CN107014930A - The assay method of canopy scattered seed finger-print - Google Patents
The assay method of canopy scattered seed finger-print Download PDFInfo
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- CN107014930A CN107014930A CN201710391962.8A CN201710391962A CN107014930A CN 107014930 A CN107014930 A CN 107014930A CN 201710391962 A CN201710391962 A CN 201710391962A CN 107014930 A CN107014930 A CN 107014930A
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Abstract
It is specifically first to take canopy scattered seed the present invention relates to a kind of assay method of canopy scattered seed finger-print, it is finely ground, plus methanol solution, ultrasonic dissolution, cooling, then add methanol solution to supply weightlessness, shake up, filter, collect filtrate and obtain canopy powder particulate samples；Then in the chromatographic column using octadecylsilane chemically bonded silica as filler, column temperature is 27 DEG C, flow velocity is 0.8~1.2ml/min, Detection wavelength is 278nm, mobile phase is elution under the conditions of the formic acid water that acetonitrile and formic acid mass fraction are 0.01%, and canopy scattered seed finger-print is established using this method, and the quality control and the true and false for canopy scattered seed, which differentiate, provides a kind of new method, and the collection of illustrative plates can comprehensively react the material information of Chinese medicine, the visualization for enhancing fingerprint peakses is compared.
Description
Technical field
The invention belongs to Chinese medicine preparation detection field, it is related to the assay method of canopy scattered seed finger-print.
Background technology
Traditional Chinese medicine ingredients are complicated, and active component is often not single component, quality control index is used as using certain single component
The requirement of traditional Chinese medicine quality control has increasingly been not suitable with.Therefore, traditional Chinese medicine fingerprint technology is arisen at the historic moment.
Traditional Chinese medicine fingerprint technology comes from fingerprint identification, more comprehensive using modern information technologies and quality analysis means
Reflect the type and quantity of chemical composition contained by Chinese medicine.For Chinese medicine, finger-print can be for discerning the false from the genuine, judge excellent
It is bad；For Chinese patent drug, finger-print can differentiate authenticity of products, judge the reasonability of preparation technology, efficiently control product matter
Amount.Most of middle the effective elements of the medicine is still not clear at this stage, and the globality and ambiguity of traditional Chinese medicine fingerprint just adapt to this
One feature, compared with single component method of quality control with more scientific and comprehensive.Have recognized that in the world at present and refer to Chinese medicine
Line collection of illustrative plates as traditional Chinese medicine quality control model.High performance liquid chromatography has the advantages that separation efficiency height, analyze speed are fast,
Main Analysis means as current finger-print.
Canopy powder comes from the old Shi Wen of Song《The formulary of peaceful benevolent dispensary》, by Chinese ephedra, roasted perilla fruit, fry semen armeniacae amarae, dried orange peel,
Totally 7 herbal medicines are constituted for honey-made mulberry bark, poria cocos, honey-fried licorice root.Using Chinese ephedra as monarch in side, relieving the exterior syndrome with drugs pungent in flavor and warm in property, freeing lung and relieving asthma with cold-dispelling.
Minister is with perilla seed, pungent fragrant lowering the adverse-rising QI to resolve phlegm, the arduous temperature of semen armeniacae amarae, expectorant cough suppressant and anti-asthmatic, two medicine co-fallings profit lung qi, expelling phlegm and arresting coughing.Assistant
Medicine dried orange peel pungent-warm, eliminating dampness and eliminating phlegm, regulating qi-flowing for activating stagnancy；Root bark of white mulberry fishy smell is sweet cold, and purging the lung of pathogenic fire profit level is breathed heavily；Poria cocos invigorating the spleen excreting dampness, prevents life
The source of phlegm；Three medicines combination clearing damp dissolving phlegm altogether.Radix glycyrrhizae is makes, coordinating the drug actions of a prescription.All medicine compatibilities, inducing diaphoresis is used in combination with resolving sputum, and phlegm wet must disappear,
Exterior cold must dissipate, all card self-healing.Full side cures mainly lung sense cold-evil, cough with dyspnea, chest diaphragm dysphoria, spasm of nape and back, low voice speaking nasal obstruction, dizzy mesh
Dizzy, mental disorder is unfavorable, it is sound to sip, and is widely used in clinical flu, cough, the lung pattern diseases such as disease, dyspnea of roaring.Taiji Group Chongqing Fu
Mound pharmacy Co., Ltd., Factory have developed first canopy powder granular preparation of China.It has been listed in national great new drug initiative science and technology weight
It is big special.But, the domestic research also without document report to canopy scattered seed finger-print at present.Dong from it is bright et al.《In
Herbal medicine magazine》(2016,47 (3):The fingerprint atlas detection method of canopy powder traditional decoction is reported in 425-429), and is passed through
Lot of experiments, the quality control of the not suitable canopy powder finished granule of this method, it is impossible to system, comprehensively reflect canopy powder
The inherent quality of particle.To ensure patient medication safely and effectively, a kind of detection side of control canopy scattered seed total quality is invented
Method is extremely urgent.Based on this, the present invention establishes a kind of new fingerprint atlas detection method for being adapted to canopy scattered seed.
The content of the invention
In view of this, it is an object of the invention to provide a kind of method for building up of canopy scattered seed finger-print, by this
Method obtains the standard finger-print of canopy scattered seed, quality control for canopy scattered seed and the true and false differentiate provides it is a kind of newly
Method, and the finger-print that this method is set up more can comprehensively react the material information of Chinese medicine, enhance fingerprint peakses
Visualization is compared.
To reach above-mentioned purpose, the present invention provides following technical scheme：
1st, the assay method of canopy scattered seed finger-print, comprises the following steps：
(1) preparation of canopy powder particulate samples is prepared：Canopy scattered seed is taken, it is finely ground, plus methanol solution, ultrasonic dissolution, cooling,
Again plus methanol solution supplies weightlessness, shake up, filter, collect filtrate and obtain canopy powder particulate samples；
(2) chromatogram is detected：Canopy powder particulate samples are made in step (1), using octadecylsilane chemically bonded silica as filler
Chromatographic column, column temperature is 27 DEG C, and flow velocity is 0.8~1.2ml/min, and Detection wavelength is 278nm, and mobile phase is acetonitrile and formic acid matter
Fraction is measured to elute under the conditions of 0.01% formic acid water.
In the present invention, the methanol solution is the methanol solution of volume fraction 50%, and the ultrasound is ultrasonic at least 30 points
Clock.
In the present invention, the methanol solution addition adds 50ml methanol solutions by every gram of canopy scattered seed.
In the present invention, step (1) is replaced by following steps：Canopy scattered seed is taken, it is finely ground, add ethanol solution shaking scattered
Afterwards, stand overnight, supernatant residue is collected in centrifugation respectively, precipitation washs colourless to residue to supernatant with ethanol solution, centrifuge,
Merge supernatant, volatilize solvent, residue methanol solution dissolves.
It is preferred that, the methanol solution is the methanol solution that volume fraction is 50%, and the ethanol solution is volume fraction
75% ethanol solution.
It is preferred that, the methanol that the methanol solution addition adds 50ml volume fractions to be 50% by every gram of canopy scattered seed is molten
Liquid.
It is furthermore preferred that described centrifuge to centrifuge 5min under the conditions of 5000r/min.
In the present invention, the elution is gradient elution, and actual conditions is：
0~25min, acetonitrile：Formic acid mass fraction is the volume ratio of 0.01% formic acid water by the ﹕ of 2% ﹕ 98% to 7%
93%；
25~38min, acetonitrile：Formic acid mass fraction is the volume ratio of 0.01% formic acid water by the ﹕ of 7% ﹕ 93% → 10%
90%；
38~60min, acetonitrile：Formic acid mass fraction is the volume ratio of 0.01% formic acid water by the ﹕ of 10% ﹕ 90% → 15%
85%；
60~120min, acetonitrile：Formic acid mass fraction is 0.01%.
The invention discloses the assay method of canopy scattered seed finger-print, have the following advantages that：
(a) foundation of first public canopy scattered seed finger-print of the invention, finger-print being capable of more single index components
The material information of Chinese medicine is more fully reacted in control, and the globality for enhancing fingerprint spectral peak compares；
(b) test sample is simple for production, and chromatographic condition is easily realized；
(c) method stability and reappearance are preferable；
(d) the Efficient Characterization quality of canopy scattered seed, is conducive to product quality monitoring；With method it is easy, stably, essence
Density is high, favorable reproducibility；It can differentiate that the true and false of product is good and bad exactly.
Brief description of the drawings
In order that the purpose of the present invention, technical scheme and beneficial effect are clearer, the present invention provides drawings described below and carried out
Explanation：
Fig. 1 is the result for carrying out HPLC finger-print detections to canopy scattered seed using different scanning mode；
Fig. 2 is the result for carrying out HPLC finger-print detections to canopy scattered seed using different chromatographic columns；
Fig. 3 is the result for carrying out HPLC finger-print detections to canopy scattered seed using different column temperatures；
Fig. 4 is the result for carrying out HPLC finger-print detections to canopy scattered seed using different mobile phases；
Fig. 5 is the standard finger-print that canopy scattered seed is detected using the method for the invention；
Fig. 6 is the chromatogram result of canopy scattered seed of the present invention and simple need testing solution；
Fig. 7 is the finger-print stacking chart of ten batches of canopy powder particulate samples, and it is commented by chromatographic fingerprints of Chinese materia medica similarity
The A editions generations of valency system.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.
Instrument of the embodiment of the present invention and reagent：
Instrument：Shimadzu 20A high performance liquid chromatographs (Japanese Shimadzu Corporation)；N-1001D-WA Rotary Evaporators (Japan
Eyela companies)；KQ2200E types ultrasonic cleaning machine (Kunshan Ultrasonic Instruments Co., Ltd.)；Sartorius-BS 124S electronics
Balance (Beijing Sai Duolisi balances Co., Ltd).The triple quadrupole rods tandem mass spectrometry instrument of the types of American AB Sciex company API 3000
(equipped with Turbo Ionspray ionization sources and the data handling systems of Analyst 1.4)；Agilent company of the U.S. Agilent
1100 quaternary gradient pumps and automatic sampler.
Reagent：Water is heartily pure water；Acetonitrile and methanol are chromatographically pure；Remaining reagent is pure to analyze.
Experimental example 1, chromatographic condition optimization
1. the investigation of scan mode
Canopy scattered seed finger-print under the conditions of different wave length is compared, selected：190~400nm all-wave lengths are swept
Retouch and (extract wavelength 278nm) and two kinds of scan modes of 278nm Single wavelength scannings are compared, the chromatogram result of acquisition is shown in Fig. 1
It is shown.
From the separating degree of spectral peak, preferably, each peak separating degree is good for 278nm Single wavelength scanning figures peak shape, and baseline is steady, good
In the wavelength 278nm figures extracted after 190~400nm full wavelength scanners, therefore select a length of canopy powder particle fingerprint image of 278nm unicasts
The scanning wavelength of spectrum.
2. the selection of chromatographic column
Under same chromatographic condition, selection：Thermo Syncronis C18(250 × 4.6mm, 5 μm) and
C18(250 × 4.6mm, 5 μm) two kinds of chromatographic columns of chromatographic column are compared, and the chromatogram result of acquisition is as shown in Figure 2.As a result show
Show, Thermo Syncronis C18The separating effect of (250 × 4.6mm, 5 μm) is preferable, detection peak is more, retention time is suitable, because
This selects Thermo Syncronis C18(250 × 4.6mm, 5 μm) chromatographic column.
3. the investigation of column temperature
Spectral peak behavior of the chromatographic column temperature at 27 DEG C, 30 DEG C, 35 DEG C and 40 DEG C is investigated, the chromatogram result of acquisition is shown in Fig. 3
It is shown.As seen from Figure 3, as the retention time of the rise chromatographic peak of column temperature shifts to an earlier date, the separation situation of chromatographic peak is deteriorated, canopy powder
Separating degree is optimal under the conditions of 27 DEG C, therefore the column temperature of selection is 27 DEG C.
4. the investigation of mobile phase
Under same chromatographic condition, to the phosphoric acid water of acetonitrile -0.01%, the phosphoric acid water of acetonitrile -0.1%, the formic acid of acetonitrile -0.01%
(volume ratio of mobile phase A ﹕ Mobile phase Bs is by the ﹕ 90% of 7% ﹕ 93% → 10% for water, acetonitrile-water and the phosphoric acid water of methanol -0.01%；From
38~60min, the volume ratio of mobile phase A ﹕ Mobile phase Bs is by the ﹕ 85% of 10% ﹕ 90% → 15%；From 60~120min, mobile phase A ﹕
The volume ratio of Mobile phase B is by the ﹕ 60% of 15% ﹕ 85% → 40%) five kinds of different mobile phases are investigated, the chromatogram knot of acquisition
Fruit is as shown in Figure 4.
The experimental result investigated from mobile phase, peak shape can be optimized by adding acid, but with the increase of acid concentration, color
The separating degree of spectral peak does not have substantial change, and higher acid concentration is unfavorable for the separation of alkaloid in canopy powder；Acetonitrile-
0.01% phosphoric acid water and the formic acid water chromatogram of acetonitrile -0.01% do not have obvious difference, for convenience mass spectral analysis selection acetonitrile -
0.01% formic acid water；The phosphoric acid water chromatographic peak of methanol -0.01% is wider, and if want to reach preferable separation, it may be necessary to it is longer
Analysis time；In summary, selection acetonitrile -0.01% formic acid water is mobile phase.
5th, optimization prepared by canopy powder particulate samples
(1) selection of need testing solution preparation method
Need testing solution is obtained using four kinds of preparation methods of the prior art, it is specific as follows：
A, canopy powder particle powder 0.25g is taken, it is accurately weighed, put in 25ml measuring bottles, plus the methanol of volume fraction 50% is molten
Liquid 20ml, ultrasonically treated 30min, take out, let cool, plus volume fraction 50% methanol solution to scale, shake up, filter, filtrate
0.45 μm of miillpore filter is crossed, is produced；
B, take canopy powder particulate samples appropriate, it is finely ground, weigh 0.50g, plus volume fraction 50% methanol solution 25ml, surpass
Sound 30min, lets cool, and supplies weightlessness, shakes up, filtering, produces；
C, take canopy powder particulate samples appropriate, it is finely ground, 0.50g, plus 75% ethanol 30ml are weighed, after shaking is scattered, is stood
Overnight, (5000r/min) 5min is centrifuged, washs that residue is colourless to supernatant (to be actually with the ethanol solution of volume fraction 75%
10ml wash twice from), centrifugation merges supernatant, and water-bath volatilizes solvent, residue with the methanol solution dissolving of volume fraction 50% simultaneously
25ml is settled to, is shaken up, filters, produces.
D, take canopy powder particulate samples appropriate, it is finely ground, weigh 0.50g, plus volume fraction 75% ethanol solution 30ml, shake
Shake after disperseing, stand overnight, centrifuge (5000r/min) 5min, residue is washed to supernatant with the ethanol solution of volume fraction 75%
Liquid is colourless (actual wash twice for 10ml from), centrifugation, merges supernatant, is concentrated under reduced pressure into and volatilizes solvent, residue volume fraction
50% methanol solution dissolves and is settled to 25ml, shakes up, filtering, produces.
The canopy scattered seed chromatic graph spectrum obtained by above-mentioned tetra- kinds of preparation methods of a-d is entered according to the condition after above-mentioned optimization respectively
Row detection.As a result show, the entirety of its finger-print is identical, each peak type of b, c, d is basically identical.But during using method a, test sample
Peak area is smaller, it is necessary to which larger sample size can be only achieved expected peak area；During using method c, d, preparation process is cumbersome, week
Phase is longer, in addition in method d, and methanol is as test sample solvent, and each chromatographic peak peak shape is poor.Consider, final choice method b
It is used as the preparation method of canopy scattered seed need testing solution.
(2) selection of sonication treatment time
Experiment is compared in need testing solution preparation, and the ultrasonically treated time is respectively 15min, 30min, 45min
Canopy scattered seed finger-print.As a result find, with the extension of ultrasonic time, each chromatographic peak peak area increased, but ultrasound
30min and 45min indifferences, preferably sonication treatment time are 30min.
Experimental example 2, the checking of canopy powder fingerprint spectrum method
1st, finger-print is detected
The finger-print detection of canopy scattered seed is carried out according to the testing conditions after optimizing in above-mentioned experiment, is specifically included：
Take canopy powder particulate samples appropriate, it is finely ground, 0.50g, plus 50% methanol 25ml, ultrasonic 30min are weighed, is let cool, is mended
Foot is weightless, shakes up, and filters, produces need testing solution.
According to high performance liquid chromatography, using octadecylsilane chemically bonded silica as filler, using acetonitrile as mobile phase A, with
0.01% formic acid water is Mobile phase B；Coutroi velocity is 0.8~1.2ml/min；27 DEG C of column temperature；Detection wavelength：278nm；According to such as
Lower program carries out gradient elution：From 0~25min, the volume ratio of mobile phase A ﹕ Mobile phase Bs is by the ﹕ 93% of 2% ﹕ 98% → 7%；From
25~38min, the volume ratio of mobile phase A ﹕ Mobile phase Bs is by the ﹕ 90% of 7% ﹕ 93% → 10%；From 38~60min, mobile phase A ﹕ stream
Dynamic phase B volume ratio is by the ﹕ 85% of 10% ﹕ 90% → 15%；From 60~120min, the volume ratios of mobile phase A ﹕ Mobile phase Bs by
The ﹕ 60% of 15% ﹕ 85% → 40%.
Need testing solution and the μ l-20 μ l of reference substance solution 10 are drawn, liquid chromatograph is injected, determined.
Detect that the standard finger-print of obtained canopy scattered seed is detailed as shown in Figure 5, the standard of the canopy scattered seed of gained
Finger-print includes 15 shared peaks, and the relative retention time at each peak number is respectively：(1)13.909、(2)15.798、(3)
46.185th, (4) 48.529, (5) 61.984, (6) 64.327, (7) 74.229, (8) 75.590 (liquiritin), (9) 80.881,
(10) 82.393, (11) 84.434 (aurantiamarin), (12) 85.568 (Rosmarinic acids), (13) 97.360, (14) 99.703, (15)
105.750。
2nd, precision test
Same need testing solution is taken, by the testing conditions continuous sample introduction 6 times after optimizing in above-mentioned experiment, chromatographic fingerprint is recorded
Collection of illustrative plates, investigates each shared peak and internal standard peak relative retention time and relative peak area, the results are shown in Table shown in 1 and 2.
1. precision tests of table-relative retention time
2 precision tests of table-relative peak area
As a result show, relative retention time RSD<0.2%, relative peak area RSD<10.0%, precision is good.
3rd, stability test
Same need testing solution is taken, empirically the testing conditions after middle optimization, respectively in 0h, 3h, 6h, 9h, 12h and 24h
Detected, record chromatographic fingerprinting, investigated each shared peak and internal standard peak relative retention time and relative peak area, as a result see
Table 3 and 4.
Table 3, stability test-relative retention time
Table 4, stability test-relative peak area
As a result show, relative retention time RSD<0.2%, relative peak area RSD<10.0%, have good stability.
4 replica tests
Same 6 parts of batch canopy scattered seed is taken, according to above-mentioned 6 parts of need testing solutions of test sample preparation method, according to above-mentioned
Detection method, continuous sample introduction 6 times records chromatographic fingerprinting, investigates each shared peak and internal standard peak relative retention time and relative
Peak area.It the results are shown in Table shown in 5 and 6.
Table 5, replica test-relative retention time
Table 6, replica test-relative peak area
As a result show, relative retention time RSD<0.2%, relative peak area RSD<12.0%, repeatability is good.
Experimental example 3, canopy scattered seed HPLC finger-print chromatographic peaks are pointed out
By investigating the retention time and ultraviolet spectra of different reference substances, it authenticated in canopy scattered seed HPLC finger-prints
No. 8 peaks (75.59min) are that liquiritin, No. 11 peaks (84.434min) are that aurantiamarin, No. 12 peaks (85.568min) are rosemary
Acid.The optical information provided by spectrogram is found, ultraviolet with corresponding known object of reference chromatographic peak in canopy powder particulate chromatography
Spectrum coincide, and as shown in Figure 6, the source analysis at canopy powder Fingerprints peak the results are shown in Table 7 to the chromatogram result of acquisition.
The source analysis result of table 7, canopy powder Fingerprints peak
The similarity evaluation of experimental example 4, canopy scattered seed HPLC finger-prints
Taking the batch products of canopy scattered seed 10, (lot number is：20160101、20160102、20160103、16050007、
16050008th, 16060009,16060010,16070011,16080012) by Taiji Group Chongqing Fuling Pharmaceutical Factory Co., Ltd.
There is provided.
The detection of finger-print is carried out according to the method provided in previous experiments example 2, the chromatogram result of acquisition is shown in Fig. 7 institutes
Show.Recommended using the Chinese Pharmacopoeia committee《Similarity evaluation 2004A editions》To HPLC collection of illustrative plates
Overall merit is carried out, similarity result is shown in Table 8.
Table 8, similarity result
As can be seen that 10 batches of canopy powder samples with reference to spectrum and according to median method with giving birth to from the similarity result of table 8
Into control spectrum between similarity be all higher than 0.9, show that different batches canopy powder sample similarity is preferable.Therefore, by canopy
The finger-print of scattered seed is included in its internal control quality standard, and its similitude is set to and cannot be less than 0.90.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical
Cross above preferred embodiment the present invention is described in detail, it is to be understood by those skilled in the art that can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (8)
1. the assay method of canopy scattered seed finger-print, it is characterised in that comprise the following steps：
(1) preparation of canopy powder particulate samples is prepared：Canopy scattered seed is taken, it is finely ground, plus methanol solution, ultrasonic dissolution, cooling, then add
Methanol solution supplies weightlessness, shakes up, filtering, collects filtrate and obtains canopy powder particulate samples；
(2) chromatogram is detected：Canopy powder particulate samples are made in step (1), using octadecylsilane chemically bonded silica as the color of filler
Post is composed, column temperature is 27 DEG C, flow velocity is 0.8~1.2ml/min, Detection wavelength is 278nm, and mobile phase is acetonitrile and formic acid quality point
Number is elution under the conditions of 0.01% formic acid water.
2. the assay method of canopy scattered seed finger-print according to claim 1, it is characterised in that：The methanol solution is
The methanol solution of volume fraction 50%, the ultrasound is ultrasonic at least 30 minutes.
3. the assay method of canopy scattered seed finger-print according to claim 1, it is characterised in that：The methanol solution adds
Enter amount by every gram of canopy scattered seed plus 50ml methanol solutions.
4. the assay method of canopy scattered seed finger-print according to claim 1, it is characterised in that step (1) is by following
Step is replaced：Canopy scattered seed is taken, it is finely ground, after addition ethanol solution shaking is scattered, stand overnight, supernatant is collected in centrifugation respectively
Residue, precipitation washs colourless to residue to supernatant with ethanol solution, centrifugation, merges supernatant, volatilizes solvent, residue methanol
Solution dissolves.
5. the assay method of canopy scattered seed finger-print according to claim 4, it is characterised in that：The methanol solution is
Volume fraction is 50% methanol solution, and the ethanol solution is the ethanol solution of volume fraction 75%.
6. the assay method of canopy scattered seed finger-print according to claim 4, it is characterised in that：The methanol solution adds
Enter amount by the methanol solution that every gram of canopy scattered seed plus 50ml volume fractions are 50%.
7. the assay method of canopy scattered seed finger-print according to claim 4, it is characterised in that the centrifugation is
5min is centrifuged under the conditions of 5000r/min.
8. the assay method of canopy scattered seed finger-print according to claim 1, it is characterised in that：The elution is gradient
Elute, actual conditions is：
0~25min, acetonitrile：Formic acid mass fraction is the volume ratio of 0.01% formic acid water by the ﹕ 93% of 2% ﹕ 98% to 7%；
25~38min, acetonitrile：Formic acid mass fraction is the volume ratio of 0.01% formic acid water by the ﹕ 90% of 7% ﹕ 93% → 10%；
38~60min, acetonitrile：Formic acid mass fraction is the volume ratio of 0.01% formic acid water by the ﹕ of 10% ﹕ 90% → 15%
85%；
60~120min, acetonitrile：Formic acid mass fraction is the volume ratio of 0.01% formic acid water by the ﹕ of 15% ﹕ 85% → 40%
60%.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101129543A (en) * | 2007-08-21 | 2008-02-27 | 王军 | Chinese ephedra Huagai powder |
-
2017
- 2017-05-27 CN CN201710391962.8A patent/CN107014930B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101129543A (en) * | 2007-08-21 | 2008-02-27 | 王军 | Chinese ephedra Huagai powder |
Non-Patent Citations (3)
| Title |
|---|
| 廖薇 等: "HPLC法测定华盖散不同煎剂中甘草酸和甘草苷的含量", 《贵阳中医学院学报》 * |
| 董自亮 等: "华盖散制剂-药材谱峰匹配指纹图谱研究", 《中草药》 * |
| 靳凤云 等: "HPLC测定华盖散传统汤剂与颗粒汤剂中盐酸麻黄碱、苦杏仁苷、甘草酸、甘草苷的含量", 《中成药》 * |
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