CN1932507A - Method for establishing evodia rutaecarpa water-soluble fingerprint and standard fingerprint thereof - Google Patents
Method for establishing evodia rutaecarpa water-soluble fingerprint and standard fingerprint thereof Download PDFInfo
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Abstract
The invention provides the establishment method of the lipid-soluble fingerprint diagram for the evodia and its standard fingerprint diagram which includes: making of the trying aqua, making of the comparing aqua, detecting by the HPLC, using fingerprint diagram software to treat the data and diagram and then get the lipid-soluble fingerprint diagram of the evodia. Compared with the existing technique, the invention is simple, stability, the precision is so much high and re-appear is good; The method to withdraw the lipid-soluble composition is brief and the time is short; the peak of lipid-soluble fingerprint diagram is many and the peak form is good, so it is easy to discriminate; The standard fingerprint diagram built up can be availably token by the quality of the evodia. So it provides a new standard for appraising the evodia.
Description
Technical field: the present invention relates to the method for building up of the finger-print of Chinese crude drug, the method for building up of evodia rutaecarpa water-soluble HPLC finger-print especially, and the resulting evodia rutaecarpa water-soluble ingredient standard of method finger-print thus.
Background technology: Chinese medicine that China is traditional and preparation thereof lack the tight quality standard and the detection means of science mostly, be difficult to effectively control its inherent quality, can not guarantee the safe, effective of medication, also not meet the requirement of international medical market, seriously restrict the development of China's Chinese medicine industry.Strengthening the Chinese crude drug quality controling research is Chinese medicine standardization, standardized key issue.Have only the quality control of science that Chinese crude drug is carried out, could guarantee traditional Chinese medicine quality, realize " safety, effective, stable, controlled " of Chinese medicine.
Evodia rutaecarpa is rutaceae evodia rutaecarpa Evodia rutaecarpa (Juss.) Benth. or stone tiger Evodiarutaecarpa (Juss.) Benth.var.officinalis (Dode) Huang or the dry almost ripe fruit of dredging hair evodia rutaecarpa Evodiarutaecarpa (Juss.) Benth.var.bodinieri (Dode) Huang.When 8～November, fruit did not ftracture as yet, cut fruit branch, dry or low temperature drying, remove impurity such as debranching, leaf, carpopodium.Another name: rice spicy, smelly spicy tree, gas spicy, bent medicine, tea spicy etc.Evodia rutaecarpa is the conventional Chinese medicine material; It also is seedling medicine commonly used.Nature,taste and action with cure mainly: hot, bitter, hot; Slightly poisonous; The effect that eliminating cold to stop pain, stopping nausea and vomiting by lowering the adverse flow of QI and supporing yang antidiarrheal are arranged is usually used in treating jueyin headache, cold hernia stomachache, the disturbance of lower legs due to pathogenic cold and dampness, dysmenorrhea, abdominal distention, vomiting acid regurgitation, has loose bowels etc. just before dawn, controls aphtha outward, vascular hypertension.As everyone knows, evodia rutaecarpa medicinal ingredient complexity mainly comprises following a few class: alkaloid, bitter principle, benzo chromogen ketone, terpene, flavones, coumarin, lignanoid, steroid, volatile oil and organic acid.Studies show that the number of chemical composition of evodia rutaecarpa has various concrete pharmacological actions.Therefore, its a certain or several active components are detected, just lose comprehensively.The globality that can not truly reflect the evodia rutaecarpa drug effect.To control the quality of evodia rutaecarpa and prescribed preparation thereof fully and effectively, must be controlled its material group integral body.
That traditional Chinese medicine fingerprint is meant is common in certain Chinese crude drug or the Chinese patent drug, have distinctive certain class or the chromatogram of number constituents or the collection of illustrative plates of spectrum.Do not have under the clear and definite situation in the present stage Effective Components of Chinese Herb overwhelming majority, finger-print has great importance for the quality of effective control Chinese crude drug or Chinese patent drug.The Japan main manufacturing enterprise of Chinese prescription medicine just adopts the high-efficiency liquid-phase fingerprint control of quality in the eighties in 20th century.Germany, France also adopt the high-efficiency liquid-phase fingerprint method in to the quality control of ginkgo biloba p.e.In the plant herbal medicine guide that U.S. FDA was formulated in recent years clearly the method for quality control of finger-print as the compounding substances group.Finger-print is become a consensus of the international community at present as Chinese herbal medicine and extraction of substance amount control method thereof.In order effectively to control the quality of evodia rutaecarpa medicinal material, make more perfect, the science of its Quality Control Technology, the applicant has carried out comprehensive and systematic finger-print research to the water-soluble substances of evodia rutaecarpa, has set up the finger print measuring method of evodia rutaecarpa water-soluble extract
Summary of the invention:
The objective of the invention is to: method for building up and standard finger-print thereof that a kind of evodia rutaecarpa water-soluble fingerprint is provided.The present invention provides a kind of better evodia rutaecarpa method of quality control by to the research of evodia rutaecarpa water-soluble extractive HPLC fingerprint, has remedied the deficiency of existing Quality Control Technology, makes the Quality Control Technology of evodia rutaecarpa medicinal material more perfect, science.
The present invention is achieved in that the method for building up of evodia rutaecarpa water-soluble fingerprint may further comprise the steps:
(1) preparation of need testing solution: get the evodia rutaecarpa pulverizing medicinal materials, sieve, take by weighing sample, soak, refluxing extraction 8 hours adds ethanol after the cooling, filters, and filtrate is as need testing solution;
(2) preparation of reference substance solution: get an amount of reference substance, add water and make reference substance solution;
(3) measure: accurate respectively need testing solution and the reference substance solution drawn, measure with high performance liquid chromatograph; The evodia rutaecarpa need testing solution is injected high performance liquid chromatograph carry out wash-out, the phosphate aqueous solution with 0.04% is that A phase, acetonitrile are that B carries out gradient elution mutually, and eluent enters the DAD UV-detector, and detecting device is gathered the detection data of 35min;
(4) relative retention time and the peak area with the reference substance chromatographic peak is 1, calculates relative retention time and peak area, with finger-print software the data and the collection of illustrative plates of gained handled, and promptly obtains evodia rutaecarpa water-soluble ingredient standard finger-print.
Wherein, the chromatographic condition during high-performance liquid chromatogram determination is: chromatographic column is filler with the octadecylsilane chemically bonded silica; Moving phase is B phase acetonitrile and A 0.04% phosphate aqueous solution mutually; Detect wavelength 327 ± 1nm.
The preparation process of need testing solution is: get the evodia rutaecarpa pulverizing medicinal materials and cross 60 mesh sieves, take by weighing sample powder 2 grams, add the 25mL distilled water immersion, put 80 ℃ of water-bath refluxing extraction 8 hours, adding ethanol after the cooling, to make its content be 50%, leave standstill, the water-soluble membrane filtration with 0.45um promptly gets need testing solution.
Being prepared as of reference substance solution: water intaking ortho acid reference substance adds distilled water and makes the reference substance solution that every 1ml contains 10ug.
Accurate respectively need testing solution and each 10uL of reference substance solution of drawing in the step (3).
In the eluent gradient elution process, the A of eluent, B phase transformation turn to: during beginning, and A phase 95.0%, B phase 5.0%; During to 7min, A phase 92.0%, B phase 8.0%; During to 13min, A phase 89.0%, B phase 11.0%; During to 30min, A phase 70%, B phase 30%; During to 35min, A phase 70%, B phase 30%.
The evodia rutaecarpa water-soluble ingredient standard finger-print that obtains according to the method for building up of above-mentioned evodia rutaecarpa water-soluble fingerprint.
Shared peak in the described standard finger-print must not be less than 24.
Compared with prior art, the present invention has the following advantages:
1. studies show that the number of chemical composition of evodia rutaecarpa has various concrete pharmacological actions.Its a certain active component is detected, just lose comprehensively.The HPLC finger-print that the present invention sets up with the evodia rutaecarpa water-soluble extract has been represented the most of pharmacologically active of evodia rutaecarpa, can characterize the quality of evodia rutaecarpa medicinal material effectively.A kind of scientific approach of thoroughly evaluating evodia rutaecarpa medicinal material is provided, has can be used as one of standard index of evodia rutaecarpa quality testing and quality control.
2. the evodia rutaecarpa finger-print is done as a wholely to treat, paid attention to its whole facial feature, both avoided only measuring the one-sidedness that one, two chemical constitution is judged the evodia rutaecarpa total quality, having reduced again is the artificial possibility of handling of requisite quality.The present invention provides new reference standard for quality complete, that accurately estimate evodia rutaecarpa, for quality and the curative effect that improves evodia rutaecarpa and prescribed preparation thereof contributes.
3. the present invention has that method is easy, stable, precision is high and characteristics such as favorable reproducibility.Because finger-print is not in order to measure the accurate content of certain composition, but will fully reflect the information of chemical constitution.Therefore, the present invention is chosen in 327 ± 1nm wavelength place and measures, and it is more that it goes out the peak, and the information of reflection is more complete; Not only chlorogenic acid has bigger absorption, and the absorption value of other chromatographic peaks is good, and separating effect is satisfied, and baseline is steady.
4. in the past for measuring the content of certain chemical constitution in the evodia rutaecarpa, often will carry out complicated processing to sample, and the present invention selects its water soluble ingredient of refluxing extraction for use, extracting method is simple, and the time is short, has saved the cost and the time of check.
5. the peak of the inventive method gained water-soluble fingerprint is many, and peak shape is good, be easy to differentiate, and the similarity height, accurately and reliably.
The present invention is described further below in conjunction with embodiment and accompanying drawing.
Description of drawings:
Fig. 1 is with the 1. evodia rutaecarpa water-soluble fingerprint chromatogram that obtains of ZORBAX RX-C18 PN:880967-902 of chromatographic column.
Fig. 2 is with the 2. evodia rutaecarpa water-soluble fingerprint chromatogram that obtains of Hypersil ODS2 PN:13134350270 of chromatographic column.
Fig. 3 is with the 3. evodia rutaecarpa water-soluble fingerprint chromatogram that obtains of Hypersil ODS2 PN:13120520183 of chromatographic column.
Fig. 4 is the evodia rutaecarpa water-soluble fingerprint of measuring at 327nm, 254nm, 284nm, 344nm, 354nm wavelength place respectively.
Fig. 5 is the DAD full scan 3D figure of evodia rutaecarpa water-soluble composition.
Fig. 6 is the common pattern figure of evodia rutaecarpa medicinal material water-soluble fingerprint.
Fig. 7 is the stacking diagram of 36 batches of evodia rutaecarpa medicinal material water-soluble fingerprints.
Fig. 8 is the water-soluble HPLC finger-print of evodia rutaecarpa medicinal material.
Embodiment:
Embodiments of the invention: the method for building up of evodia rutaecarpa water-soluble HPLC finger-print and evodia rutaecarpa water-soluble ingredient standard finger-print
1. instrument and reagent
1.1 instrument
Agilent 1100 high performance liquid chromatographs; Agilent DAD detecting device; The Agilent chromatographic work station.
1.2 reagent
The chlorogenic acid reference substance is purchased in Nat'l Pharmaceutical ﹠ Biological Products Control Institute; Acetonitrile, chromatographically pure; Distilled water; The syringe-type nuclepore membrane filter, diameter 13mm, 0.45um; The evodia rutaecarpa medicinal material
2. method and result
2.1 the investigation of extraction conditions
Bath temperature in the middle of the leaching process and extraction time are investigated, according to extracting method and by the condition of (table 1), parallelly do nine experiments, calculate with chlorogenic acid contents, results sample 6. i.e. 80 ℃ of water-baths extractions was an optimum extraction condition in 8 hours, and whole spectrogram peak shape is better.
Table 1 extraction conditions is investigated
2.2 the selection of chromatographic condition
2.2.1 determining of moving phase and gradient elution program
The applicant investigates moving phase and gradient elution procedure condition, determines that its condition is as follows:
Table 2 eluent gradient elution program
| Time(min) | 0 | 7 | 13 | 30 | 35 |
| CH 3CN(％) | 5 | 8 | 11 | 30 | 30 |
| H 2O contains 0.04%H 3PO 4(％) | 95 | 92 | 89 | 70 | 70 |
2.2.2 the selection of chromatographic column
The applicant has investigated three different chromatographic columns [1. Agilent Technologies:ZORBAX RX-C18 PN:880967-902 (4.6 * 250mm, 5 μ m) 2. Dalian Yi Lite scientific instrument company limited: Hypersil ODS2 PN:13134350270 (4.0 * 250mm, 5mm) 3. Dalian Yi Lite scientific instrument company limited: Hypersil ODS2PN:13120520183 (4.6 * 250mm, 5mm)] under selected identical chromatographic conditions, measure.(seeing accompanying drawing 1, Fig. 2, shown in Figure 3)
By accompanying drawing 1, Fig. 2, Fig. 3 as can be seen 3. the separating effect of number post be better than preceding two chromatographic columns, so adopt 3. number post to set up evodia rutaecarpa water-soluble fingerprint.
2.2.3 detection wavelength determination
The applicant has selected 327,254,284,344nm and these five wavelength of 354nm detect (seeing accompanying drawing 4) simultaneously.
Also utilize the DAD diode array detector simultaneously, water-soluble portion is carried out full wavelength scanner, 327nm place chlorogenic acid has obtained the maximum absorption (seeing accompanying drawing 5).In the bigger absorption of selecting chlorogenic acid, the absorption value of other chromatographic peaks is good, and separating effect is satisfied, and baseline is steady, and this detects the finger-print that wavelength is done evodia rutaecarpa water-soluble so select 327nm.
By above experiment, determined that chromatographic condition is as follows:
Chromatographic column: octadecyl silane; Moving phase: acetonitrile and 0.04% phosphate aqueous solution; Flow velocity: 1mL/min; Detect wavelength 327 ± 1nm; Column temperature: 25 ℃.
3. the mensuration of water-soluble fingerprint
3.1.1 the preparation of evodia rutaecarpa water-soluble fingerprint
The preparation of reference substance solution: water intaking ortho acid reference substance adds distilled water and makes the reference substance solution that every 1ml contains 10ug.
Object of reference: select for use the water ortho acid as object of reference.
The preparation of need testing solution: get the evodia rutaecarpa pulverizing medicinal materials and cross 60 mesh sieves, take by weighing sample powder 2 grams, add the 25mL distilled water immersion, put 80 ℃ of water-bath refluxing extraction 8 hours, adding ethanol after the cooling, to make its content be 50%, leaves standstill, water-soluble membrane filtration with 0.45um promptly gets need testing solution.
Accurate respectively need testing solution and each 10uL of reference substance solution of drawing injects high performance liquid chromatograph respectively, measures, and writes down 35 minutes chromatogram, promptly obtains required finger-print.Determined that by reference substance spectrum peak No. 11 peaks are water ortho acid reference substance peaks.Relative retention time and calculated by peak area relative retention time and relative peak area with water ortho acid chromatographic peak.Simultaneously, with finger-print software gained data and collection of illustrative plates are handled and promptly obtained standard finger-print.
3.1.2 precision experiment
Get the evodia rutaecarpa medicinal material of Jiangxi camphor tree, prepare test sample by the need testing solution preparation method who sets up, continuous sample introduction 6 times is to detect index with the chlorogenic acid, and the RSD that calculates relative peak area is 0.14%, and the result shows that instrument precision is good.
3.1.3 stability experiment
Get the evodia rutaecarpa medicinal material at Tongren Jiangkou, prepare test sample by the need testing solution preparation method who sets up, respectively 0,2,4,8,12, the 24h sample introduction, sample size is 10 μ L, with the chlorogenic acid is to detect index, and the RSD that calculates relative peak area is 1.36%, the result showed in 24 hours, the figure of evodia rutaecarpa chromatographic fingerprinting is basicly stable, does not have significant change, meets the finger-print requirement.
3.1.4 reappearance experiment
Get 6 parts of the evodia rutaecarpa medicinal materials of Jiangxi camphor tree, by 6 parts of test samples of the parallel preparation of need testing solution preparation method of setting up, sample introduction is to detect index with the chlorogenic acid respectively, and the RSD that calculates relative peak area is 1.4%, and the result shows that the reappearance of method is good.
3.1.5 recovery experiment
Precision takes by weighing 6 parts of the evodia rutaecarpa medicinal materials of the Jiangxi camphor tree of measuring content, quantitatively adding reference substance chlorogenic acid 4.14mg (80%), 4.10mg (80%), 5.27mg (100%), 5.24mg (100%), 6.16mg (120%), 6.17mg (120%) put in the sample, prepare test sample by the need testing solution preparation method who sets up, carrying out HPLC by same chromatographic condition detects, calculate recovery rate the results are shown in Table 3.
The experiment of table 3 chlorogenic acid average recovery
| Sample size/mg | Reference substance addition/mg | The amount of recording/mg | The recovery/% | Average recovery rate/% | RSD/％ |
| 5.24 | 4.14 | 9.26 | 97.2 | 96.2 | 0.98 |
| 5.25 | 4.10 | 9.17 | 95.6 | ||
| 5.25 | 5.27 | 10.25 | 94.9 | ||
| 5.24 | 5.24 | 10.31 | 96.8 | ||
| 5.26 | 6.16 | 11.15 | 95.7 | ||
| 5.25 | 6.17 | 11.24 | 97.1 |
3.1.6 determining and similarity calculating of the total peak of evodia rutaecarpa water-soluble fingerprint
By the mensuration of evodia rutaecarpa water-soluble fingerprint, and, determine 24 at total peak by of the processing of finger-print software to chromatogram and determination data to 36 batches of different places of production, the whole nation.Obtained the water-soluble fingerprint stacking diagram (accompanying drawing 7) of 36 batches of medicinal materials, water-soluble fingerprint common pattern figure (accompanying drawing 6), the similarity analysis result (table 4) of water-soluble fingerprint is an object of reference with the water ortho acid wherein, its peak is No. 11 peaks (accompanying drawing 6).
Evodia rutaecarpa water-soluble fingerprint similarity calculating of the different places of production, the whole nation and similarity analysis result are as follows:
The similarity analysis result of 36 batches of evodia rutaecarpa medicinal materials of table 4 water-soluble fingerprint
| Numbering | The place of production | Related coefficient (median) | Related coefficient (average) | Coefficient (median) is harmonious | Coefficient (average) is harmonious |
| NO.1 | The Nanchang | 0.9868 | 0.9880 | 0.9866 | 0.9879 |
| NO.2 | The Tongren Sinan | 0.9703 | 0.9743 | 0.9749 | 0.9781 |
| NO.3 | Guangzhou-Sheng | 0.9635 | 0.9729 | 0.9638 | 0.9725 |
| NO.4 | Concoct in Jiangxi | 0.9792 | 0.9852 | 0.9823 | 0.9871 |
| NO.5 | Guangzhou-the process of preparing Chinese medicine | 0.9720 | 0.9800 | 0.9714 | 0.9789 |
| NO.6 | The Tongren Jiangkou | 0.9871 | 0.9887 | 0.9889 | 0.9903 |
| NO.7 | Zun Yi Feng Gang | 0.9901 | 0.9894 | 0.9915 | 0.9909 |
| NO.8 | Tongren jade screen 1 | 0.9836 | 0.9887 | 0.9861 | 0.9903 |
| NO.9 | The Hunan | 0.9795 | 0.9752 | 0.9827 | 0.9789 |
| NO.10 | Zhejiang is celestial fragrant | 0.8722 | 0.8897 | 0.8860 | 0.9015 |
| NO.11 | Guangxi 2 | 0.9742 | 0.9797 | 0.9779 | 0.9826 |
| NO.12 | The Bozhou, Anhui | 0.9308 | 0.9263 | 0.9403 | 0.9359 |
| NO.13 | Tongren jade screen 2 | 0.9760 | 0.9728 | 0.9797 | 0.9769 |
| NO.14 | The Pingwu, Sichuan | 0.9399 | 0.9407 | 0.9431 | 0.9428 |
| NO.15 | Xiang Tan, Hunan | 0.9292 | 0.9262 | 0.9403 | 0.9374 |
| NO.16 | The Shaanxi Shiquan | 0.9793 | 0.9727 | 0.9794 | 0.9734 |
| NO.17 | The Jiangxi camphor tree | 0.9639 | 0.9688 | 0.9653 | 0.9699 |
| NO.18 | Guangxi 1 | 0.9659 | 0.9753 | 0.9663 | 0.9750 |
| NO.19 | Zhejiang | 0.9728 | 0.9815 | 0.9748 | 0.9827 |
| NO.20 | Neck is closed in Anshun | 0.9794 | 0.9861 | 0.9823 | 0.9881 |
| NO.21 | Taizhou, Zhejiang | 0.8771 | 0.8893 | 0.8891 | 0.9001 |
| NO.22 | Yunnan | 0.9129 | 0.9041 | 0.9253 | 0.9175 |
| NO.23 | The Sichuan Aba | 0.9795 | 0.9849 | 0.9799 | 0.9850 |
| NO.24 | The Xingyi, Guizhou | 0.9266 | 0.9183 | 0.9365 | 0.9290 |
| NO.25 | Concoct in Guizhou | 0.9528 | 0.9657 | 0.9544 | 0.9662 |
| NO.26 | Anshun | 0.7036 | 0.7040 | 0.7554 | 0.7540 |
| NO.27 | Hubei Li Zhou | 0.9506 | 0.9508 | 0.9571 | 0.9568 |
| NO.28 | The Linxiang, Hunan | 0.9641 | 0.9528 | 0.9693 | 0.9596 |
| NO.29 | The Guizhou Tongren | 0.9796 | 0.9752 | 0.9823 | 0.9786 |
| NO.30 | Tongren Shiqian 2 | 0.9747 | 0.9691 | 0.9785 | 0.9737 |
| NO.31 | Anhui | 0.8556 | 0.8392 | 0.8764 | 0.8623 |
| NO.32 | Xi'an, Shaanxi | 0.9683 | 0.9636 | 0.9700 | 0.9662 |
| NO.33 | The Kaiyang, Kweiyang | 0.9792 | 0.9761 | 0.9824 | 0.9797 |
| NO.34 | Road, Zun Yi is true | 0.9895 | 0.9834 | 0.9911 | 0.9859 |
| NO.35 | The Tongren Shiqian | 0.9848 | 0.9825 | 0.9870 | 0.9850 |
| NO.36 | Tongren pine peach | 0.9718 | 0.9637 | 0.9757 | 0.9689 |
3.1.7 the description at common characteristic peak: (seeing accompanying drawing 6)
(1) characteristic peak has 24, and wherein the area maximum at No. 10 peaks is the highest.
(2) 2,3,4,5,6,11,12,17 the peak area and the peak height at totally eight peaks is bigger.
(3) peak height of reference substance water ortho acid, peak area and peak shape are all fine.The total finger-print of gained evodia rutaecarpa medicinal material such as accompanying drawing 6.
(4) similarity coefficient at common characteristic peak is except the NO.26 sample is low, and it is in all higher.The similarity that finger-print is described is higher, can be used as the water-soluble standard finger-print of evodia rutaecarpa medicinal material.
4. above experimental result shows, uses this method the evodia rutaecarpa water-soluble composition is measured, and method is simple and reliable.The finger-print of setting up, peak shape is good, the peak good separating effect, peak area is bigger.Can be used as the standard diagram of evodia rutaecarpa water-soluble composition.Provide a good method to evodia rutaecarpa plantation, the quality control of producing and the discriminating of evodia rutaecarpa.
Claims (8)
1. the method for building up of an evodia rutaecarpa water-soluble fingerprint, it is characterized in that: it may further comprise the steps:
(1) preparation of need testing solution: get the evodia rutaecarpa pulverizing medicinal materials, sieve, take by weighing sample, soak, refluxing extraction 8 hours adds ethanol after the cooling, filters, and filtrate is as need testing solution;
(2) preparation of reference substance solution: get an amount of reference substance, add water and make reference substance solution;
(3) measure: accurate respectively need testing solution and the reference substance solution drawn, measure with high performance liquid chromatograph; The evodia rutaecarpa need testing solution is injected high performance liquid chromatograph carry out wash-out, the phosphate aqueous solution with 0.04% is that A phase, acetonitrile are that B carries out gradient elution mutually, and eluent enters the DAD UV-detector, and detecting device is gathered the detection data of 35min;
(4) relative retention time and the peak area with the reference substance chromatographic peak is 1, calculates relative retention time and peak area, with finger-print software the data and the collection of illustrative plates of gained handled, and promptly obtains evodia rutaecarpa water-soluble ingredient standard finger-print.
2. according to the method for building up of the described evodia rutaecarpa water-soluble fingerprint of claim 1, it is characterized in that: the chromatographic condition during high-performance liquid chromatogram determination is: chromatographic column is filler with the octadecylsilane chemically bonded silica; Moving phase is B phase acetonitrile and A 0.04% phosphate aqueous solution mutually; Detect wavelength 327 ± 1nm.
3. according to the method for building up of the described evodia rutaecarpa water-soluble fingerprint of claim 1, it is characterized in that: the preparation process of need testing solution is: get the evodia rutaecarpa pulverizing medicinal materials and cross 60 mesh sieves, take by weighing sample powder 2 grams, add the 25mL distilled water immersion, put 80 ℃ of water-bath refluxing extraction 8 hours, adding ethanol after the cooling, to make its content be 50%, leaves standstill, water-soluble membrane filtration with 0.45um promptly gets need testing solution.
4. according to the method for building up of the described evodia rutaecarpa water-soluble fingerprint of claim 1, it is characterized in that: being prepared as of reference substance solution: water intaking ortho acid reference substance adds distilled water and makes the reference substance solution that every 1ml contains 10ug.
5. according to the method for building up of the described evodia rutaecarpa water-soluble fingerprint of claim 1, it is characterized in that: accurate respectively need testing solution and each 10uL of reference substance solution of drawing in the step (3).
6. according to the method for building up of the described evodia rutaecarpa water-soluble fingerprint of claim 1, it is characterized in that: in the eluent gradient elution process, the A of eluent, B phase transformation turn to: during beginning, and A phase 95.0%, B phase 5.0%; During to 7min, A phase 92.0%, B phase 8.0%; During to 13min, A phase 89.0%, B phase 11.0%; During to 30min, A phase 70%, B phase 30%; During to 35min, A phase 70%, B phase 30%.
7. the evodia rutaecarpa water-soluble ingredient standard finger-print that obtains of the method for building up of evodia rutaecarpa water-soluble fingerprint according to claim 1.
8. according to the described evodia rutaecarpa water-soluble ingredient standard of claim 7 finger-print, it is characterized in that: the shared peak in the described collection of illustrative plates must not be less than 24.
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| CN107356717A (en) * | 2017-08-01 | 2017-11-17 | 临沂大学 | A kind of quality evaluating method of Chinese medicine evodia rutaecarpa |
| CN107478743A (en) * | 2017-08-11 | 2017-12-15 | 洛阳泽达慧康医药科技有限公司 | A kind of method for establishing evodia rutaecarpa standard decoction finger-print processed |
| CN109212120A (en) * | 2018-09-30 | 2019-01-15 | 湖南省中医药研究院 | A kind of construction method and evodia rutaecarpa quality of medicinal material detection method of evodia rutaecarpa medicinal material characteristic spectrum |
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2006
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Cited By (7)
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| CN102141555A (en) * | 2010-12-27 | 2011-08-03 | 贵阳中医学院 | Method for establishing high-pressure liquid-phase fingerprinting of evodia and extractives thereof |
| CN102141555B (en) * | 2010-12-27 | 2013-04-10 | 贵阳中医学院 | Method for establishing high-pressure liquid-phase fingerprinting of evodia and extractives thereof |
| CN107356717A (en) * | 2017-08-01 | 2017-11-17 | 临沂大学 | A kind of quality evaluating method of Chinese medicine evodia rutaecarpa |
| CN107478743A (en) * | 2017-08-11 | 2017-12-15 | 洛阳泽达慧康医药科技有限公司 | A kind of method for establishing evodia rutaecarpa standard decoction finger-print processed |
| CN109212120A (en) * | 2018-09-30 | 2019-01-15 | 湖南省中医药研究院 | A kind of construction method and evodia rutaecarpa quality of medicinal material detection method of evodia rutaecarpa medicinal material characteristic spectrum |
| CN113759018A (en) * | 2021-02-24 | 2021-12-07 | 北京康仁堂药业有限公司 | Evaluation method of evodia rutaecarpa decoction preparation process |
| CN113759018B (en) * | 2021-02-24 | 2023-04-18 | 北京康仁堂药业有限公司 | Evaluation method of evodia rutaecarpa decoction preparation process |
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