CN102662019B - Ziziphora clinopodioides Lam fingerprint and establishment method thereof - Google Patents
Ziziphora clinopodioides Lam fingerprint and establishment method thereof Download PDFInfo
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Abstract
The present invention provides a Ziziphora clinopodioides Lam fingerprint establishment method and a Ziziphora clinopodioides Lam fingerprint obtained thereby, including the following steps: (1) standard solution preparation: weighing standards, such as, diosmin, linarin and pulegone, dissolving the standards by using a methanol solution containing dimethyl sulfoxide and performing volume metering to obtain a standard solution; (2) test solution preparation: using the methanol solution containing dimethyl sulfoxide to immerse Ziziphora clinopodioides Lam powder, and performing ultrasonic extraction, filtration, volume metering and microfiltration membrane filtration to obtain a test solution; and (3) RRLC analysis: performing gradient elute with an XDB-C18 chromatographic column according to the following conditions to obtain a Ziziphora clinopodioides Lam HPLC fingerprint, wherein the column volume is 50 mm*4.6 mm*1.8 mm, flow rate is 0.9 ml/min, a detection wavelength is 270 nm, a column temperature is 30 DEG C, a sample volume is 6 ml and a mobile phase is an acetic acid solution-methanol. Based on existence and non-existence of the common peak in the fingerprint provided in the invention, the quality of Ziziphora clinopodioides Lam can be effectively monitored, stable, uniform and controllable quality being guaranteed.
Description
Technical field
The present invention relates to a kind of method for building up and finger-print of lip vanilla finger-print, belong to Pharmaceutical Analysis technical field.
Background technology
At present, finger-print has become the effective means of internationally recognized control Chinese medicine or natural drug quality, and fingerprint pattern technology has become the hot issue that current Chinese medicine circle is paid close attention to.Finger-print Quality Control technology is adopted to have Korea S, Japan, Germany etc. to the country that autonomic drug carries out quality control in the world, as Germany's quality of fingerprint pattern technology control ginkgo agent; U.S. FDA then requires the examination criteria that must control finger-print to the quality control of autonomic drug.Formulate injection quality standard with finger-print and be also included into pharmacopeia, but in China's existing standard, the quality standard of Chinese crude drug, Chinese patent drug is only limitted to appearance identification, proterties inspection in a large number, seldom wherein effective constituent is checked.Even if in the standard setting up composition measurement, survey composition major part and be only one or several index components, instead of directly relevant to curative effect effective constituent.In routine inspection, the discriminating of outward appearance, proterties and chemistry differentiate, in item, to there is a large amount of universality content, and the specificity of effective constituent is not strong, and being difficult to has one comprehensively to describe to the characteristic of medicinal material or preparation.Traditional Chinese medicine fingerprint can analyze biology, the physicochemical characteristics of Chinese medicine on the whole, have again certain can quantization parameter, fully demonstrated the feature of Chinese medicine globality and ambiguity.Therefore, obtain the good finger-print of reappearance through severe test and be used for traditional Chinese medicine quality control, Chinese medicine modernization and internationalization are significant.The authentication method being generally usually used in vegetable drug finger-print has Microscopic Identification, Characters Identification, physics and chemistry to identify.
The dry aerial parts that lip vanilla (Ziziphora clinopodioides Lam.) is Labiatae new calamint lip vanilla, Uygur's name is called Su Ze.This product is perennial suffruticose draft, and low hillside, meadow and arid slope are born in happiness, and being distributed in Xinjiang, USSR (Union of Soviet Socialist Republics), Mongolia and Central Asia also has distribution.Pungent in flavor and cool in property, micro-hardship, has effect of cardiac stimulant dampness removing, regulating qi-flowing for eliminating phlegm, diminishing inflammation and resolving masses, and lip vanilla is used in the compound of clinical treatment coronary heart diseases and angina pectoris, tracheitis, pulmonary abscess by Uygur medicine for a long time.Modem animal experimental result confirms, lip vanilla all has significant protective effect to the cardiac muscle of acute ischemia and the cardiac muscle cell of oxidative damage.The effective constituent of bibliographical information lip vanilla has volatile oil, organic acid, the Multiple components such as flavonoids, and only it is carried out to the standard control device of qualitative and quantitative analysis shortage comprehensive reflection lip vanilla quality.It is inadequate for depending merely on the stability measuring certain effective constituent examination quality, is difficult to reach the effective control to lip vanilla quality.
Summary of the invention
The technical problem to be solved in the present invention is the defect overcoming prior art, provide a kind of method for building up of lip vanilla finger-print, and the finger-print of lip vanilla that obtains of method thus, reach with this and improve its quality evaluation system, effectively control the object of lip vanilla quality of medicinal material.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
The method for building up of lip vanilla finger-print, comprises the following steps;
(1) preparation of standard solution:
Take standard items diosmin, linarin and pulegone respectively, with containing the dissolve with methanol solution constant volume that dimethyl sulfoxide (DMSO) is 20%-30%v/v, the concentration of diosmin, linarin and pulegone is made to be respectively the solution of 0.0122-0.1708mg/ml, 0.0276-0.3804mg/ml, 0.0063-0.0879mg/ml, as standard solution;
(2) preparation of need testing solution:
Take lip vanilla powder, it is the methanol solution 8-15ml of 20%-30%v/v that every 1g adds containing dimethyl sulfoxide (DMSO), soaks 0.5-1.5h, ultrasonic extraction 0.5-1h, filters, with the methanol solution constant volume containing dimethyl sulfoxide (DMSO) being 20%-30%v/v, with filtering with microporous membrane, obtain need testing solution;
(3) high separation fast liquid chromatography (RRLC) method analysis:
Chromatographic condition: XDB-C18 chromatographic column, 50mm × 4.6mm, 1.8 μm, flow velocity 0.9ml/min, determined wavelength 270nm, column temperature 30 DEG C, sample size 6ml, mobile phase A is 1%v/v acetic acid aqueous solution, and Mobile phase B is methyl alcohol, adopt gradient elution: 0 – 4min, acetic acid aqueous solution is reduced to 58% by 77%; 4 – 10min, acetic acid aqueous solution is reduced to 50% by 58%;
Draw above-mentioned standard solution and need testing solution respectively, inject high separation fast liquid chromatography instrument and carry out the detection of high separation fast liquid chromatography, according to above-mentioned conditional operation, obtain the RRLC finger-print of lip vanilla.
Common characteristic peak in this finger-print is diosmin (12), linarin (15), pulegone (16) three peaks, and its retention time is respectively 29.617min, 40.522min and 46.897min.
Further, common characteristic peak in the RRLC finger-print of the lip vanilla obtained in the inventive method also comprises (1), (2), (3), (4), (5), (6), (7), (8), (9), (10), (11), (13), (14), (17), (18) ten five peaks, its retention time is respectively 1.405min, 2.015min, 2.472min, 3.132min, 3.571min, 5.972min, 7.548min, 12.637min, 15.548min, 21.309min, 22.846min, 34.362min, 36.636min, 55.02min and 56.42min.
According to the method described in the present invention, when preparation standard product solution, preferably:
Take standard items diosmin, linarin and pulegone respectively, with containing the dissolve with methanol solution constant volume that dimethyl sulfoxide (DMSO) is 25%v/v, the concentration of diosmin, linarin and pulegone is made to be respectively the solution of 0.0122-0.1708mg/ml, 0.0276-0.3804mg/ml, 0.0063-0.0879mg/ml, as standard solution.
According to the method described in the present invention, when preparing need testing solution, preferably:
Take lip vanilla powder, it is the methanol solution 10ml of 25%v/v that every 1g adds containing dimethyl sulfoxide (DMSO), soaks 1h, ultrasonic extraction 0.5h, filters, and with the methanol solution constant volume containing dimethyl sulfoxide (DMSO) being 25%v/v, with filtering with microporous membrane, obtains need testing solution.
In lip vanilla medicinal material in the present invention, principle active component diosmin and linarin are insoluble in general Extraction solvent, and this method adds the stripping that cosolvent dimethyl sulfoxide (DMSO) (DMSO) helps effective constituent first in Extraction solvent.
Quick high score has been used to be better than Microscopic Identification, Characters Identification, physics and chemistry qualification from liquid phase (RRLC) first, there is higher sensitivity, degree of separation and analysis speed, be a kind of comprehensively fast Analysis and Identification method detect for the qualification of lip vanilla medicinal material.
According to the present invention, by the presence or absence at peak total in finger-print, effectively can monitor the quality of lip vanilla, ensure the stable, homogeneous, controlled of its quality.
Lip vanilla medicinal material integrally being treated, nuance between different medicinal material can be found out by comparing its total peak.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for instructions, together with embodiments of the present invention for explaining the present invention, is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the chromatogram of standard items of the present invention;
Fig. 2 is the chromatogram of No. 2 sample need testing solutions in the embodiment of the present invention 1;
Fig. 3 utilizes chromatographic fingerprints of Chinese materia medica similarity evaluation software (2004A version) to process the lip vanilla common pattern characteristic fingerprint pattern of the present invention obtained;
Fig. 4 is the RRLC finger-print of the lip vanilla by the inventive method acquisition.
Wherein, 1-18 is the total peak in the RRLC finger-print of lip vanilla, and S1-S10 is the RRLC finger-print of the lip vanilla of Different sources.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
Embodiment 1
1. crude drug source:
10 Different sources lip vanilla sample sources and similarity
Lip vanilla is accredited as labiate lip vanilla (Ziziphora clinopodioides Lam.) through the college of traditional Chinese medicine of Xinjiang Medicine University department of Chinese materia medica Lee Yonghe County professor of pharmacy.
1. the preparation of standard solution
This method standard reference material is diosmin, linarin, pulegone
Take standard items respectively appropriate, be dissolved in methyl alcohol, what discovery pulegone can be good is dissolved in methyl alcohol, and diosmin and linarin solubleness in methyl alcohol is very little, dissolves hardly.It is helped to dissolve so add cosolvent DMSO.With containing 25%v/v DMSO methanol solution preparation standard product.The concentration of diosmin, linarin and pulegone is made to be respectively the solution of 0.122mg/ml, 0.276mg/ml, 0.063mg/ml, as standard solution.
2. the preparation of need testing solution
The lip vanilla meal 1.000g of accurately weighed Different sources loads in 30mL tool plug conical flask, with 10mL25%DMSO methyl alcohol for solvent, soak 1h, ultrasonic (frequency 40kHz) extracts 30min, filter, be settled in 10mL volumetric flask by 25%DMSO methanol wash, shake up, cross 0.22 μm of miillpore filter, to obtain final product.
3. chromatographic condition
Serial RRLC, the DAD detecting device of Agilent 1200, XDB-C18 post (50mm × 4.6mm, 1.8 μm), flow velocity 0.9mL/min, column temperature 30 DEG C, mobile phase is 1% acetic acid aqueous solution (A) and methyl alcohol (B) gradient elution, 0 – 4min, 77% – 58%A; 4 – 10min, 58% – 50%A, sample size 6ml.
4. methodological study
Precision test: get with a need testing solution (the board house ditch place of production), continuous sample introduction 5 times, record chromatogram (Fig. 2).With the chromatographic peak of diosmin for reference peak, the RSD calculating its each total chromatographic peak relative retention time and relative peak area, respectively at 0-0.947% and 0.11%-2.829%, shows that instrument precision is good.
Stability test: get with a need testing solution (the board house ditch place of production), record 0,4,8,12, the chromatogram of 24h.The relative retention time of each chromatographic peak and the RSD of relative peak area are respectively 0.076%-1.156% and 1.422%-2.95%.Show that sample is stable in 24h.
Replica test: get same sample (the board house ditch place of production) 5 parts, need testing solution is prepared according under " 2 " item, chromatogram is recorded under " 3 " item chromatographic condition, the RSD calculating its each total chromatographic peak relative retention time and relative peak area is respectively 0.216%-2.057% and 0.597%-2.928%, shows that method repeatability is good.
5. the foundation of the RRLC finger-print of lip vanilla medicinal material
Lip vanilla medicinal material RRLC finger-print general characteristic: 10 parts of Different sources lip vanilla samples are measured by above-mentioned chromatographic condition, use chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A version software, generate the reference fingerprint (figure tri-) of lip vanilla medicinal material common pattern, wherein total chromatographic peak 18.10 batches of lip vanilla medicinal material spectrum datas are imported, through Data Matching, generates reference fingerprint with median method.By with reference substance comparison retention time, can determine that No. 12, peak is the chromatographic peak of diosmin, No. 15, peak is the chromatographic peak of linarin, and No. 16, peak is the chromatographic peak of pulegone.Similarity Measure is carried out to the RRLC collection of illustrative plates of 10 batches of lip vanilla samples.Similarity Measure result shows, each sample with contrast the similarity of collection of illustrative plates between 0.914-0.994,10 place of production samples with contrast collection of illustrative plates similarity all more than 0.9.The method on the whole, macroscopically can characterize the quality of lip vanilla medicinal material, can be used for the true and false differentiating lip vanilla medicinal material.
Table one 10 batches of medicinal materials have peak retention time
Table two 10 batches of medicinal materials have peak relative retention time (with No. 12 peaks for contrast)
Table three 10 batches of medicinal materials have peak and retain peak area
Table four 10 batches of medicinal materials have peak and relatively retain peak area (with No. 12 peaks for contrast)
Embodiment 2
(1) preparation of standard solution:
Take standard items diosmin, linarin and pulegone respectively, with containing the dissolve with methanol solution constant volume that dimethyl sulfoxide (DMSO) is 20%v/v, the concentration of diosmin, linarin and pulegone is made to be respectively the solution of 0.122mg/ml, 0.276mg/ml, 0.063mg/ml, as standard solution.
(2) preparation of need testing solution:
The lip vanilla meal 1.000g of accurately weighed Different sources loads in 30mL tool plug conical flask, with 8mL20%DMSO methyl alcohol for solvent, soaks 0.5h, ultrasonic extraction 30min, filters, is settled in 10mL volumetric flask by 20%DMSO methanol wash, shake up, cross 0.22 μm of miillpore filter, to obtain final product.
All the other operations are with embodiment 1.
Embodiment 3
(1) preparation of standard solution:
Take standard items diosmin, linarin and pulegone respectively, with containing the dissolve with methanol solution constant volume that dimethyl sulfoxide (DMSO) is 30%v/v, the concentration of diosmin, linarin and pulegone is made to be respectively the solution of 0.122mg/ml, 0.276mg/ml, 0.063mg/ml, as standard solution.
(2) preparation of need testing solution:
The lip vanilla meal 1.000g of accurately weighed Different sources loads in 30mL tool plug conical flask, with 15mL30%DMSO methyl alcohol for solvent, soaks 1.5h, ultrasonic extraction 1h, filters, is settled in 10mL volumetric flask by 30%DMSO methanol wash, shake up, cross 0.22 μm of miillpore filter, to obtain final product.
All the other operations are with embodiment 1.
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. the method for building up of lip vanilla finger-print, is characterized in that, comprises the following steps:
(1) preparation of standard solution:
Take standard items diosmin, linarin and pulegone respectively, with being that percent by volume is the dissolve with methanol solution of 20%-30% containing dimethyl sulfoxide (DMSO) and constant volume makes standard solution;
(2) preparation of need testing solution:
Take lip vanilla powder, every 1g adds the methanol solution 8-15ml containing dimethyl sulfoxide (DMSO) to be percent by volume be 20%-30%, soak 0.5-1.5h, ultrasonic extraction 0.5-1h, filter, with the methanol solution constant volume of to be percent by volume be containing dimethyl sulfoxide (DMSO) 20%-30%, with filtering with microporous membrane, obtain need testing solution;
(3) high separation fast liquid chromatography method is analyzed:
Chromatographic condition: XDB-C18 chromatographic column, 50mm × 4.6mm, 1.8 μm, flow velocity 0.9 ml/min, determined wavelength 270nm, column temperature 30 DEG C, sample size 6 μ l, mobile phase A to be percent by volume be 1% acetic acid aqueous solution, Mobile phase B is methyl alcohol, adopt gradient elution: 0-4min, acetic acid aqueous solution percent by volume is reduced to 58% by 77%; 4-10min, acetic acid aqueous solution percent by volume is reduced to 50% by 58%;
Draw above-mentioned standard solution and need testing solution respectively, inject high separation fast liquid chromatography instrument and carry out the detection of high separation fast liquid chromatography, according to above-mentioned conditional operation, obtain the high separation fast performance liquid finger-print of lip vanilla.
2. the method for building up of lip vanilla finger-print according to claim 1, it is characterized in that: the common characteristic peak in the high separation fast performance liquid finger-print of the lip vanilla obtained is diosmin (12), linarin (15), pulegone (16) three peaks, and its retention time is respectively 29.617min, 40.522min and 46.897min.
3. the method for building up of lip vanilla finger-print according to claim 2, it is characterized in that: the common characteristic peak in the high separation fast performance liquid finger-print of the lip vanilla obtained also comprises (1), (2), (3), (4), (5), (6), (7), (8), (9), (10), (11), (13), (14), (17), (18) ten five peaks, its retention time is respectively 1.405 min, 2.015min, 2.472 min, 3.132 min, 3.571 min, 5.972 min, 7.548 min, 12.637 min, 15.548 min, 21.309 min, 22.846 min, 34.362 min, 36.636 min, 55.02 min and 56.42 min.
4. the method for building up of the lip vanilla finger-print according to any one of claim 1-3, is characterized in that, in described step (1) with containing dimethyl sulfoxide (DMSO) percent by volume be 25% dissolve with methanol solution and constant volume.
5. the method for building up of the lip vanilla finger-print according to any one of claim 1-3, is characterized in that, the preparation of described step (2) need testing solution:
Take lip vanilla powder, every 1g is the methanol solution 10ml of 25% as entered containing dimethyl sulfoxide (DMSO) percent by volume, soaks 1h, ultrasonic extraction 0.5h, filters, with the methanol solution constant volume containing dimethyl sulfoxide (DMSO) percent by volume being 25%, with filtering with microporous membrane, obtain need testing solution.
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| CN201110366670.1A CN102662019B (en) | 2011-09-06 | 2011-11-17 | Ziziphora clinopodioides Lam fingerprint and establishment method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1375309A (en) * | 2001-03-19 | 2002-10-23 | 艾静 | Hypertension treating medicine capable of protecting target organ and its production process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1375309A (en) * | 2001-03-19 | 2002-10-23 | 艾静 | Hypertension treating medicine capable of protecting target organ and its production process |
Non-Patent Citations (2)
| Title |
|---|
| Essential oil composition and biological activity of Ziziphora clinopodioides Lam. from Iran;Verdian-rizi Mohammadreza;《American-Eurasian Journal of Sustainable Agriculture》;20080630;第2卷(第1期);69-71 * |
| HPLC 测定新疆不同产地唇香草中齐墩果酸和熊果酸的含量;施洋 等;《中国实验方剂学杂志》;20101130;第16卷(第16期);33-35 * |
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