CN102297923A - Method for fingerprint detection of Guanxinqiwei dripping pills - Google Patents
Method for fingerprint detection of Guanxinqiwei dripping pills Download PDFInfo
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Abstract
The invention discloses a method for fingerprint detection of Guanxinqiwei dripping pills. The method comprises the following steps of 1, carrying out gradient elution through adopting octadecylsilane chemically bonded silica as a filler, a formic acid solution as a mobile phase A and acetonitrile as mobile phase B, and carrying out detection by an ultraviolet detector, 2, preparing a reference solution through the process of dissolving an appropriate amount of a salvianolic acid B in methanol, 3, preparing a solution needing to be detected through the processes of collecting Guanxinqiwei dripping pills, grinding into powder, putting an appropriate amount of the powder into an erlenmeyer flask, adding methanol into the erlenmeyer flask, carrying out ultrasonic treatment, filtering and collecting subsequent filtrate, and 4, detecting the sample solution obtained by the step 3 through the processes of taking accurately the solution needing to be detected and the reference solution by suction, injecting them into a liquid chromatograph, recording chromatograms and carrying out calculation according to a traditional Chinese medicine chromatogram fingerprint similarity evaluation system, wherein the similarity of a sample fingerprint and a reference fingerprint shall not be less than 0.90. The method for fingerprint detection of Guanxinqiwei dripping pills has the advantages of strong specificity, good stability and good reproducibility.
Description
Technical field
The present invention relates to a kind of finger-print and detection method of dripping pill, particularly a kind of detection method of coronary disease seven flavor dripping pill finger-prints.
Background technology
Coronary disease seven flavor dripping pills be the applicant on the basis of coronary disease tablet of seven ingredients, the novel form that uses present Chinese medicine preparation technology to make, however the coronary disease tablet of seven ingredients has only the coherence check of proterties and tablet aspect quality control, can not control the inherent quality of product substantially.
Coronary disease seven flavor dripping pills of the present invention have increased the quality control of aspects such as discriminating, assay and finger-print, can effectively control the quality of product, thereby guarantee the curative effect of product.Wherein finger-print is used for the quality control genus initiative of coronary disease seven flavor dripping pills.
Summary of the invention
The object of the invention is to provide a kind of detection method of coronary disease seven flavor dripping pill finger-prints.
The present invention is achieved through the following technical solutions:
A kind of detection method of coronary disease seven flavor dripping pill finger-prints, this method comprises the steps:
Chromatographic condition and system suitability test: chromatographic column Inertsil ODS-3 150 * 4.6mm, 5 μ m; 25～45 ℃ of column temperatures; With the octadecylsilane chemically bonded silica is filling agent; With 0.1～3.0% formic acid solution is mobile phase A, and acetonitrile is a Mobile phase B, flow velocity 0.5～1.5ml/min; Carry out gradient elution by following program: since 0 minute to 45 minutes, mobile phase A became 20% by 85%, and since 45 minutes to 55 minutes, mobile phase A became 85% by 20%, and is maintained until 65 minutes, and gradient is linear gradient;
Prepare with reference to the peak: get tanshin polyphenolic acid B reference substance 0.005-0.015 weight portion, the accurate title, decide, and adds 65～85% methyl alcohol and make the solution that every 0.5-1.5 parts by volume contains the 0.0001-0.0003 weight portion, promptly;
The need testing solution preparation: get coronary disease seven flavor dripping pills, porphyrize is got 0.2～0.4 weight portion, the accurate title, decide, and puts in the conical flask, accurate 65～85% methyl alcohol, 20～80 parts by volume that add, claim to decide weight, power 220～350W, frequency 20-60kHz sonicated 7～23 minutes, put coldly, claim again to decide weight, supply with 65～85% methyl alcohol and subtract weight loss, shake up, filter, get subsequent filtrate, promptly;
Determination method: accurate respectively the absorption with reference to product solution and each 5～15 μ l of need testing solution, inject liquid chromatograph, UV-detector detects, and the mensuration wavelength is 280nm, the record chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press chromatographic fingerprints of Chinese materia medica similarity evaluation system-computed, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90.
The detection method of coronary disease seven flavor dripping pill finger-prints of the present invention comprises the steps:
Chromatographic condition and system suitability test: chromatographic column Inertsil ODS-3 150 * 4.6mm, 5 μ m; 35 ℃ of column temperatures; With the octadecylsilane chemically bonded silica is filling agent; With 1.0% formic acid solution is mobile phase A, and acetonitrile is a Mobile phase B, flow velocity 1.0ml/min; Carry out gradient elution by following program: since 0 minute to 45 minutes, mobile phase A became 20% by 85%, and since 45 minutes to 55 minutes, mobile phase A became 85% by 20%, and is maintained until 65 minutes, and gradient is linear gradient;
Reference product formulations prepared from solutions: get tanshin polyphenolic acid B reference substance 0.01 weight portion, the accurate title, decide, and adds 75% methyl alcohol and make the solution that per 1 parts by volume contains 0.001 weight portion, promptly;
The need testing solution preparation: get coronary disease seven flavor dripping pills, porphyrize is got 0.3 weight portion, the accurate title, decide, and puts in the conical flask, accurate 75% methyl alcohol, 50 parts by volume that add, claim to decide weight, power 280W, frequency 40kHz sonicated 15 minutes, put coldly, claim again to decide weight, supply with 75% methyl alcohol and subtract weight loss, shake up, filter, get subsequent filtrate, promptly;
Determination method: accurate respectively the absorption with reference to product solution and each 10 μ l of need testing solution, inject liquid chromatograph, UV-detector detects, and the mensuration wavelength is 280nm, the record chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press chromatographic fingerprints of Chinese materia medica similarity evaluation system-computed, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90.
14 corresponding characteristic peaks are in the coronary disease seven flavor dripping pill finger-prints of the present invention:
No. 1 peak: relative retention time 0.170-0.208, the area that accounts for reference to the peak compares 1.48%-28.03%;
No. 2 peak: relative retention time 0.199-0.243, the area that accounts for reference to the peak compares 1.33%-25.29%;
No. 3 peak: relative retention time 0.332-0.406, the area that accounts for reference to the peak compares 0.40%-7.63%;
No. 4 peak: relative retention time 0.772-0.943, the area that accounts for reference to the peak compares 1.26%-23.94%;
No. 5 peak: relative retention time 0.811-0.991, the area that accounts for reference to the peak compares 1.18%-22.46%;
No. 6 peaks: be the reference peak;
No. 7 peak: relative retention time 0.965-1.180, the area that accounts for reference to the peak compares 18.69%-43.61%;
No. 8 peak: relative retention time 1.544-1.887, the area that accounts for reference to the peak compares 1.33%-25.22%;
No. 9 peak: relative retention time 1.614-1.973, the area that accounts for reference to the peak compares 33.20%-68.96%;
No. 10 peak: relative retention time 1.802-2.203, the area that accounts for reference to the peak compares 1.22%-23.21%;
No. 11 peak: relative retention time 2.087-2.550, the area that accounts for reference to the peak compares 20.10%-46.90%;
No. 12 peak: relative retention time 2.493-3.047, the area that accounts for reference to the peak compares 0.50%-9.48%;
No. 13 peak: relative retention time 2.540-3.104, the area that accounts for reference to the peak compares 1.50%-28.44%; No. 14 peak: relative retention time 2.958-3.616, the area that accounts for reference to the peak compares 13.56%-31.64%.
14 corresponding characteristic peaks are in the coronary disease seven flavor dripping pill finger-prints of the present invention:
No. 1 peak: relative retention time 0.170-0.208, the area that accounts for reference to the peak compares 8.48%-20.03%;
No. 2 peak: relative retention time 0.199-0.243, the area that accounts for reference to the peak compares 7.33%-20.29%;
No. 3 peak: relative retention time 0.332-0.406, the area that accounts for reference to the peak compares 2.40%-5.63%;
No. 4 peak: relative retention time 0.772-0.943, the area that accounts for reference to the peak compares 8.26%-19.94%;
No. 5 peak: relative retention time 0.811-0.991, the area that accounts for reference to the peak compares 8.18%-18.46%;
No. 6 peaks: be the reference peak;
No. 7 peak: relative retention time 0.965-1.180, the area that accounts for reference to the peak compares 25.69%-35.61%;
No. 8 peak: relative retention time 1.544-1.887, the area that accounts for reference to the peak compares 8.33%-20.22%;
No. 9 peak: relative retention time 1.614-1.973, the area that accounts for reference to the peak compares 45.20%-60.96%;
No. 10 peak: relative retention time 1.802-2.203, the area that accounts for reference to the peak compares 8.22%-18.21%;
No. 11 peak: relative retention time 2.087-2.550, the area that accounts for reference to the peak compares 30.10%-40.90%;
No. 12 peak: relative retention time 2.493-3.047, the area that accounts for reference to the peak compares 3.50%-6.48%;
No. 13 peak: relative retention time 2.540-3.104, the area that accounts for reference to the peak compares 10.50%-20.44%;
No. 14 peak: relative retention time 2.958-3.616, the area that accounts for reference to the peak compares 18.56%-28.64%.
14 corresponding characteristic peaks are in the coronary disease seven flavor dripping pill finger-prints of the present invention:
No. 1 peak: relative retention time 0.189 accounts for area with reference to the peak than 14.75%;
No. 2 peaks: relative retention time 0.221 accounts for area with reference to the peak than 13.31%;
No. 3 peaks: relative retention time 0.369 accounts for area with reference to the peak than 4.02%;
No. 4 peaks: relative retention time 0.857 accounts for area with reference to the peak than 12.60%;
No. 5 peaks: relative retention time 0.901 accounts for area with reference to the peak than 11.82%;
No. 6 peaks: be the reference peak;
No. 7 peaks: relative retention time 1.073 accounts for area with reference to the peak than 31.15%;
No. 8 peaks: relative retention time 1.716 accounts for area with reference to the peak than 13.27%;
No. 9 peaks: relative retention time 1.793 accounts for area with reference to the peak than 51.08%;
No. 10 peaks: relative retention time 2.002 accounts for area with reference to the peak than 12.22%;
No. 11 peaks: relative retention time 2.318 accounts for area with reference to the peak than 33.50%;
No. 12 peaks: relative retention time 2.770 accounts for area with reference to the peak than 4.99%;
No. 13 peaks: relative retention time 2.822 accounts for area with reference to the peak than 14.97%;
No. 14 peaks: relative retention time 3.287 accounts for area with reference to the peak than 22.60%.
Coronary disease seven flavor dripping pills of the present invention are made by following method:
The bulk drug of coronary disease seven flavor dripping pills of the present invention consists of:
Red sage root 19.2-57.6 weight portion santal 2.1-6.5 weight portion dalbergia wood 4.2-12.8 weight portion
Kaempferia galanga 3.2-9.6 weight portion nutmeg 6.4-19.2 weight portion fructus choerospondiatis 6.4-19.2 weight portion
Sea-buckthorn 6.4-19.2 weight portion
The bulk drug composition of coronary disease seven flavor dripping pills of the present invention is preferably:
The red sage root 38.4 weight portion santals 4.3 weight portion dalbergia woods 8.5 weight portions
Kaempferia galanga 6.4 weight portion nutmegs 12.8 weight portion fructus choerospondiatis 12.8 weight portions
Sea-buckthorn 12.8 weight portions;
Or the red sage root 21 weight portion santals 6 weight portion dalbergia woods 6 weight portions
Sea-buckthorn 8 weight portions;
Or the red sage root 50 weight portion santals 3 weight portion dalbergia woods 11 weight portions
Sea-buckthorn 18 weight portions.
The preparation method of coronary disease seven flavor dripping pills of the present invention is:
More than seven flavors, santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 2-8 hour with 5-10 times of water gaging, the aqueous solution after distillation device is in addition collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor medicinal materials are doubly measured the 75-95% alcohol reflux 1-3 time with 2-8, each 0.5-1.5 hour, filter, collect filtrate, the dregs of a decoction decoct 1-3 time with 4-10 times of water gaging, each 1-2 hour, filter, collect filtrate, relative density is 1.30～1.40 thick paste when concentrating each extract to 60 ℃ respectively, merge above-mentioned aqueous solution and filtrate, 80 ℃ of drying under reduced pressure are ground into fine powder, get extract powder, add volatile oil, the PEG400 of 2-10 weight portion, the Macrogol 4000 of 20-28 weight portion is a cooling medium with the dimethyl silicon oil, makes dripping pill.
The preparation method of coronary disease seven flavor dripping pills of the present invention is preferably:
More than seven flavors, santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 5 hours with 7.8 times of water gagings, the device collection in addition of the aqueous solution after the distillation; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor medicinal materials are measured 95% alcohol reflux secondaries with 5 times, each 1 hour, filter, collect filtrate, the dregs of a decoction decoct secondary with 7 times of water gagings, each 1.5 hours, filter, collect filtrate, relative density is 1.30～1.40 thick paste when concentrating each extract to 60 ℃ respectively, merge each thick paste, 80 ℃ of drying under reduced pressure are ground into fine powder, get extract powder, adding volatile oil, the PEG400 of 5 weight portions, the Macrogol 4000 of 25 weight portions, is cooling medium with the dimethyl silicon oil, makes dripping pill.
The corresponding relation of weight portion of the present invention and parts by volume is g/ml or kg/l.
The detection method advantage of coronary disease seven flavor dripping pills of the present invention is: (1) specificity is strong, and this finger-print is that coronary disease seven flavor dripping pills are exclusive, and the chemical information of its reflection is to have height optionally.(2) good stability, this finger-print are the general character of summarizing from many batches of coronary diseases seven flavor dripping pills, and the characteristic peak in the collection of illustrative plates is stable.(3) favorable reproducibility, this finger print measuring method can be reproduced the fingerprint characteristic of coronary disease seven flavor dripping pills under the regulation condition determination.The quality and the curative effect of control coronary disease seven flavor dripping pills are significant.
Description of drawings
Fig. 1 is a reference fingerprint;
Fig. 2 is with reference to the product collection of illustrative plates;
Fig. 3 is a reference fingerprint;
Fig. 4 is sample 2 collection of illustrative plates;
Fig. 5 is sample 3 collection of illustrative plates;
Fig. 6 is sample 4 collection of illustrative plates;
Fig. 7 is sample 5 collection of illustrative plates;
Fig. 8 is sample 6 collection of illustrative plates;
Fig. 9 is sample 7 collection of illustrative plates;
Figure 10 is sample 8 collection of illustrative plates;
Figure 11 is sample 9 collection of illustrative plates;
Figure 12 is sample 10 collection of illustrative plates;
Figure 13 is sample 11 collection of illustrative plates.
Following experimental example is used to further specify the present invention, but is not limited to the present invention.
Experimental example one: chromatographic system screening experiment
1, the selection of moving phase selects three kinds of moving phases to test.
First kind of moving phase: with 1.0% formic acid solution is mobile phase A, and acetonitrile is a Mobile phase B, flow velocity 0.8ml/min; Carry out gradient elution by following program: since 0 minute to 50 minutes, mobile phase A became 10% by 90%, and since 50 minutes to 65 minutes, mobile phase A became 90% by 10%, and is maintained until 75 minutes, and gradient is linear gradient.
Second kind of moving phase: with water is mobile phase A, and acetonitrile is a Mobile phase B, flow velocity 1.0ml/min; Carry out gradient elution by following program: since 0 minute to 45 minutes, mobile phase A became 20% by 85%, and since 45 minutes to 55 minutes, mobile phase A became 85% by 20%, and is maintained until 65 minutes, and gradient is linear gradient.
The third moving phase: with 1.0% formic acid solution is mobile phase A, and acetonitrile is a Mobile phase B, flow velocity 1.0ml/min; Carry out gradient elution by following program: since 0 minute to 45 minutes, mobile phase A became 20% by 85%, and since 45 minutes to 55 minutes, mobile phase A became 85% by 20%, and is maintained until 65 minutes, and gradient is linear gradient.
Test findings: the finger-print peak type and the degree of separation of the third moving phase gained are all best, and acquisition time is also less, so select the third moving phase.
2, the selection of chromatographic column selects four kinds of chromatographic columns to test.
First kind of chromatographic column: Alltech C18 250 * 4.6mm, 5 μ m.
Second kind of chromatographic column: Waters C18 250 * 4.6mm, 5 μ m.
The third chromatographic column: Yi Lite C18 250 * 4.6mm, 5 μ m.
The 4th kind of chromatographic column: Inertsil ODS-3 150 * 4.6mm, 5 μ m
Test findings: except that the finger-print peak type of the third chromatographic column gained and degree of separation are relatively poor, its excess-three kind chromatographic column is all better, and the finger-print peak type and the degree of separation of the 4th kind of chromatographic column gained are best, so final definite the 4th kind of chromatographic column (Inertsil ODS-3 150 * 4.6mm, 5 μ m) of using.
Experimental example two, coronary disease of the present invention seven flavor dripping pill detection method experiments
1, coronary disease seven flavor dripping pill finger-print test methods of the present invention
(1) chromatographic condition
Chromatographic column: Inertsil ODS-3 150 * 4.6mm, 5 μ m
Column temperature: 35 ℃
Moving phase: A, 1% formic acid solution
B, acetonitrile
Carry out gradient elution by following program:
Flow velocity: 1.0ml/min
| | A | B | |
| 0 | 85 | 15 | |
| 45 | 20 | 80 | |
| 55 | 85 | 15 | |
| 65 | 85 | 15 |
(2), prepare with reference to the peak
It is an amount of to get the tanshin polyphenolic acid B reference substance, and accurate the title decides, and adds 75% methyl alcohol and makes the solution that every 1ml contains 0.1mg, promptly.
(3), need testing solution preparation
Get coronary disease seven flavor dripping pills, porphyrize is got about 0.3g, and accurate the title decides, and puts in the conical flask, the accurate 75% methyl alcohol 50ml that adds, claim decide weight, sonicated (power 280W, frequency 40kHz) 15 minutes is put coldly, and weight decided in title again, supply with 75% methyl alcohol and to subtract weight loss, shake up, filter, get subsequent filtrate, promptly.
(4), determination method is respectively accurate draws with reference to product solution and each 10 μ l of need testing solution, injects liquid chromatograph, UV-detector detects, the mensuration wavelength is 280nm, writes down chromatogram.
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press chromatographic fingerprints of Chinese materia medica similarity evaluation system-computed, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90.
2, standard finger-print (see figure 1)
Instrument, chromatographic column and integral parameter: Waters2695-2996 high performance liquid chromatograph, Empower chromatographic work station.Chromatographic column be Inertsil ODS-3 (150mm * 4.6mm, 5um); 35 ℃ of column temperatures.Slope: 50; Peak width: 30.
3, to the explanation of finger-print
Coronary disease seven flavor dripping pills are prepared from by seven flavor Chinese medicines, and wherein three flavor salviamiltiorrhizabungs, fructus choerospondiatis and myristic correlated characteristic composition all have embodiment in finger-print.
Such as: the composition danshensu in the red sage root (No. 2 peaks), protocatechualdehyde (No. 3 peaks), tanshin polyphenolic acid B (S peak); Composition gallic acid in the fructus choerospondiatis (No. 1 peak); Volatile ingredient in the nutmeg: dehydrogenation two isoeugenols (No. 11 peaks), all embody in finger-print.So this method is significant to the quality control of coronary disease seven flavor dripping pills.
4, sample determining fingerprint pattern
(1) chromatographic condition
Chromatographic column: Inertsil ODS-3 150 * 4.6mm, 5 μ m
Column temperature: 35 ℃
Moving phase: A, 1% formic acid solution
C, acetonitrile
Carry out gradient elution by following program:
Flow velocity: 1.0ml/min
| | A | B | |
| 0 | 85 | 15 | |
| 45 | 20 | 80 | |
| 55 | 85 | 15 | |
| 65 | 85 | 15 |
(2), prepare with reference to the peak
It is an amount of to get the tanshin polyphenolic acid B reference substance, and accurate the title decides, and adds 75% methyl alcohol and makes the solution that every 1ml contains 0.1mg, promptly.
(3), need testing solution preparation
(4), determination method is respectively accurate draws with reference to product solution and each 10 μ l of need testing solution, injects liquid chromatograph, UV-detector detects, the mensuration wavelength is 280nm, writes down chromatogram.
Discussion of results: the finger-print of comparative sample 1～11, find: 1., 14 of total chromatographic peaks are all arranged in 11 batch samples; 2., the finger-print of sample 1 is the most representative, so determine that the finger-print of sample 1 is a reference fingerprint.
The finger-print and the reference fingerprint of other samples are compared, in the test sample chromatogram, 14 and reference fingerprint characteristic of correspondence peak are all arranged, press chromatographic fingerprints of Chinese materia medica similarity evaluation system-computed, the similarity of test sample finger-print and reference fingerprint is all greater than 0.90.
| Sample number into spectrum | Characteristic | Similarity |
| Sample | ||
| 1 | 14 | 1.00 |
| |
14 | 9.92 |
| |
14 | 9.89 |
| |
14 | 9.90 |
| |
14 | 9.88 |
| |
14 | 9.93 |
| |
14 | 9.95 |
| |
14 | 9.87 |
| |
14 | 9.91 |
| |
14 | 9.90 |
| |
14 | 9.89 |
Finger-print is seen Fig. 2-Figure 12.
Following embodiment all can realize the effect of above-mentioned experimental example.
Red sage root 38.4g santal 4.3g dalbergia wood 8.5g Kaempferia galanga 6.4g
Nutmeg 12.8g fructus choerospondiatis 12.8g sea-buckthorn 12.8g
More than seven flavors, santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 5 hours with 7.8 times of water gagings, the device collection in addition of the aqueous solution after the distillation; Three flavor medicinal materials such as the dregs of a decoction and all the other reds sage root each 1 hour, filter with 5 times of amount 95% alcohol reflux secondaries, collect filtrate, the dregs of a decoction decoct secondary, each 1.5 hours with 7 times of water gagings, filter, collect filtrate, concentrating each extract to relative density respectively is the thick paste of 1.30～1.40 (60 ℃), merge each thick paste, 80 ℃ of drying under reduced pressure are ground into fine powder, extract powder, add volatile oil and PEG400, Macrogol 4000 is an amount of, is cooling medium with the dimethyl silicon oil, make dripping pill, promptly.
Detection method:
Chromatographic condition and system suitability test: chromatographic column Inertsil ODS-3 150 * 4.6mm, 5 μ m; 35 ℃ of column temperatures; With the octadecylsilane chemically bonded silica is filling agent; With 1.0% formic acid solution is mobile phase A, and acetonitrile is a Mobile phase B, flow velocity 1.0ml/min; Carry out gradient elution by following program: since 0 minute to 45 minutes, mobile phase A became 20% by 85%, and since 45 minutes to 55 minutes, mobile phase A became 85% by 20%, and is maintained until 65 minutes, and gradient is linear gradient;
Prepare with reference to the peak: get tanshin polyphenolic acid B reference substance 0.01g, the accurate title, decide, and adds 75% methyl alcohol and make the solution that every 1ml contains 0.0001g, promptly;
The need testing solution preparation: get coronary disease seven flavor dripping pills, porphyrize is got about 0.3g, the accurate title, decide, and puts in the conical flask, the accurate 75% methyl alcohol 50ml that adds, claim to decide weight, power 280W, frequency 40kHz sonicated 15 minutes, put coldly, claim again to decide weight, supply with 75% methyl alcohol and subtract weight loss, shake up, filter, get subsequent filtrate, promptly;
Determination method: accurate respectively the absorption with reference to product solution and each 10 μ l of need testing solution, inject liquid chromatograph, UV-detector detects, and the mensuration wavelength is 280nm, the record chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press chromatographic fingerprints of Chinese materia medica similarity evaluation system-computed, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90;
14 corresponding characteristic peaks are in the described coronary disease seven flavor dripping pill finger-prints:
No. 1 peak: relative retention time 0.189 accounts for area with reference to the peak than 14.75%;
No. 2 peaks: relative retention time 0.221 accounts for area with reference to the peak than 13.31%;
No. 3 peaks: relative retention time 0.369 accounts for area with reference to the peak than 4.02%;
No. 4 peaks: relative retention time 0.857 accounts for area with reference to the peak than 12.60%;
No. 5 peaks: relative retention time 0.901 accounts for area with reference to the peak than 11.82%;
No. 6 peaks: be the reference peak;
No. 7 peaks: relative retention time 1.073 accounts for area with reference to the peak than 31.15%;
No. 8 peaks: relative retention time 1.716 accounts for area with reference to the peak than 13.27%;
No. 9 peaks: relative retention time 1.793 accounts for area with reference to the peak than 51.08%;
No. 10 peaks: relative retention time 2.002 accounts for area with reference to the peak than 12.22%;
No. 11 peaks: relative retention time 2.318 accounts for area with reference to the peak than 33.50%;
No. 12 peaks: relative retention time 2.770 accounts for area with reference to the peak than 4.99%;
No. 13 peaks: relative retention time 2.822 accounts for area with reference to the peak than 14.97%;
No. 14 peaks: relative retention time 3.287 accounts for area with reference to the peak than 22.60%.
Red sage root 21g santal 6g dalbergia wood 6g Kaempferia galanga 8g nutmeg 8g
Fructus choerospondiatis 18g sea-buckthorn 8g
More than seven flavors, santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 5 hours with 7.8 times of water gagings, the device collection in addition of the aqueous solution after the distillation; Three flavor medicinal materials such as the dregs of a decoction and all the other reds sage root each 1 hour, filter with 5 times of amount 95% alcohol reflux secondaries, collect filtrate, the dregs of a decoction decoct secondary, each 1.5 hours with 7 times of water gagings, filter, collect filtrate, concentrating each extract to relative density respectively is the thick paste of 1.30～1.40 (60 ℃), merge each thick paste, 80 ℃ of drying under reduced pressure are ground into fine powder, extract powder, add volatile oil and PEG400, Macrogol 4000 is an amount of, is cooling medium with the dimethyl silicon oil, make dripping pill, promptly.
Detection method:
Chromatographic condition and system suitability test: chromatographic column Inertsil ODS-3 150 * 4.6mm, 5 μ m; 30 ℃ of column temperatures; With the octadecylsilane chemically bonded silica is filling agent; With 2.0% formic acid solution is mobile phase A, and acetonitrile is a Mobile phase B, flow velocity 0.8ml/min; Carry out gradient elution by following program: since 0 minute to 45 minutes, mobile phase A became 20% by 85%, and since 45 minutes to 55 minutes, mobile phase A became 85% by 20%, and is maintained until 65 minutes, and gradient is linear gradient;
Prepare with reference to the peak: get tanshin polyphenolic acid B reference substance 0.008g, the accurate title, decide, and adds 80% methyl alcohol and make the solution that every 0.7ml contains 0.00013g, promptly;
The need testing solution preparation: get coronary disease seven flavor dripping pills, porphyrize is got 0.2g, the accurate title, decide, and puts in the conical flask, the accurate 70% methyl alcohol 30ml that adds, claim to decide weight, power 250W, frequency 30kHz sonicated 20 minutes, put coldly, claim again to decide weight, supply with 80% methyl alcohol and subtract weight loss, shake up, filter, get subsequent filtrate, promptly;
Determination method: accurate respectively the absorption with reference to product solution and each 7 μ l of need testing solution, inject liquid chromatograph, UV-detector detects, and the mensuration wavelength is 280nm, the record chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press chromatographic fingerprints of Chinese materia medica similarity evaluation system-computed, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90;
14 corresponding characteristic peaks are in the described coronary disease seven flavor dripping pill finger-prints:
No. 1 peak: relative retention time 0.175 accounts for area with reference to the peak than 25.03%;
No. 2 peaks: relative retention time 0.201 accounts for area with reference to the peak than 20.21%;
No. 3 peaks: relative retention time 0.365 accounts for area with reference to the peak than 6.13%;
No. 4 peaks: relative retention time 0.812 accounts for area with reference to the peak than 20.73%;
No. 5 peaks: relative retention time 0.851 accounts for area with reference to the peak than 20.16%;
No. 6 peaks: be the reference peak;
No. 7 peaks: relative retention time 0.986 accounts for area with reference to the peak than 38.11%;
No. 8 peaks: relative retention time 1.612 accounts for area with reference to the peak than 21.12%;
No. 9 peaks: relative retention time 1.634 accounts for area with reference to the peak than 60.92%;
No. 10 peaks: relative retention time 1.832 accounts for area with reference to the peak than 20.11%;
No. 11 peaks: relative retention time 2.137 accounts for area with reference to the peak than 41.30%;
No. 12 peaks: relative retention time 2.523 accounts for area with reference to the peak than 7.68%;
No. 13 peaks: relative retention time 2.610 accounts for area with reference to the peak than 26.34%;
No. 14 peaks: relative retention time 2.983 accounts for area with reference to the peak than 28.34%.
Red sage root 50g santal 3g dalbergia wood 11g Kaempferia galanga 4g nutmeg g
Fructus choerospondiatis 8g sea-buckthorn 18g
More than seven flavors, santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 5 hours with 7.8 times of water gagings, the device collection in addition of the aqueous solution after the distillation; Three flavor medicinal materials such as the dregs of a decoction and all the other reds sage root each 1 hour, filter with 5 times of amount 95% alcohol reflux secondaries, collect filtrate, the dregs of a decoction decoct secondary, each 1.5 hours with 7 times of water gagings, filter, collect filtrate, concentrating each extract to relative density respectively is the thick paste of 1.30～1.40 (60 ℃), merge each thick paste, 80 ℃ of drying under reduced pressure are ground into fine powder, extract powder, add volatile oil and PEG400, Macrogol 4000 is an amount of, is cooling medium with the dimethyl silicon oil, make dripping pill, promptly.
Detection method:
Chromatographic condition and system suitability test: chromatographic column Inertsil ODS-3 150 * 4.6mm, 5 μ m; 40 ℃ of column temperatures; With the octadecylsilane chemically bonded silica is filling agent; With 0.5% formic acid solution is mobile phase A, and acetonitrile is a Mobile phase B, flow velocity 1.2ml/min; Carry out gradient elution by following program: since 0 minute to 45 minutes, mobile phase A became 20% by 85%, and since 45 minutes to 55 minutes, mobile phase A became 85% by 20%, and is maintained until 65 minutes, and gradient is linear gradient;
Prepare with reference to the peak: get tanshin polyphenolic acid B reference substance 0.012g, the accurate title, decide, and adds 70% methyl alcohol and make the solution that every 1.3ml contains 0.00007g, promptly.
The need testing solution preparation: get coronary disease seven flavor dripping pills, porphyrize is got 0.4g, the accurate title, decide, and puts in the conical flask, the accurate 80% methyl alcohol 70ml that adds, claim to decide weight, power 320W, frequency 50kHz sonicated 10 minutes, put coldly, claim again to decide weight, supply with 70% methyl alcohol and subtract weight loss, shake up, filter, get subsequent filtrate, promptly;
Determination method: accurate respectively the absorption with reference to product solution and each 12 μ l of need testing solution, inject liquid chromatograph, UV-detector detects, and the mensuration wavelength is 280nm, the record chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press chromatographic fingerprints of Chinese materia medica similarity evaluation system-computed, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90;
14 corresponding characteristic peaks are in the described coronary disease seven flavor dripping pill finger-prints:
No. 1 peak: relative retention time 0.201 accounts for area with reference to the peak than 1.89%;
No. 2 peaks: relative retention time 0.223 accounts for area with reference to the peak than 1.56%;
No. 3 peaks: relative retention time 0.398 accounts for area with reference to the peak than 0.65%;
No. 4 peaks: relative retention time 0.875 accounts for area with reference to the peak than 1.51%;
No. 5 peaks: relative retention time 0.973 accounts for area with reference to the peak than 1.68%;
No. 6 peaks: be the reference peak;
No. 7 peaks: relative retention time 1.165 accounts for area with reference to the peak than 20.63%;
No. 8 peaks: relative retention time 1.851 accounts for area with reference to the peak than 1.83%;
No. 9 peaks: relative retention time 1.651 accounts for area with reference to the peak than 35.12%;
No. 10 peaks: relative retention time 2.123 accounts for area with reference to the peak than 1.51%;
No. 11 peaks: relative retention time 2.356 accounts for area with reference to the peak than 22.33%;
No. 12 peaks: relative retention time 3.027 accounts for area with reference to the peak than 0.78%;
No. 13 peaks: relative retention time 3.002 accounts for area with reference to the peak than 1.83%;
No. 14 peaks: relative retention time 3.412 accounts for area with reference to the peak than 13.89%.
Red sage root 38.4g santal 4.3g dalbergia wood 8.5g Kaempferia galanga 6.4g
Nutmeg 12.8g fructus choerospondiatis 12.8g sea-buckthorn 12.8g
More than seven flavors, santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 5 hours with 7.8 times of water gagings, the device collection in addition of the aqueous solution after the distillation; Three flavor medicinal materials such as the dregs of a decoction and all the other reds sage root each 1 hour, filter with 5 times of amount 95% alcohol reflux secondaries, collect filtrate, the dregs of a decoction decoct secondary, each 1.5 hours with 7 times of water gagings, filter, collect filtrate, concentrating each extract to relative density respectively is the thick paste of 1.30～1.40 (60 ℃), merge each thick paste, 80 ℃ of drying under reduced pressure are ground into fine powder, extract powder, add volatile oil and PEG400, Macrogol 4000 is an amount of, is cooling medium with the dimethyl silicon oil, make dripping pill, promptly.
Detection method:
Chromatographic condition and system suitability test: chromatographic column Inertsil ODS-3 150 * 4.6mm, 5 μ m; 35 ℃ of column temperatures; With the octadecylsilane chemically bonded silica is filling agent; With 1.0% formic acid solution is mobile phase A, and acetonitrile is a Mobile phase B, flow velocity 1.0ml/min; Carry out gradient elution by following program: since 0 minute to 45 minutes, mobile phase A became 20% by 85%, and since 45 minutes to 55 minutes, mobile phase A became 85% by 20%, and is maintained until 65 minutes, and gradient is linear gradient;
Prepare with reference to the peak: get tanshin polyphenolic acid B reference substance 0.01g, the accurate title, decide, and adds 75% methyl alcohol and make the solution that every 1ml contains 0.0001g, promptly;
The need testing solution preparation: get coronary disease seven flavor dripping pills, porphyrize is got about 0.3g, the accurate title, decide, and puts in the conical flask, the accurate 75% methyl alcohol 50ml that adds, claim to decide weight, power 280W, frequency 40kHz sonicated 15 minutes, put coldly, claim again to decide weight, supply with 75% methyl alcohol and subtract weight loss, shake up, filter, get subsequent filtrate, promptly;
Determination method: accurate respectively the absorption with reference to product solution and each 10 μ l of need testing solution, inject liquid chromatograph, UV-detector detects, and the mensuration wavelength is 280nm, the record chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press chromatographic fingerprints of Chinese materia medica similarity evaluation system-computed, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90.
Red sage root 21g santal 6g dalbergia wood 6g Kaempferia galanga 8g nutmeg 8g
Fructus choerospondiatis 18g sea-buckthorn 8g
More than seven flavors, santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 5 hours with 7.8 times of water gagings, the device collection in addition of the aqueous solution after the distillation; Three flavor medicinal materials such as the dregs of a decoction and all the other reds sage root each 1 hour, filter with 5 times of amount 95% alcohol reflux secondaries, collect filtrate, the dregs of a decoction decoct secondary, each 1.5 hours with 7 times of water gagings, filter, collect filtrate, concentrating each extract to relative density respectively is the thick paste of 1.30～1.40 (60 ℃), merge each thick paste, 80 ℃ of drying under reduced pressure are ground into fine powder, extract powder, add volatile oil and PEG400, Macrogol 4000 is an amount of, is cooling medium with the dimethyl silicon oil, make dripping pill, promptly.
Detection method:
Chromatographic condition and system suitability test: chromatographic column Inertsil ODS-3 150 * 4.6mm, 5 μ m; 30 ℃ of column temperatures; With the octadecylsilane chemically bonded silica is filling agent; With 2.0% formic acid solution is mobile phase A, and acetonitrile is a Mobile phase B, flow velocity 0.8ml/min; Carry out gradient elution by following program: since 0 minute to 45 minutes, mobile phase A became 20% by 85%, and since 45 minutes to 55 minutes, mobile phase A became 85% by 20%, and is maintained until 65 minutes, and gradient is linear gradient;
Prepare with reference to the peak: get tanshin polyphenolic acid B reference substance 0.008g, the accurate title, decide, and adds 80% methyl alcohol and make the solution that every 0.7ml contains 0.00013g, promptly;
The need testing solution preparation: get coronary disease seven flavor dripping pills, porphyrize is got 0.2g, the accurate title, decide, and puts in the conical flask, the accurate 70% methyl alcohol 30ml that adds, claim to decide weight, power 250W, frequency 30kHz sonicated 20 minutes, put coldly, claim again to decide weight, supply with 80% methyl alcohol and subtract weight loss, shake up, filter, get subsequent filtrate, promptly;
Determination method: accurate respectively the absorption with reference to product solution and each 7 μ l of need testing solution, inject liquid chromatograph, UV-detector detects, and the mensuration wavelength is 280nm, the record chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press chromatographic fingerprints of Chinese materia medica similarity evaluation system-computed, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90.
Red sage root 50g santal 3g dalbergia wood 11g Kaempferia galanga 4g nutmeg g
Fructus choerospondiatis 8g sea-buckthorn 18g
More than seven flavors, santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 5 hours with 7.8 times of water gagings, the device collection in addition of the aqueous solution after the distillation; Three flavor medicinal materials such as the dregs of a decoction and all the other reds sage root each 1 hour, filter with 5 times of amount 95% alcohol reflux secondaries, collect filtrate, the dregs of a decoction decoct secondary, each 1.5 hours with 7 times of water gagings, filter, collect filtrate, concentrating each extract to relative density respectively is the thick paste of 1.30～1.40 (60 ℃), merge each thick paste, 80 ℃ of drying under reduced pressure are ground into fine powder, extract powder, add volatile oil and PEG400, Macrogol 4000 is an amount of, is cooling medium with the dimethyl silicon oil, make dripping pill, promptly.
Detection method:
Chromatographic condition and system suitability test: chromatographic column Inertsil ODS-3 150 * 4.6mm, 5 μ m; 40 ℃ of column temperatures; With the octadecylsilane chemically bonded silica is filling agent; With 0.5% formic acid solution is mobile phase A, and acetonitrile is a Mobile phase B, flow velocity 1.2ml/min; Carry out gradient elution by following program: since 0 minute to 45 minutes, mobile phase A became 20% by 85%, and since 45 minutes to 55 minutes, mobile phase A became 85% by 20%, and is maintained until 65 minutes, and gradient is linear gradient;
Prepare with reference to the peak: get tanshin polyphenolic acid B reference substance 0.012g, the accurate title, decide, and adds 70% methyl alcohol and make the solution that every 1.3ml contains 0.00007g, promptly.
The need testing solution preparation: get coronary disease seven flavor dripping pills, porphyrize is got 0.4g, the accurate title, decide, and puts in the conical flask, the accurate 80% methyl alcohol 70ml that adds, claim to decide weight, power 320W, frequency 50kHz sonicated 10 minutes, put coldly, claim again to decide weight, supply with 70% methyl alcohol and subtract weight loss, shake up, filter, get subsequent filtrate, promptly;
Determination method: accurate respectively the absorption with reference to product solution and each 12 μ l of need testing solution, inject liquid chromatograph, UV-detector detects, and the mensuration wavelength is 280nm, the record chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press chromatographic fingerprints of Chinese materia medica similarity evaluation system-computed, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90.
Claims (13)
1. the detection method of coronary disease seven flavor dripping pill finger-prints is characterized in that this method comprises the steps:
Chromatographic condition and system suitability test: chromatographic column Inertsil ODS-3 150 * 4.6mm, 5 μ m; 25～45 ℃ of column temperatures; With the octadecylsilane chemically bonded silica is filling agent; With 0.1～3.0% formic acid solution is mobile phase A, and acetonitrile is a Mobile phase B, flow velocity 0.5～1.5ml/min; Carry out gradient elution by following program: since 0 minute to 45 minutes, mobile phase A became 20% by 85%, and since 45 minutes to 55 minutes, mobile phase A became 85% by 20%, and is maintained until 65 minutes, and gradient is linear gradient;
Reference product formulations prepared from solutions: get tanshin polyphenolic acid B reference substance 0.005-0.015 weight portion, the accurate title, decide, and adds 65～85% methyl alcohol and make the solution that every 0.5-1.5 parts by volume contains the 0.00005-0.00015 weight portion, promptly;
The need testing solution preparation: get coronary disease seven flavor dripping pills, porphyrize is got 0.2～0.4 weight portion, the accurate title, decide, and puts in the conical flask, accurate 65～85% methyl alcohol, 20～80 parts by volume that add, claim to decide weight, power 220～350W, frequency 20-60kHz sonicated 7～23 minutes, put coldly, claim again to decide weight, supply with 65～85% methyl alcohol and subtract weight loss, shake up, filter, get subsequent filtrate, promptly;
Determination method: accurate respectively the absorption with reference to product solution and each 5～15 μ l of need testing solution, inject liquid chromatograph, UV-detector detects, and the mensuration wavelength is 280nm, the record chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press chromatographic fingerprints of Chinese materia medica similarity evaluation system-computed, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90.
2. the detection method of coronary disease seven flavor dripping pill finger-prints as claimed in claim 1 is characterized in that this method comprises the steps:
Chromatographic condition and system suitability test: chromatographic column Inertsil ODS-3 150 * 4.6mm, 5 μ m; 35 ℃ of column temperatures; With the octadecylsilane chemically bonded silica is filling agent; With 1.0% formic acid solution is mobile phase A, and acetonitrile is a Mobile phase B, flow velocity 1.0ml/min; Carry out gradient elution by following program: since 0 minute to 45 minutes, mobile phase A became 20% by 85%, and since 45 minutes to 55 minutes, mobile phase A became 85% by 20%, and is maintained until 65 minutes, and gradient is linear gradient;
Reference product formulations prepared from solutions: get tanshin polyphenolic acid B reference substance 0.01 weight portion, the accurate title, decide, and adds 75% methyl alcohol and make the solution that per 1 parts by volume contains 0.0001 weight portion, promptly;
The need testing solution preparation: get coronary disease seven flavor dripping pills, porphyrize is got 0.3 weight portion, the accurate title, decide, and puts in the conical flask, accurate 75% methyl alcohol, 50 parts by volume that add, claim to decide weight, power 280W, frequency 40kHz sonicated 15 minutes, put coldly, claim again to decide weight, supply with 75% methyl alcohol and subtract weight loss, shake up, filter, get subsequent filtrate, promptly;
Determination method: accurate respectively the absorption with reference to product solution and each 10 μ l of need testing solution, inject liquid chromatograph, UV-detector detects, and the mensuration wavelength is 280nm, the record chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press chromatographic fingerprints of Chinese materia medica similarity evaluation system-computed, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90.
3. the detection method of coronary disease seven flavor dripping pill finger-prints as claimed in claim 1 or 2 is characterized in that 14 corresponding characteristic peaks are in the described coronary disease seven flavor dripping pill finger-prints:
No. 1 peak: relative retention time 0.170-0.208, the area that accounts for reference to the peak compares 1.48%-28.03%;
No. 2 peak: relative retention time 0.199-0.243, the area that accounts for reference to the peak compares 1.33%-25.29%;
No. 3 peak: relative retention time 0.332-0.406, the area that accounts for reference to the peak compares 0.40%-7.63%;
No. 4 peak: relative retention time 0.772-0.943, the area that accounts for reference to the peak compares 1.26%-23.94%;
No. 5 peak: relative retention time 0.811-0.991, the area that accounts for reference to the peak compares 1.18%-22.46%;
No. 6 peaks: be the reference peak;
No. 7 peak: relative retention time 0.965-1.180, the area that accounts for reference to the peak compares 18.69%-43.61%;
No. 8 peak: relative retention time 1.544-1.887, the area that accounts for reference to the peak compares 1.33%-25.22%;
No. 9 peak: relative retention time 1.614-1.973, the area that accounts for reference to the peak compares 33.20%-68.96%;
No. 10 peak: relative retention time 1.802-2.203, the area that accounts for reference to the peak compares 1.22%-23.21%;
No. 11 peak: relative retention time 2.087-2.550, the area that accounts for reference to the peak compares 20.10%-46.90%;
No. 12 peak: relative retention time 2.493-3.047, the area that accounts for reference to the peak compares 0.50%-9.48%;
No. 13 peak: relative retention time 2.540-3.104, the area that accounts for reference to the peak compares 1.50%-28.44%;
No. 14 peak: relative retention time 2.958-3.616, the area that accounts for reference to the peak compares 13.56%-31.64%.
4. the detection method of coronary disease seven flavor dripping pill finger-prints as claimed in claim 3 is characterized in that 14 corresponding characteristic peaks are in the described coronary disease seven flavor dripping pill finger-prints:
No. 1 peak: relative retention time 0.170-0.208, the area that accounts for reference to the peak compares 8.48%-20.03%;
No. 2 peak: relative retention time 0.199-0.243, the area that accounts for reference to the peak compares 7.33%-20.29%;
No. 3 peak: relative retention time 0.332-0.406, the area that accounts for reference to the peak compares 2.40%-5.63%;
No. 4 peak: relative retention time 0.772-0.943, the area that accounts for reference to the peak compares 8.26%-19.94%;
No. 5 peak: relative retention time 0.811-0.991, the area that accounts for reference to the peak compares 8.18%-18.46%;
No. 6 peaks: be the reference peak;
No. 7 peak: relative retention time 0.965-1.180, the area that accounts for reference to the peak compares 25.69%-35.61%;
No. 8 peak: relative retention time 1.544-1.887, the area that accounts for reference to the peak compares 8.33%-20.22%;
No. 9 peak: relative retention time 1.614-1.973, the area that accounts for reference to the peak compares 45.20%-60.96%;
No. 10 peak: relative retention time 1.802-2.203, the area that accounts for reference to the peak compares 8.22%-18.21%;
No. 11 peak: relative retention time 2.087-2.550, the area that accounts for reference to the peak compares 30.10%-40.90%;
No. 12 peak: relative retention time 2.493-3.047, the area that accounts for reference to the peak compares 3.50%-6.48%;
No. 13 peak: relative retention time 2.540-3.104, the area that accounts for reference to the peak compares 10.50%-20.44%;
No. 14 peak: relative retention time 2.958-3.616, the area that accounts for reference to the peak compares 18.56%-28.64%.
5. the detection method of coronary disease seven flavor dripping pill finger-prints as claimed in claim 3 is characterized in that 14 corresponding characteristic peaks are in the described coronary disease seven flavor dripping pill finger-prints:
No. 1 peak: relative retention time 0.189 accounts for area with reference to the peak than 14.75%;
No. 2 peaks: relative retention time 0.221 accounts for area with reference to the peak than 13.31%;
No. 3 peaks: relative retention time 0.369 accounts for area with reference to the peak than 4.02%;
No. 4 peaks: relative retention time 0.857 accounts for area with reference to the peak than 12.60%;
No. 5 peaks: relative retention time 0.901 accounts for area with reference to the peak than 11.82%;
No. 6 peaks: be the reference peak;
No. 7 peaks: relative retention time 1.073 accounts for area with reference to the peak than 31.15%;
No. 8 peaks: relative retention time 1.716 accounts for area with reference to the peak than 13.27%;
No. 9 peaks: relative retention time 1.793 accounts for area with reference to the peak than 51.08%;
No. 10 peaks: relative retention time 2.002 accounts for area with reference to the peak than 12.22%;
No. 11 peaks: relative retention time 2.318 accounts for area with reference to the peak than 33.50%;
No. 12 peaks: relative retention time 2.770 accounts for area with reference to the peak than 4.99%;
No. 13 peaks: relative retention time 2.822 accounts for area with reference to the peak than 14.97%;
No. 14 peaks: relative retention time 3.287 accounts for area with reference to the peak than 22.60%.
6. as the detection method of claim 1,2,4 or 5 described coronary disease seven flavor dripping pill finger-prints, it is characterized in that the bulk drug of described coronary disease seven flavor dripping pills consists of:
Red sage root 19.2-57.6 weight portion santal 2.1-6.5 weight portion dalbergia wood 4.2-12.8 weight portion
Kaempferia galanga 3.2-9.6 weight portion nutmeg 6.4-19.2 weight portion fructus choerospondiatis 6.4-19.2 weight portion
Sea-buckthorn 6.4-19.2 weight portion.
7. the detection method of coronary disease seven flavor dripping pill finger-prints as claimed in claim 3 is characterized in that the bulk drug of described coronary disease seven flavor dripping pills consists of:
Red sage root 19.2-57.6 weight portion santal 2.1-6.5 weight portion dalbergia wood 4.2-12.8 weight portion
Kaempferia galanga 3.2-9.6 weight portion nutmeg 6.4-19.2 weight portion fructus choerospondiatis 6.4-19.2 weight portion
Sea-buckthorn 6.4-19.2 weight portion.
8. the detection method of coronary disease seven flavor dripping pill finger-prints as claimed in claim 6 is characterized in that the bulk drug of described coronary disease seven flavor dripping pills consists of:
The red sage root 38.4 weight portion santals 4.3 weight portion dalbergia woods 8.5 weight portions
Kaempferia galanga 6.4 weight portion nutmegs 12.8 weight portion fructus choerospondiatis 12.8 weight portions
Sea-buckthorn 12.8 weight portions;
Or the red sage root 21 weight portion santals 6 weight portion dalbergia woods 6 weight portions
Kaempferia galanga 8 weight portion nutmegs 8 weight portion fructus choerospondiatis 18 weight portions
Sea-buckthorn 8 weight portions;
Or the red sage root 50 weight portion santals 3 weight portion dalbergia woods 11 weight portions
Kaempferia galanga 4 weight portion nutmegs 18 weight portion fructus choerospondiatis 8 weight portions
Sea-buckthorn 18 weight portions.
9. the detection method of coronary disease seven flavor dripping pill finger-prints as claimed in claim 7 is characterized in that the bulk drug of described coronary disease seven flavor dripping pills consists of:
The red sage root 38.4 weight portion santals 4.3 weight portion dalbergia woods 8.5 weight portions
Kaempferia galanga 6.4 weight portion nutmegs 12.8 weight portion fructus choerospondiatis 12.8 weight portions
Sea-buckthorn 12.8 weight portions;
Or the red sage root 21 weight portion santals 6 weight portion dalbergia woods 6 weight portions
Kaempferia galanga 8 weight portion nutmegs 8 weight portion fructus choerospondiatis 18 weight portions
Sea-buckthorn 8 weight portions;
Or the red sage root 50 weight portion santals 3 weight portion dalbergia woods 11 weight portions
Kaempferia galanga 4 weight portion nutmegs 18 weight portion fructus choerospondiatis 8 weight portions
Sea-buckthorn 18 weight portions.
10. the detection method of coronary disease seven flavor dripping pill finger-prints as claimed in claim 6 is characterized in that the preparation method of described coronary disease seven flavor dripping pills is:
Santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 2-8 hour with 5-10 times of water gaging, and the aqueous solution after distillation device is in addition collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor medicinal materials are doubly measured the 75-95% alcohol reflux 1-3 time with 2-8, each 0.5-1.5 hour, filter, collect filtrate, the dregs of a decoction decoct 1-3 time with 4-10 times of water gaging, each 1-2 hour, filter, collect filtrate, relative density is 1.30～1.40 thick paste when concentrating each extract to 60 ℃ respectively, merge above-mentioned aqueous solution and filtrate, 80 ℃ of drying under reduced pressure are ground into fine powder, get extract powder, add volatile oil, the PEG400 of 2-10 weight portion, the Macrogol 4000 of 20-28 weight portion is a cooling medium with the dimethyl silicon oil, makes dripping pill.
11., it is characterized in that the preparation method of described coronary disease seven flavor dripping pills is as the detection method of the described coronary disease seven flavor dripping pill finger-prints of one of claim 7-9:
Santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 2-8 hour with 5-10 times of water gaging, and the aqueous solution after distillation device is in addition collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor medicinal materials are doubly measured the 75-95% alcohol reflux 1-3 time with 2-8, each 0.5-1.5 hour, filter, collect filtrate, the dregs of a decoction decoct 1-3 time with 4-10 times of water gaging, each 1-2 hour, filter, collect filtrate, relative density is 1.30～1.40 thick paste when concentrating each extract to 60 ℃ respectively, merge above-mentioned aqueous solution and filtrate, 80 ℃ of drying under reduced pressure are ground into fine powder, get extract powder, add volatile oil, the PEG400 of 2-10 weight portion, the Macrogol 4000 of 20-28 weight portion is a cooling medium with the dimethyl silicon oil, makes dripping pill.
12. the detection method of coronary disease seven flavor dripping pill finger-prints as claimed in claim 10 is characterized in that the preparation method of described coronary disease seven flavor dripping pills is:
Santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 5 hours with 7.8 times of water gagings, and the aqueous solution after distillation device is in addition collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor medicinal materials are measured 95% alcohol reflux secondaries with 5 times, each 1 hour, filter, collect filtrate, the dregs of a decoction decoct secondary with 7 times of water gagings, each 1.5 hours, filter, collect filtrate, relative density is 1.30～1.40 thick paste when concentrating each extract to 60 ℃ respectively, merge each thick paste, 80 ℃ of drying under reduced pressure are ground into fine powder, get extract powder, adding volatile oil, the PEG400 of 5 weight portions, the Macrogol 4000 of 25 weight portions, is cooling medium with the dimethyl silicon oil, makes dripping pill.
13. the detection method of coronary disease seven flavor dripping pill finger-prints as claimed in claim 11 is characterized in that the preparation method of described coronary disease seven flavor dripping pills is:
Santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 5 hours with 7.8 times of water gagings, and the aqueous solution after distillation device is in addition collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor medicinal materials are measured 95% alcohol reflux secondaries with 5 times, each 1 hour, filter, collect filtrate, the dregs of a decoction decoct secondary with 7 times of water gagings, each 1.5 hours, filter, collect filtrate, relative density is 1.30～1.40 thick paste when concentrating each extract to 60 ℃ respectively, merge each thick paste, 80 ℃ of drying under reduced pressure are ground into fine powder, get extract powder, adding volatile oil, the PEG400 of 5 weight portions, the Macrogol 4000 of 25 weight portions, is cooling medium with the dimethyl silicon oil, makes dripping pill.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104777253A (en) * | 2015-04-17 | 2015-07-15 | 国药控股深圳中药有限公司 | Establishment method for Guanxindanshen capsule fingerprint spectrum and fingerprint spectrum thereof |
| WO2018090380A1 (en) * | 2016-11-21 | 2018-05-24 | 内蒙古天奇中蒙制药股份有限公司 | Capsule and preparation process therefor |
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| CN104777253A (en) * | 2015-04-17 | 2015-07-15 | 国药控股深圳中药有限公司 | Establishment method for Guanxindanshen capsule fingerprint spectrum and fingerprint spectrum thereof |
| WO2018090380A1 (en) * | 2016-11-21 | 2018-05-24 | 内蒙古天奇中蒙制药股份有限公司 | Capsule and preparation process therefor |
| CN109298091A (en) * | 2018-10-24 | 2019-02-01 | 安徽安科余良卿药业有限公司 | The standard feature map construction method and its quality determining method of wind eggplant Pingchuan ointment |
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| Publication number | Publication date |
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| CN102297923B (en) | 2014-02-19 |
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