can also further by standard finger-print
The peak area at the corresponding peak of 8 reference substances, peak area corresponding with testing sample is compared, and the latter's peak area is bigger,
Illustrate that sample quality is better.In another preferred embodiment, can further compare this 8 similarity at peak, similarity
Higher, then drug quality is better.
Method validation
The investigation of precision
Preparation method according to need testing solution prepares a sample, and sample introduction is repeated 6 times with the optimal chromatographic condition for determining,
The relative retention time at each total peak and the RSD values of relative peak area are measured respectively 0.06~0.14% and 0.15~3.00%
Between, show that instrument precision is good, meet the technical requirements of finger-print.It is shown in Table 3,4.
The Radix Rhapontici seu Radix Echinopsis of table 3 spends medicinal materials fingerprint Precision Experiment (relative retention time)
The Radix Rhapontici seu Radix Echinopsis of table 4 spends medicinal materials fingerprint Precision Experiment (relative peak area)
Study on the stability
Preparation method according to the need testing solution for determining prepares S7 samples, is existed respectively with the optimal chromatographic condition for determining
0th, 2,4,8,12, the analysis of 24h sample introductions, measure the relative retention time at each total peak and the RSD values of relative peak area 0.05~
Between 0.18% and 0.49~2.93%, show that need testing solution is good in 24 hours internal stabilities.It is shown in Table 5,6.
The Radix Rhapontici seu Radix Echinopsis of table 5 spends medicinal materials fingerprint stability experiment (relative retention time)
The Radix Rhapontici seu Radix Echinopsis of table 6 spends medicinal materials fingerprint stability experiment (relative peak area)
Replica test
According to parallel 5 parts of the preparation S7 samples of preparation method of the need testing solution for determining, with the optimal color of foregoing determination
Spectral condition difference sample introduction analysis, measure the relative retention time at each total peak and the RSD values of relative peak area 0.08~
Between 0.20% and 0.89~2.90%, show that the method repeatability is good.It is shown in Table 7,8.
The Radix Rhapontici seu Radix Echinopsis of table 7 spends medicinal materials fingerprint repeated experiment (relative retention time)
The Radix Rhapontici seu Radix Echinopsis of table 8 flower medicinal materials fingerprint repeatability experiment (relative peak area)
11 careless mistake reed catkins sample similarity evaluations
A sample is respectively taken in foregoing 11 careless mistake reed catkins medicinal material, the HPLC for obtaining each batch of medicinal material with method same as before refers to
Line collection of illustrative plates, utilizes " similarity evaluation (2004A editions) " to 13 total peaks in each chromatogram
It is analyzed and evaluated, similarity is calculated with average method, draws 11 batches of similar degrees of data (table 9) of medicinal material.Each batch sample
HPLC finger-print stacking charts see Fig. 4.
The similar degrees of data of 9 11 batches of medicinal materials of table
Claims (6)
1. a kind of utilization finger-print evaluates the method that Radix Rhapontici seu Radix Echinopsis spends quality of medicinal material, comprises the following steps:
Standard finger-print is set up, including:A) preparation of need testing solution:11 Radix Rhapontici seu Radix Echinopsis style product of different batches are prepared respectively
Need testing solution, takes sample powder, in putting 100mL conical flask with cover, plus 70% methyl alcohol, ultrasonic extraction, after being placed into room temperature, then
Weighed weight, the weight of less loss is supplied with solvent, filtration, is taken filtrate and is filtered with 0.45 μm of miillpore filter, standby;B) reference substance is molten
The preparation of liquid:Weigh 1) ecdysterone, 2) Quercetin -3-O- alpha-L-rhamnosides, 3) apigenin-7-O-beta-D-glucuronic acid
Glycosides, 4) Kaempferol -3-O- alpha-L-rhamnosides, 5) Ni Hu lignanoids B glycosides, 6) cyanidenon, 7) apiolin, 8) 5,7,4 '-three
Hydroxyl -3 '-methoxy flavone totally 8 kinds of reference substances, constant volume is dissolved with methyl alcohol, it is made certain density single contrast solution, micropore
0.45 μm of filtration of filter membrane, it is standby;C) by each need testing solution and reference substance solution injection high performance liquid chromatograph, obtain respectively
Finger-print, chromatographic condition is:Chromatographic column:Octadecylsilane chemically bonded silica chromatographic column;Mobile phase:Acetonitrile A-0.2% phosphoric acid
Aqueous solution B, using gradient elution:0min~12min~13min~60min, 85%B~78%B~74%B~60%B;Inspection
Survey condition:DAD detectors, 230~400nm of Detection wavelength;Column temperature:20~40 DEG C;Sample size:5~30 μ L;D) commented with similarity
Valency software calculates 11 similarities of sample, therefrom determines a similarity highest as standard finger-print;
A finger-print for sample to be evaluated is obtained with above-mentioned identical mode;
With the similarity of sample finger-print to be evaluated and the standard finger-print described in foregoing similarity evaluation software evaluation,
Similarity judges that the sample quality to be evaluated meets the requirements more than 0.9.
2. the method for claim 1, wherein chromatographic column using Shimadzu Inertsil ODS-SP HPLC chromatograms posts or
Specification is 250mm × 4.6mm, 5 μm of YMC-Pack ODS-A chromatographic columns.
3. the method for claim 1, wherein in step a), medicinal powder about 0.2g, accurately weighed, addition 70% are taken
Methyl alcohol 25mL, ultrasonic extraction 40min, after being placed into room temperature, then weighed weight, the weight of less loss is supplied with solvent, filter, take filter
Liquid is filtered with 0.45 μm of miillpore filter.
4. method as claimed in claim 3, wherein, flow velocity is 1.2mL/min;Detection wavelength 254nm;25 DEG C of column temperature;Sample introduction
Measure 10 μ L.
5. method as claimed in claim 4, wherein, the standard finger-print includes following 13 total peaks, the guarantor at each peak
The time is stayed to be respectively:5.40,11.24,16.47,17.46,18.53,18.91,20.92,22.62,23.01,25.43,
27.66,33.59,35.22.
6. method as claimed in claim 5, wherein, the relative peak area at 13 total peaks is respectively 0.164,1.000,
1.280,0.378,0.115,0.061,0.617,0.056,0.251,0.446,0.491,0.268,0.038.
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CN115389652B (en) * | 2022-07-28 | 2023-11-03 | 江阴天江药业有限公司 | Method for establishing fingerprinting of rhizoma phragmitis medicinal material |
CN115798573B (en) * | 2023-02-02 | 2023-05-09 | 武汉宏韧生物医药股份有限公司 | Method and device for analyzing pharmaceutical ingredients |
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