CN104569236A - Establishment method of Aquilaria sinensis leaf high performance liquid chromatography (HPLC) fingerprint spectrum - Google Patents
Establishment method of Aquilaria sinensis leaf high performance liquid chromatography (HPLC) fingerprint spectrum Download PDFInfo
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Abstract
The invention relates to the field of the quality control technology of traditional Chinese medicinal materials and in particular discloses an establishment method of an Aquilaria sinensis leaf high performance liquid chromatography (HPLC) fingerprint spectrum. The establishment method comprises the steps of preparing reference solution, preparing test article solution, determining the chromatographic conditions of the fingerprint spectrum, and determining a standard fingerprint spectrum; the establishment method is characterized in that the chromatographic conditions of the fingerprint spectrum are as follows: a C18 chromatographic column is adopted, acetonitrile-0.1-0.5% of phosphate buffer solution is used as mobile phase for gradient elution; an ultraviolet detector is used for detection and the detection wavelength is 300-360nm. The fingerprint spectrum has strong characteristic feature, main common peaks can achieve good baseline separation, a test article can be prepared simply and conveniently, the chromatographic conditions can be realized easily, and the method is simple and convenient, has good stability and good reproducibility and is suitable for the quality control of Aquilaria sinensis leaves.
Description
Technical field
The present invention relates to Chinese crude drug Quality Control Technology field, be specifically related to a kind of method for building up of whitewood spiceleaf HPLC finger-print.
Background technology
Utilizing chromatographic fingerprinting to obtain comprehensive chemical composition of Chinese materia medica characteristic information has been widely used among the quality control of Chinese medicine, and chromatographic fingerprints of Chinese materia medica is expression to the chemical feature of Chinese medicine globality and reflection.At present, FDA (Food and Drug Adminstration) (FDA), British Herbal Pharmacopoeia, German medicinal plant association, India herbal medicine allusion quotation, Canadian medicinal plant association all accept and record the method for quality control of finger-print, and current finger-print has become the most effective method of internationally recognized control Chinese patent drug, natural drug quality.The traditional Chinese medicine ingredients overwhelming majority can carry out analysis and detect on high performance liquid chromatograph, and therefore high performance liquid chromatography has become the prefered method of traditional Chinese medicine fingerprint technology.
Suspension culture of Aquilaria sinensis is practised and is claimed buta-buta, and main product is in India, Malaysian Deng Guo country in Southeast Asia.Abound with in China's Lingnan area, it is the time-honored rare traditional Chinese medicine of China, also be important " southern medicine " resource, rank one of " ten great Nan medicines ", its medicinal part source is Isolated From Thymelaeaceae Species suspension culture of Aquilaria sinensis [Aquilaria sinensis (Lour.) Gilg.] resiniferous heartwood part.Modern clinic is usually used in the treatment that digestive system, nervous system and cardiovascular system are main various diseases, has good effect.Each version " Chinese Pharmacopoeia " is all recorded suspension culture of Aquilaria sinensis, and from 2010 editions pharmacopeia, suspension culture of Aquilaria sinensis is defined as the unique legal plant origin of agalloch eaglewood medicinal material.
The exploitation of current suspension culture of Aquilaria sinensis resource are only limitted to the research of its medicinal part (resinous heartwood), and whitewood spiceleaf is as this plant rich in natural resources position the most, and its pharmacological research is but only in the starting stage.It is active that whitewood spiceleaf oral administration has significant anti-inflammatory and antalgic pharmacology.By setting up whitewood spiceleaf HPLC finger-print, can monitor each chemical composition of suspension culture of Aquilaria sinensis leaf n-butanol portion.
Summary of the invention
Technical matters to be solved by this invention is, in order to better control the quality of Chinese crude drug whitewood spiceleaf, provides a kind of method for building up of whitewood spiceleaf HPLC finger-print.
Above-mentioned technical matters to be solved by this invention is achieved by the following technical programs:
A method for building up for whitewood spiceleaf HPLC finger-print, comprises the preparation of reference substance solution, the preparation of need testing solution, the determination of the chromatographic condition of finger-print, the determination of standard finger-print, and the chromatographic condition of described finger-print is: adopt C
18chromatographic column; With acetonitrile-0.1 ~ 0.5% phosphate buffered saline(PBS) for mobile phase carries out gradient elution; Use UV-detector to detect, determined wavelength is 300 ~ 360nm;
Described condition of gradient elution is: during 0min, and the volume fraction of acetonitrile is 10%, and the volume fraction of phosphate buffered saline(PBS) is 90%; During 15min, the volume fraction of acetonitrile is 15%, and the volume fraction of phosphate buffered saline(PBS) is 85%; During 25min, the volume fraction of acetonitrile is 15%, and the volume fraction of phosphate buffered saline(PBS) is 85%; During 27min, the volume fraction of acetonitrile is 20%, and the volume fraction of phosphate buffered saline(PBS) is 80%; During 40min, the volume fraction of acetonitrile is 25%, and the volume fraction of phosphate buffered saline(PBS) is 75%; During 55min, the volume fraction of acetonitrile is 32%, and the volume fraction of phosphate buffered saline(PBS) is 68%.
In order to make each peak energy separate enough as much as possible, reach best separating effect, the present invention adjusts mobile phase ratio by great many of experiments is repeated multiple times, finally determines above-mentioned condition of gradient elution.
As a kind of preferred version, described C
18chromatographic column is kromasil-C
18chromatographic column.Specification is 4.6mm × 250mm, 5 μm.
The present invention has investigated many chromatographic columns respectively, wherein kromasil-C
18(4.6mm × 250mm, 5 μm) chromatographic column, Agilent-C
18(4.6mm × 250mm, 5 μm) chromatographic column, Thermo-C
18(4.6mm × 250mm, 5 μm) chromatographic column is better to separating effect, result display (see accompanying drawing 1), kromasil-C
18chromatographic column is best to target peak separating effect.
As a kind of preferred version, described phosphate buffered saline(PBS) mass concentration is 0.3% phosphate buffered saline(PBS).
Adopt the formic acid buffer salt of phosphate-buffered salt or high concentration obviously can improve the separation elute effect of each composition in whitewood spiceleaf.But because too high acidity easily makes buffer salt crystallization, cause the blocking of chromatographic column, thus affect experiment process and chromatographic column life-span, therefore the present invention is under the condition of multiple buffer salinity, investigate buffer salinity to the impact of each component separating effect, determine optimized buffer salt ratio.The results are shown in accompanying drawing 2.Result shows, and the phosphate-buffered salt of concentration more than 0.3% can improve separating effect, may affect the chromatographic column life-span, therefore this experimental selection 0.3% phosphate-buffered salt is as water system mobile phase owing to continuing to increase acidity.
As a kind of preferred version, described determined wavelength is 340nm.
The maximum absorption wavelength of each chromatographic peak is considered according to actual conditions, select out peak number more, and the comparatively balanced wavelength of response is as optimum determining wavelength, and mark the larger peak of 13 responses at that wavelength as characteristic peak, and reference substance peak is identified.The results are shown in accompanying drawing 3.Synthesise various factor, final 340nm wavelength of selecting is as mensuration wavelength.
As a kind of preferred version, column temperature is 25 DEG C, and flow velocity is 0.8ml/min, sample size 10 μ l.
Under different column temperature conditions, the separating effect of this elution program is verified respectively.The results are shown in accompanying drawing 4.Result shows, and 25 DEG C of column temperatures (room temperature condition) can reach good separating effect, therefore follow-up test is all selected to carry out at ambient temperature.
As a kind of preferred version, described reference substance solution is mangiferin reference substance solution, and its concentration is 0.2 ~ 0.4mg/ml.
As one most preferably scheme, described reference substance solution is mangiferin reference substance solution, and its concentration is 0.254mg/ml.
As a kind of preferred version, described need testing solution, its preparation method is: precision takes dry whitewood spiceleaf powder, be placed in conical flask, add methyl alcohol, ultrasonic extraction, filter, filtrate reduced in volume is extremely without alcohol taste, use the extracting n-butyl alcohol after ether and water saturation successively, merge butanol extraction liquid, concentrated constant volume, cross 0.45 μm of miillpore filter, for subsequent use.
As one most preferably scheme, described need testing solution, its preparation method is: precision takes dry whitewood spiceleaf powder 3g, be placed in 150ml conical flask, add methyl alcohol 50ml, ultrasonic 30min, suction filtration after cooling, filtrate reduced in volume is extremely without alcohol taste, successively with the normal butyl alcohol after ether and water saturation by volume 1:1 respectively extract 3 times, merge butanol extraction liquid, concentrated be settled to 25ml, cross 0.45 μm of miillpore filter, for subsequent use.
As a kind of preferred version, this finger-print determines 13 common characteristic peaks, with No. 3 peaks and mangiferin peak for reference to peak, calculate each common characteristic peak and the relative retention time with reference to peak, 1 to No. 13 peak relative retention times are: 0.705 ± 3%, 0.770 ± 3%, 1.000 ± 3%, 1.078 ± 3%, 1.095 ± 3%, 1.642 ± 3%, 1.688 ± 3%, 1.916 ± 3%, 2.116 ± 3%, 2.121 ± 3%, 2.224 ± 3%, 2.257 ± 3%, 2.292 ± 3%.
The present invention has following beneficial effect:
(1) the present invention filters out the chromatographic condition of suitable whitewood spiceleaf n-butanol portion finger-print, parameters is selected, finally determine optimum Parameter Conditions, adopt gradient elution method in 60min, obtain the characteristic spectrum of better separating effect, determine that 13 principal character peaks are as total peak, establish the fingerprint spectrum method of whitewood spiceleaf; (2) this Fingerprints is comparatively strong, and main total peak reaches good baseline separation; (3) preparation of test sample is easy, convenient and easy, and chromatographic condition easily realizes; (4) through methodological study, the whitewood spiceleaf fingerprint spectrum method of foundation meets the requirement of finger-print, and the stability of the method and reappearance are all relatively good; (5) the method is applicable to the quality control of whitewood spiceleaf.
Accompanying drawing explanation
Fig. 1 is for selecting kromasil-C
18chromatographic column, Agilent-C
18chromatographic column, Thermo-C
18hPLC collection of illustrative plates.
Fig. 2 is the HPLC collection of illustrative plates under 0.1%, 0.3%, 0.5% concentration buffer salt condition.
Fig. 3 be 210,257,286,317,332,340, HPLC collection of illustrative plates under 360nm condition.
Fig. 4 is the HPLC collection of illustrative plates under 25 DEG C, 28 DEG C, 30 DEG C column temperature conditions.
Fig. 5 is whitewood spiceleaf finger-print.
Embodiment
Explain the present invention further below in conjunction with specific embodiment, but embodiment does not limit in any form to the present invention.
Experiment material and the instrument of the present invention's use are as follows:
Medicinal material: same collecting season, 10 batches of whitewood spiceleafs (referring to table 2-1) of Different sources, the blade of Isolated From Thymelaeaceae Species suspension culture of Aquilaria sinensis [Aquilaria sinensis (Lour.) Gilg.] with spray is accredited as through Dongguan Institute of Traditional Chinese Medicine Engineering,Guangzhou Univers Lai little Ping researcher, pulverize after each batch of medicinal material dries 12h in 60 DEG C, cross No. 4 sieves, for subsequent use.
Table 1 whitewood spiceleaf crude drug source
Reagent: mangiferin standard items (made by oneself by this laboratory, detect through Shimadzu HPLC-DAD, normalization method calculates, purity >=98%);
Analyze methyl alcohol (Tianjin Fu Yu Fine Chemical Co., Ltd, lot number 120902);
Chromatogram acetonitrile (German merck company, lot number: 1.00003.4004);
Experimental apparatus: Shimadzu LC-20A (UV/Vis) high performance liquid chromatograph (Japanese Shimadzu Corporation, comprise: quaternary geopressure gradient pump, online vacuum degassing machine, DAD diode array detector, LCsolution Ver 1.X chromatographic work station);
Kromasil-C
18(4.6mm × 250mm, 5 μm) chromatographic column, Agilent-C
18(4.6mm × 250mm, 5 μm) chromatographic column, Thermo-C
18(4.6mm × 250mm, 5 μm) chromatographic column;
KQ5200DA type numerical control ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.);
BS224S sartorius 100,000/analytical balance (the prosperous safe high-tech instrument manufacturing company limited of Hebi City).
The method for building up of embodiment 1 whitewood spiceleaf finger-print
(1) reference substance solution preparation
Precision takes mangiferin reference substance 12.7mg and puts in 50ml volumetric flask, adds methyl alcohol ultrasonic dissolution and is diluted to scale, shaking up, and makes the mangiferin reference substance solution that concentration is 0.254mg/ml.Sealing compound sealing is placed in 4 DEG C of refrigerators, keeps in Dark Place.
(2) preparation of need testing solution
Precision takes dry whitewood spiceleaf powder and (picks up from agalloch eaglewood GAP base, Dongguan City, Guangdong Province, lot number: 201208) 3g, is placed in 150ml conical flask, adds methyl alcohol 50ml, ultrasonic 30min, suction filtration after cooling, filtrate reduced in volume to without alcohol taste, successively with the normal butyl alcohol after ether and water saturation by volume 1:1 respectively extract 3 times, merge butanol extraction liquid, concentrate and be settled to 25ml, cross 0.45 μm of miillpore filter, for subsequent use.
(3) foundation of chromatographic condition
Get need testing solution 1 part, adopt kromasil-C
18chromatographic column, with acetonitrile-0.3% phosphate buffered saline(PBS) for mobile phase carries out gradient elution, fixed flow rate is 0.8ml/min, sample size 10 μ l, and determined wavelength is that the condition of 340nm gradient elution is in table 2.
Table 2 gradient elution program
(4) methodological study
4.1 Precision Experiment
Get need testing solution 1 part, each sample introduction 10 μ l, continuous sample introduction 5 times, calculates the RSD value of each characteristic peak relative retention time and relative peak area, the results are shown in Table 3, table 4.
Table 3 Precision Experiment relative retention time (n=6)
Table 4 Precision Experiment relative peak area (n=6)
Table 3, table 4 result shows, and the RSD value of each total peak relative retention time and relative peak area is all less than 3%, illustrates that this system precision is good.
4.2 stability experiment
Get need testing solution 1 part, respectively at 0,3,6,9,12h sample introduction measures, each sample introduction 10 μ l, calculates the RSD value of each characteristic peak relative retention time and relative peak area, the results are shown in Table 5, table 6.
Table 5 stability experiment relative retention time (n=5)
Table 6 Precision Experiment relative peak area (n=5)
Table 5, table 6 result shows, and the RSD value of each total peak relative retention time and relative peak area is all less than 3%, illustrates that this need testing solution is good at 12h internal stability.
4.3 repeated experiment
Precision takes 6 parts same batch and (picks up from agalloch eaglewood GAP base, Dongguan City, Guangdong Province, lot number: each 3g of dry whitewood spiceleaf powder 201208), respectively by the operation of (2) item, prepare need testing solution, every part of test sample sample introduction 10 μ l, calculate the RSD value of each characteristic peak relative retention time and relative peak area, the results are shown in Table 7, table 8.
Table 7 repeated experiment relative retention time (n=6)
Table 8 repeated experiment relative peak area (n=6)
Table 7, table 8 result shows, and the RSD value of each total peak relative retention time and relative peak area is all less than 3%, illustrates that this method repeatability is good.
(5) determination of whitewood spiceleaf HPLC finger-print
5.1 sample tests
Precision takes the dry whitewood spiceleaf powder 3g of different batches in table 1, and operate by under (2) item respectively, prepare need testing solution, successively sample introduction, each sample sample size is 10 μ l, record chromatogram and every HPLC parameter.Calculate relative retention time and relative peak area value.The results are shown in Table 9,10.
Table 9 10 batches of whitewood spiceleafs have peak relative retention time
Table 10 10 batches of whitewood spiceleafs have peak relative peak area
The determination of 5.2 whitewood spiceleaf finger-prints
" the similarity evaluation 2004A version " that use Chinese Pharmacopoeia Commission to provide carries out analyzing and processing to each batch of whitewood spiceleaf HPLC finger-print, obtain the whitewood spiceleaf n-butanol portion finger-print that can reflect each sample HPLC chromatogram common feature, see accompanying drawing 5.
5.3 fingerprint similarity analyses
Bian carries out the analysis of similarity with " similarity evaluation 2004A version " to the characteristic fingerprint pattern of each batch of whitewood spiceleaf, with the contrast collection of illustrative plates generated for contrast, calculate the similarity result of each batch sample in table 11.
Table 11 different batches whitewood spiceleaf characteristic fingerprint pattern carries out similarity evaluation
The present invention is optimized exploration by a large amount of experiments to finger-print condition, finally establish whitewood spiceleaf HPLC characteristic fingerprint pattern, by carrying out characteristic mensuration to Different sources 10 batches of whitewood spiceleaf medicinal materials, mark 13 total peaks altogether, the relative retention time RSD value that each batch sample has peak is all less than 3%, similarity evaluation found that, each batch of medicinal material has peak similarity all more than 0.95, show under this chromatographic condition, between 10 batches of medicinal materials of Different sources, similarity is good, meets the technical manual of Chinese medicine characteristic finger-print completely.Therefore, the present invention, by setting up whitewood spiceleaf HPLC finger-print, can monitor each chemical composition of suspension culture of Aquilaria sinensis leaf, can control the quality of suspension culture of Aquilaria sinensis leaf.
Claims (10)
1. the method for building up of a whitewood spiceleaf HPLC finger-print, comprise the preparation of reference substance solution, the preparation of need testing solution, the determination of the chromatographic condition of finger-print, the determination of standard finger-print, it is characterized in that, the chromatographic condition of described finger-print is: adopt C
18chromatographic column; With acetonitrile-0.1 ~ 0.5% phosphate buffered saline(PBS) for mobile phase carries out gradient elution; Use UV-detector to detect, determined wavelength is 300 ~ 360nm;
Described condition of gradient elution is: during 0min, and the volume fraction of acetonitrile is 10%, and the volume fraction of phosphate buffered saline(PBS) is 90%; During 15min, the volume fraction of acetonitrile is 15%, and the volume fraction of phosphate buffered saline(PBS) is 85%; During 25min, the volume fraction of acetonitrile is 15%, and the volume fraction of phosphate buffered saline(PBS) is 85%; During 27min, the volume fraction of acetonitrile is 20%, and the volume fraction of phosphate buffered saline(PBS) is 80%; During 40min, the volume fraction of acetonitrile is 25%, and the volume fraction of phosphate buffered saline(PBS) is 75%; During 55min, the volume fraction of acetonitrile is 32%, and the volume fraction of phosphate buffered saline(PBS) is 68%.
2. method according to claim 1, is characterized in that, described C
18chromatographic column is kromasil-C
18chromatographic column, specification is 4.6mm × 250mm, 5 μm.
3. method according to claim 1, is characterized in that, described phosphate buffered saline(PBS) mass concentration is 0.3% phosphate buffered saline(PBS).
4. method according to claim 1, is characterized in that, described determined wavelength is 340nm.
5. method according to claim 1, is characterized in that, column temperature is 25 DEG C, and flow velocity is 0.8ml/min, sample size 10 μ l.
6. method according to claim 1, is characterized in that, described reference substance solution is mangiferin reference substance solution, and its concentration is 0.2 ~ 0.4mg/ml.
7. method according to claim 6, is characterized in that, described reference substance solution is mangiferin reference substance solution, and its concentration is 0.254mg/ml.
8. method according to claim 1, is characterized in that, described need testing solution, its preparation method is: precision takes dry whitewood spiceleaf powder, is placed in conical flask, adds methyl alcohol, ultrasonic extraction, filter, filtrate reduced in volume, to without alcohol taste, uses the extracting n-butyl alcohol after ether and water saturation successively, merge butanol extraction liquid, concentrated constant volume, crosses 0.45 μm of miillpore filter, for subsequent use.
9. method according to claim 8, is characterized in that, described need testing solution, its preparation method is: precision takes dry whitewood spiceleaf powder 3g, is placed in 150ml conical flask, adds methyl alcohol 50ml, ultrasonic 30min, suction filtration after cooling, filtrate reduced in volume to without alcohol taste, successively with the normal butyl alcohol after ether and water saturation by volume 1:1 respectively extract 3 times, merge butanol extraction liquid, concentrate and be settled to 25ml, cross 0.45 μm of miillpore filter, for subsequent use.
10. method according to claim 1, it is characterized in that, this finger-print determines 13 common characteristic peaks, with No. 3 peaks and mangiferin peak for reference to peak, calculate each common characteristic peak and the relative retention time with reference to peak, 1 to No. 13 peak relative retention times are: 0.705 ± 3%, 0.770 ± 3%, 1.000 ± 3%, 1.078 ± 3%, 1.095 ± 3%, 1.642 ± 3%, 1.688 ± 3%, 1.916 ± 3%, 2.116 ± 3%, 2.121 ± 3%, 2.224 ± 3%, 2.257 ± 3%, 2.292 ± 3%.
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| CN112986406A (en) * | 2019-12-13 | 2021-06-18 | 江西青峰药业有限公司 | Detection method of HPLC (high performance liquid chromatography) characteristic spectrum of turpinia formosana leaves |
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| WO2007083594A1 (en) * | 2006-01-18 | 2007-07-26 | Nagoya Industrial Science Research Institute | Laxative and food containing the same |
| CN102424678A (en) * | 2011-12-09 | 2012-04-25 | 林励 | High-purity mangiferin prepared from leaves and twigs of aquilaria sinensis and preparation method thereof |
| CN104211690A (en) * | 2014-08-27 | 2014-12-17 | 中山市格好生物科技发展有限公司 | Method for separating and purifying mangiferin from aquilaria sinensis leaves |
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| WO2007083594A1 (en) * | 2006-01-18 | 2007-07-26 | Nagoya Industrial Science Research Institute | Laxative and food containing the same |
| CN102424678A (en) * | 2011-12-09 | 2012-04-25 | 林励 | High-purity mangiferin prepared from leaves and twigs of aquilaria sinensis and preparation method thereof |
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| CN112986406A (en) * | 2019-12-13 | 2021-06-18 | 江西青峰药业有限公司 | Detection method of HPLC (high performance liquid chromatography) characteristic spectrum of turpinia formosana leaves |
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Application publication date: 20150429 |