CN102297923B - Method for fingerprint detection of Guanxinqiwei dripping pills - Google Patents
Method for fingerprint detection of Guanxinqiwei dripping pills Download PDFInfo
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- CN102297923B CN102297923B CN201110132727.1A CN201110132727A CN102297923B CN 102297923 B CN102297923 B CN 102297923B CN 201110132727 A CN201110132727 A CN 201110132727A CN 102297923 B CN102297923 B CN 102297923B
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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 taste dripping pill finger-prints.
Background technology
Coronary disease seven taste dripping pills be applicant on the basis of coronary disease tablet of seven ingredients, the novel form that uses present Chinese medicine preparation technology to make, however coronary disease tablet of seven ingredients only has the coherence check of proterties and tablet aspect quality control, substantially can not control the inherent quality of product.
Coronary disease seven taste dripping pills of the present invention have increased the quality control of the 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 belongs to pioneering for the quality control of coronary disease seven taste dripping pills.
Summary of the invention
The object of the invention is to provide a kind of detection method of coronary disease seven taste dripping pill finger-prints.
The present invention is achieved through the following technical solutions:
A detection method for coronary disease seven taste dripping pill finger-prints, the method comprises the steps:
Chromatographic condition and system suitability: chromatographic column Inertsil ODS-3150 * 4.6mm, 5 μ m; 25～45 ℃ of column temperatures; Take octadecylsilane chemically bonded silica as filling agent; Take 0.1～3.0% formic acid solution as mobile phase A, and acetonitrile is Mobile phase B, flow velocity 0.5～1.5ml/min; By following program, carry out gradient elution: since 0 minute to 45 minutes, mobile phase A became 20% from 85%, since 45 minutes to 55 minutes, mobile phase A became 85% from 20%, and is maintained until 65 minutes, and gradient is linear gradient;
With reference to peak, prepare: get tanshin polyphenolic acid B reference substance 0.005-0.015 weight portion, accurately weighed, add 65～85% methyl alcohol and make every 0.5-1.5 parts by volume containing the solution of 0.0001-0.0003 weight portion, obtain;
Need testing solution preparation: get coronary disease seven taste dripping pills, porphyrize, gets 0.2～0.4 weight portion, accurately weighed, to put in conical flask, precision adds 65～85% methyl alcohol 20～80 parts by volume, weighed weight, power 220～350W, the ultrasonic processing of frequency 20-60kHz 7～23 minutes, let cool, more weighed weight, with 65～85% methyl alcohol, supply less loss weight, shake up, filter, get subsequent filtrate, obtain;
Determination method: precision is drawn with reference to product solution and each 5～15 μ l of need testing solution respectively, injection liquid chromatography, UV-detector detects, and mensuration wavelength is 280nm, records chromatogram;
Test sample finger-print and reference fingerprint are compared, in test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press similarity evaluation and calculate, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90.
The detection method of coronary disease seven taste dripping pill finger-prints of the present invention comprises the steps:
Chromatographic condition and system suitability: chromatographic column Inertsil ODS-3150 * 4.6mm, 5 μ m; 35 ℃ of column temperatures; Take octadecylsilane chemically bonded silica as filling agent; Take 1.0% formic acid solution as mobile phase A, and acetonitrile is Mobile phase B, flow velocity 1.0ml/min; By following program, carry out gradient elution: since 0 minute to 45 minutes, mobile phase A became 20% from 85%, since 45 minutes to 55 minutes, mobile phase A became 85% from 20%, and is maintained until 65 minutes, and gradient is linear gradient;
With reference to product solution, prepare: get tanshin polyphenolic acid B reference substance 0.01 weight portion, accurately weighed, add 75% methyl alcohol and make every 1 parts by volume containing the solution of 0.001 weight portion, obtain;
Need testing solution preparation: get coronary disease seven taste dripping pills, porphyrize, gets 0.3 weight portion, accurately weighed, to put in conical flask, precision adds 75% methyl alcohol 50 parts by volume, weighed weight, power 280W, the ultrasonic processing of frequency 40kHz 15 minutes, let cool, more weighed weight, with 75% methyl alcohol, supply less loss weight, shake up, filter, get subsequent filtrate, obtain;
Determination method: precision is drawn with reference to product solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, UV-detector detects, and mensuration wavelength is 280nm, records chromatogram;
Test sample finger-print and reference fingerprint are compared, in test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press similarity evaluation and calculate, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90.
14 characteristic peaks corresponding in coronary disease seven taste dripping pill finger-prints of the present invention are:
No. 1 peak: relative retention time 0.170-0.208, accounts for the Area Ratio 1.48%-28.03% with reference to peak;
No. 2 peak: relative retention time 0.199-0.243, account for the Area Ratio 1.33%-25.29% with reference to peak;
No. 3 peak: relative retention time 0.332-0.406, account for the Area Ratio 0.40%-7.63% with reference to peak;
No. 4 peak: relative retention time 0.772-0.943, account for the Area Ratio 1.26%-23.94% with reference to peak;
No. 5 peak: relative retention time 0.811-0.991, account for the Area Ratio 1.18%-22.46% with reference to peak;
No. 6 peaks: for reference to peak;
No. 7 peak: relative retention time 0.965-1.180, account for the Area Ratio 18.69%-43.61% with reference to peak;
No. 8 peak: relative retention time 1.544-1.887, account for the Area Ratio 1.33%-25.22% with reference to peak;
No. 9 peak: relative retention time 1.614-1.973, account for the Area Ratio 33.20%-68.96% with reference to peak;
No. 10 peak: relative retention time 1.802-2.203, account for the Area Ratio 1.22%-23.21% with reference to peak;
No. 11 peak: relative retention time 2.087-2.550, account for the Area Ratio 20.10%-46.90% with reference to peak;
No. 12 peak: relative retention time 2.493-3.047, account for the Area Ratio 0.50%-9.48% with reference to peak;
No. 13 peak: relative retention time 2.540-3.104, account for the Area Ratio 1.50%-28.44% with reference to peak; 14
Number peak: relative retention time 2.958-3.616, accounts for the Area Ratio 13.56%-31.64% with reference to peak.
14 characteristic peaks corresponding in coronary disease seven taste dripping pill finger-prints of the present invention are:
No. 1 peak: relative retention time 0.170-0.208, accounts for the Area Ratio 8.48%-20.03% with reference to peak;
No. 2 peak: relative retention time 0.199-0.243, account for the Area Ratio 7.33%-20.29% with reference to peak;
No. 3 peak: relative retention time 0.332-0.406, account for the Area Ratio 2.40%-5.63% with reference to peak;
No. 4 peak: relative retention time 0.772-0.943, account for the Area Ratio 8.26%-19.94% with reference to peak;
No. 5 peak: relative retention time 0.811-0.991, account for the Area Ratio 8.18%-18.46% with reference to peak;
No. 6 peaks: for reference to peak;
No. 7 peak: relative retention time 0.965-1.180, account for the Area Ratio 25.69%-35.61% with reference to peak;
No. 8 peak: relative retention time 1.544-1.887, account for the Area Ratio 8.33%-20.22% with reference to peak;
No. 9 peak: relative retention time 1.614-1.973, account for the Area Ratio 45.20%-60.96% with reference to peak;
No. 10 peak: relative retention time 1.802-2.203, account for the Area Ratio 8.22%-18.21% with reference to peak;
No. 11 peak: relative retention time 2.087-2.550, account for the Area Ratio 30.10%-40.90% with reference to peak;
No. 12 peak: relative retention time 2.493-3.047, account for the Area Ratio 3.50%-6.48% with reference to peak;
No. 13 peak: relative retention time 2.540-3.104, account for the Area Ratio 10.50%-20.44% with reference to peak;
No. 14 peak: relative retention time 2.958-3.616, account for the Area Ratio 18.56%-28.64% with reference to peak.
14 characteristic peaks corresponding in coronary disease seven taste dripping pill finger-prints of the present invention are:
No. 1 peak: relative retention time 0.189, accounts for the Area Ratio 14.75% with reference to peak;
No. 2 peaks: relative retention time 0.221, accounts for the Area Ratio 13.31% with reference to peak;
No. 3 peaks: relative retention time 0.369, accounts for the Area Ratio 4.02% with reference to peak;
No. 4 peaks: relative retention time 0.857, accounts for the Area Ratio 12.60% with reference to peak;
No. 5 peaks: relative retention time 0.901, accounts for the Area Ratio 11.82% with reference to peak;
No. 6 peaks: for reference to peak;
No. 7 peaks: relative retention time 1.073, accounts for the Area Ratio 31.15% with reference to peak;
No. 8 peaks: relative retention time 1.716, accounts for the Area Ratio 13.27% with reference to peak;
No. 9 peaks: relative retention time 1.793, accounts for the Area Ratio 51.08% with reference to peak;
No. 10 peaks: relative retention time 2.002, accounts for the Area Ratio 12.22% with reference to peak;
No. 11 peaks: relative retention time 2.318, accounts for the Area Ratio 33.50% with reference to peak;
No. 12 peaks: relative retention time 2.770, accounts for the Area Ratio 4.99% with reference to peak;
No. 13 peaks: relative retention time 2.822, accounts for the Area Ratio 14.97% with reference to peak;
No. 14 peaks: relative retention time 3.287, accounts for the Area Ratio 22.60% with reference to peak.
Coronary disease seven taste dripping pills of the present invention are made by the following method:
The bulk drug of coronary disease seven taste 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 taste dripping pills of the present invention is preferably:
The red sage root 38.4 weight portion santal 4.3 weight portion dalbergia wood 8.5 weight portions
Kaempferia galanga 6.4 weight portion nutmeg 12.8 weight portion fructus choerospondiatis 12.8 weight portions
Sea-buckthorn 12.8 weight portions;
Or the red sage root 21 weight portion santal 6 weight portion dalbergia wood 6 weight portions
Sea-buckthorn 8 weight portions;
Or the red sage root 50 weight portion santal 3 weight portion dalbergia wood 11 weight portions
Sea-buckthorn 18 weight portions.
The preparation method of coronary disease seven taste dripping pills of the present invention is:
Above seven tastes, extract volatile oil 2-8 hour by Tan Xiang ﹑ Jiang Xiang ﹑ Shan Nai ﹑ nutmeg with 5-10 times of water gaging, and the another device of aqueous solution after distillation is collected, the dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three taste medicinal materials are doubly measured 75-95% alcohol reflux with 2-8 and are extracted 1-3 time, 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, the thick paste that relative density is 1.30～1.40 during concentrated each extract to 60 ℃ respectively, merge above-mentioned aqueous solution and filtrate, 80 ℃ of drying under reduced pressure, be ground into fine powder, obtain extract powder, add volatile oil, the PEG400 of 2-10 weight portion, the Macrogol 4000 of 20-28 weight portion, take dimethyl silicon oil as cooling medium, make dripping pill.
The preparation method of coronary disease seven taste dripping pills of the present invention is preferably:
Above seven tastes, extract volatile oil 5 hours by Tan Xiang ﹑ Jiang Xiang ﹑ Shan Nai ﹑ nutmeg with 7.8 times of water gagings, and the another device of aqueous solution after distillation is collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three taste medicinal materials extract secondary with 5 times of amount 95% alcohol refluxs, 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, the thick paste that relative density is 1.30 ~ 1.40 during concentrated each extract to 60 ℃ respectively, merge each thick paste, 80 ℃ of drying under reduced pressure, are ground into fine powder, obtain extract powder, add the PEG400 of volatile oil, 5 weight portions, the Macrogol 4000 of 25 weight portions, take dimethyl silicon oil as cooling medium, make 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 taste dripping pills of the present invention is: (1) specificity is strong, and this finger-print is that coronary disease seven taste dripping pills are exclusive, and the chemical information of its reflection is to have height optionally.(2) good stability, this finger-print is the general character of summarizing from many batches of coronary diseases seven taste dripping pills, the characteristic peak in collection of illustrative plates is stable.(3) favorable reproducibility, this finger print measuring method can reproduce the fingerprint characteristic of coronary disease seven taste dripping pills under regulation condition determination.Quality and the curative effect of controlling coronary disease seven taste dripping pills are significant.
Accompanying drawing explanation
Fig. 1 is reference fingerprint;
Fig. 2 is with reference to product collection of illustrative plates;
Fig. 3 is 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 for further illustrating the present invention, but is not limited to the present invention.
Experimental example one: chromatographic system screening experiment
1, the selection of mobile phase selects three kinds of mobile phases to test.
The first mobile phase: take 1.0% formic acid solution as mobile phase A, acetonitrile is Mobile phase B, flow velocity 0.8ml/min; By following program, carry out gradient elution: since 0 minute to 50 minutes, mobile phase A became 10% from 90%, since 50 minutes to 65 minutes, mobile phase A became 90% from 10%, and is maintained until 75 minutes, and gradient is linear gradient.
The second mobile phase: take water as mobile phase A, acetonitrile is Mobile phase B, flow velocity 1.0ml/min; By following program, carry out gradient elution: since 0 minute to 45 minutes, mobile phase A became 20% from 85%, since 45 minutes to 55 minutes, mobile phase A became 85% from 20%, and is maintained until 65 minutes, and gradient is linear gradient.
The third mobile phase: take 1.0% formic acid solution as mobile phase A, acetonitrile is Mobile phase B, flow velocity 1.0ml/min; By following program, carry out gradient elution: since 0 minute to 45 minutes, mobile phase A became 20% from 85%, since 45 minutes to 55 minutes, mobile phase A became 85% from 20%, and is maintained until 65 minutes, and gradient is linear gradient.
Test findings: finger-print peak type and the degree of separation of the third mobile phase gained are all best, and acquisition time is also less, so select the third mobile phase.
2, the selection of chromatographic column selects four kinds of chromatographic columns to test.
The first chromatographic column: Alltech C18250 * 4.6mm, 5 μ m.
The second chromatographic column: Waters C18250 * 4.6mm, 5 μ m.
The third chromatographic column: Yi Lite C18250 * 4.6mm, 5 μ m.
The 4th kind of chromatographic column: Inertsil ODS-3150 * 4.6mm, 5 μ m
Test findings: except the finger-print peak type of the third chromatographic column gained and degree of separation poor, its excess-three kind chromatographic column is all better, and finger-print peak type and the degree of separation of the 4th kind of chromatographic column gained are best, so final, determine and use the 4th kind of chromatographic column (Inertsil ODS-3150 * 4.6mm, 5 μ m).
Experimental example two, coronary disease of the present invention seven taste dripping pill detection method experiments
1, coronary disease seven taste dripping pill finger-print test methods of the present invention
(1) chromatographic condition
Chromatographic column: Inertsil ODS-3150 * 4.6mm, 5 μ m
Column temperature: 35 ℃
Mobile phase: A, 1% formic acid solution
B, acetonitrile
By following program, carry out gradient elution:
Flow velocity: 1.0ml/min
| Time | A | B |
| 0 | 85 | 15 |
| 45 | 20 | 80 |
| 55 | 85 | 15 |
| 65 | 85 | 15 |
(2), with reference to peak, prepare
Get tanshin polyphenolic acid B reference substance appropriate, accurately weighed, add 75% methyl alcohol and make every 1ml containing the solution of 0.1mg, obtain.
(3), need testing solution preparation
Get coronary disease seven taste dripping pills, porphyrize, gets about 0.3g, accurately weighed, to put in conical flask, precision adds 75% methyl alcohol 50ml, weighed weight, ultrasonic processing (power 280W, frequency 40kHz) 15 minutes, let cool, more weighed weight, with 75% methyl alcohol, supply less loss weight, shake up, filter, get subsequent filtrate, obtain.
(4), determination method accurate absorption with reference to product solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, UV-detector detects, mensuration wavelength is 280nm, records chromatogram.
Test sample finger-print and reference fingerprint are compared, in test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press similarity evaluation and calculate, 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.Look
Spectrum post is Inertsil ODS-3(150mm * 4.6mm, 5um); 35 ℃ of column temperatures.Slope: 50; Peak width: 30.
3, the explanation to finger-print
Coronary disease seven taste dripping pills are formed by seven taste Chinese drug preparations, and wherein three taste 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 fructus choerospondiatis (No. 1 peak); Volatile ingredient in nutmeg: Dehydrodiisoeugenol (No. 11 peaks) all embodies in finger-print.So this method is significant to the quality control of coronary disease seven taste dripping pills.
4, sample determining fingerprint pattern
(1) chromatographic condition
Chromatographic column: Inertsil ODS-3150 * 4.6mm, 5 μ m
Column temperature: 35 ℃
Mobile phase: A, 1% formic acid solution
C, acetonitrile
By following program, carry out gradient elution:
Flow velocity: 1.0ml/min
| Time | A | B |
| 0 | 85 | 15 |
| 45 | 20 | 80 |
| 55 | 85 | 15 |
| 65 | 85 | 15 |
(2), with reference to peak, prepare
Get tanshin polyphenolic acid B reference substance appropriate, accurately weighed, add 75% methyl alcohol and make every 1ml containing the solution of 0.1mg, obtain.
(3), need testing solution preparation
(4), determination method accurate absorption with reference to product solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, UV-detector detects, mensuration wavelength is 280nm, records chromatogram.
Discussion of results: the finger-print of comparative sample 1～11, find: 1., all have 14 of total chromatographic peaks 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 reference fingerprint.
The finger-print of other samples and reference fingerprint are compared, in test sample chromatogram, all there are 14 and reference fingerprint characteristic of correspondence peak, press similarity evaluation and calculate, 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 |
| Sample 6 | 14 | 9.93 |
| |
14 | 9.95 |
| |
14 | 9.87 |
| Sample 9 | 14 | 9.91 |
| |
14 | 9.90 |
| |
14 | 9.89 |
Fig. 2-Figure 12 is shown in by finger-print.
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
Above seven tastes, Tan Xiang ﹑ falls fragrant ﹑ mountain a kind of apple ﹑ nutmeg and extracts volatile oil 5 hours with 7.8 times of water gagings, and the another device of aqueous solution after distillation is collected; The three taste medicinal materials such as the dregs of a decoction and all the other reds sage root extract secondary with 5 times of amount 95% alcohol refluxs, each 1 hour, filter, collect filtrate, the dregs of a decoction decoct secondary, each 1.5 hours with 7 times of water gagings, filter, collect filtrate, concentrated each extract to relative density is 1.30～1.40(60 ℃ respectively) thick paste, merge each thick paste, 80 ℃ of drying under reduced pressure, are ground into fine powder, extract powder, add volatile oil and PEG400, Macrogol 4000 appropriate, take dimethyl silicon oil as cooling medium, make dripping pill, obtain.
Detection method:
Chromatographic condition and system suitability: chromatographic column Inertsil ODS-3150 * 4.6mm, 5 μ m; 35 ℃ of column temperatures; Take octadecylsilane chemically bonded silica as filling agent; Take 1.0% formic acid solution as mobile phase A, and acetonitrile is Mobile phase B, flow velocity 1.0ml/min; By following program, carry out gradient elution: since 0 minute to 45 minutes, mobile phase A became 20% from 85%, since 45 minutes to 55 minutes, mobile phase A became 85% from 20%, and is maintained until 65 minutes, and gradient is linear gradient;
With reference to peak, prepare: get tanshin polyphenolic acid B reference substance 0.01g, accurately weighed, add 75% methyl alcohol and make every 1ml containing the solution of 0.0001g, obtain;
Need testing solution preparation: get coronary disease seven taste dripping pills, porphyrize, gets about 0.3g, accurately weighed, to put in conical flask, precision adds 75% methyl alcohol 50ml, weighed weight, power 280W, the ultrasonic processing of frequency 40kHz 15 minutes, let cool, more weighed weight, with 75% methyl alcohol, supply less loss weight, shake up, filter, get subsequent filtrate, obtain;
Determination method: precision is drawn with reference to product solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, UV-detector detects, and mensuration wavelength is 280nm, records chromatogram;
Test sample finger-print and reference fingerprint are compared, in test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press similarity evaluation and calculate, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90;
14 characteristic peaks corresponding in described coronary disease seven taste dripping pill finger-prints are:
No. 1 peak: relative retention time 0.189, accounts for the Area Ratio 14.75% with reference to peak;
No. 2 peaks: relative retention time 0.221, accounts for the Area Ratio 13.31% with reference to peak;
No. 3 peaks: relative retention time 0.369, accounts for the Area Ratio 4.02% with reference to peak;
No. 4 peaks: relative retention time 0.857, accounts for the Area Ratio 12.60% with reference to peak;
No. 5 peaks: relative retention time 0.901, accounts for the Area Ratio 11.82% with reference to peak;
No. 6 peaks: for reference to peak;
No. 7 peaks: relative retention time 1.073, accounts for the Area Ratio 31.15% with reference to peak;
No. 8 peaks: relative retention time 1.716, accounts for the Area Ratio 13.27% with reference to peak;
No. 9 peaks: relative retention time 1.793, accounts for the Area Ratio 51.08% with reference to peak;
No. 10 peaks: relative retention time 2.002, accounts for the Area Ratio 12.22% with reference to peak;
No. 11 peaks: relative retention time 2.318, accounts for the Area Ratio 33.50% with reference to peak;
No. 12 peaks: relative retention time 2.770, accounts for the Area Ratio 4.99% with reference to peak;
No. 13 peaks: relative retention time 2.822, accounts for the Area Ratio 14.97% with reference to peak;
No. 14 peaks: relative retention time 3.287, accounts for the Area Ratio 22.60% with reference to peak.
Red sage root 21g santal 6g dalbergia wood 6g Kaempferia galanga 8g nutmeg 8g
Fructus choerospondiatis 18g sea-buckthorn 8g
Above seven tastes, Tan Xiang ﹑ falls fragrant ﹑ mountain a kind of apple ﹑ nutmeg and extracts volatile oil 5 hours with 7.8 times of water gagings, and the another device of aqueous solution after distillation is collected; The three taste medicinal materials such as the dregs of a decoction and all the other reds sage root extract secondary with 5 times of amount 95% alcohol refluxs, each 1 hour, filter, collect filtrate, the dregs of a decoction decoct secondary, each 1.5 hours with 7 times of water gagings, filter, collect filtrate, concentrated each extract to relative density is 1.30～1.40(60 ℃ respectively) thick paste, merge each thick paste, 80 ℃ of drying under reduced pressure, are ground into fine powder, extract powder, add volatile oil and PEG400, Macrogol 4000 appropriate, take dimethyl silicon oil as cooling medium, make dripping pill, obtain.
Detection method:
Chromatographic condition and system suitability: chromatographic column Inertsil ODS-3150 * 4.6mm, 5 μ m; 30 ℃ of column temperatures; Take octadecylsilane chemically bonded silica as filling agent; Take 2.0% formic acid solution as mobile phase A, and acetonitrile is Mobile phase B, flow velocity 0.8ml/min; By following program, carry out gradient elution: since 0 minute to 45 minutes, mobile phase A became 20% from 85%, since 45 minutes to 55 minutes, mobile phase A became 85% from 20%, and is maintained until 65 minutes, and gradient is linear gradient;
With reference to peak, prepare: get tanshin polyphenolic acid B reference substance 0.008g, accurately weighed, add 80% methyl alcohol and make every 0.7ml containing the solution of 0.00013g, obtain;
Need testing solution preparation: get coronary disease seven taste dripping pills, porphyrize, gets 0.2g, accurately weighed, to put in conical flask, precision adds 70% methyl alcohol 30ml, weighed weight, power 250W, the ultrasonic processing of frequency 30kHz 20 minutes, let cool, more weighed weight, with 80% methyl alcohol, supply less loss weight, shake up, filter, get subsequent filtrate, obtain;
Determination method: precision is drawn with reference to product solution and each 7 μ l of need testing solution respectively, injection liquid chromatography, UV-detector detects, and mensuration wavelength is 280nm, records chromatogram;
Test sample finger-print and reference fingerprint are compared, in test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press similarity evaluation and calculate, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90;
14 characteristic peaks corresponding in described coronary disease seven taste dripping pill finger-prints are:
No. 1 peak: relative retention time 0.175, accounts for the Area Ratio 25.03% with reference to peak;
No. 2 peaks: relative retention time 0.201, accounts for the Area Ratio 20.21% with reference to peak;
No. 3 peaks: relative retention time 0.365, accounts for the Area Ratio 6.13% with reference to peak;
No. 4 peaks: relative retention time 0.812, accounts for the Area Ratio 20.73% with reference to peak;
No. 5 peaks: relative retention time 0.851, accounts for the Area Ratio 20.16% with reference to peak;
No. 6 peaks: for reference to peak;
No. 7 peaks: relative retention time 0.986, accounts for the Area Ratio 38.11% with reference to peak;
No. 8 peaks: relative retention time 1.612, accounts for the Area Ratio 21.12% with reference to peak;
No. 9 peaks: relative retention time 1.634, accounts for the Area Ratio 60.92% with reference to peak;
No. 10 peaks: relative retention time 1.832, accounts for the Area Ratio 20.11% with reference to peak;
No. 11 peaks: relative retention time 2.137, accounts for the Area Ratio 41.30% with reference to peak;
No. 12 peaks: relative retention time 2.523, accounts for the Area Ratio 7.68% with reference to peak;
No. 13 peaks: relative retention time 2.610, accounts for the Area Ratio 26.34% with reference to peak;
No. 14 peaks: relative retention time 2.983, accounts for the Area Ratio 28.34% with reference to peak.
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
Above seven tastes, Tan Xiang ﹑ falls fragrant ﹑ mountain a kind of apple ﹑ nutmeg and extracts volatile oil 5 hours with 7.8 times of water gagings, and the another device of aqueous solution after distillation is collected; The three taste medicinal materials such as the dregs of a decoction and all the other reds sage root extract secondary with 5 times of amount 95% alcohol refluxs, each 1 hour, filter, collect filtrate, the dregs of a decoction decoct secondary, each 1.5 hours with 7 times of water gagings, filter, collect filtrate, concentrated each extract to relative density is 1.30 ~ 1.40(60 ℃ respectively) thick paste, merge each thick paste, 80 ℃ of drying under reduced pressure, are ground into fine powder, extract powder, add volatile oil and PEG400, Macrogol 4000 appropriate, take dimethyl silicon oil as cooling medium, make dripping pill, obtain.
Detection method:
Chromatographic condition and system suitability: chromatographic column Inertsil ODS-3150 * 4.6mm, 5 μ m; 35 ℃ of column temperatures; Take octadecylsilane chemically bonded silica as filling agent; Take 1.0% formic acid solution as mobile phase A, and acetonitrile is Mobile phase B, flow velocity 1.0ml/min; By following program, carry out gradient elution: since 0 minute to 45 minutes, mobile phase A became 20% from 85%, since 45 minutes to 55 minutes, mobile phase A became 85% from 20%, and is maintained until 65 minutes, and gradient is linear gradient;
With reference to peak, prepare: get tanshin polyphenolic acid B reference substance 0.01g, accurately weighed, add 75% methyl alcohol and make every 1ml containing the solution of 0.0001g, obtain;
Need testing solution preparation: get coronary disease seven taste dripping pills, porphyrize, gets about 0.3g, accurately weighed, to put in conical flask, precision adds 75% methyl alcohol 50ml, weighed weight, power 280W, the ultrasonic processing of frequency 40kHz 15 minutes, let cool, more weighed weight, with 75% methyl alcohol, supply less loss weight, shake up, filter, get subsequent filtrate, obtain;
Determination method: precision is drawn with reference to product solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, UV-detector detects, and mensuration wavelength is 280nm, records chromatogram;
Test sample finger-print and reference fingerprint are compared, in test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press similarity evaluation and calculate, 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
Above seven tastes, Tan Xiang ﹑ falls fragrant ﹑ mountain a kind of apple ﹑ nutmeg and extracts volatile oil 5 hours with 7.8 times of water gagings, and the another device of aqueous solution after distillation is collected; The three taste medicinal materials such as the dregs of a decoction and all the other reds sage root extract secondary with 5 times of amount 95% alcohol refluxs, each 1 hour, filter, collect filtrate, the dregs of a decoction decoct secondary, each 1.5 hours with 7 times of water gagings, filter, collect filtrate, concentrated each extract to relative density is 1.30 ~ 1.40(60 ℃ respectively) thick paste, merge each thick paste, 80 ℃ of drying under reduced pressure, are ground into fine powder, extract powder, add volatile oil and PEG400, Macrogol 4000 appropriate, take dimethyl silicon oil as cooling medium, make dripping pill, obtain.
Detection method:
Chromatographic condition and system suitability: chromatographic column Inertsil ODS-3150 * 4.6mm, 5 μ m; 30 ℃ of column temperatures; Take octadecylsilane chemically bonded silica as filling agent; Take 2.0% formic acid solution as mobile phase A, and acetonitrile is Mobile phase B, flow velocity 0.8ml/min; By following program, carry out gradient elution: since 0 minute to 45 minutes, mobile phase A became 20% from 85%, since 45 minutes to 55 minutes, mobile phase A became 85% from 20%, and is maintained until 65 minutes, and gradient is linear gradient;
With reference to peak, prepare: get tanshin polyphenolic acid B reference substance 0.008g, accurately weighed, add 80% methyl alcohol and make every 0.7ml containing the solution of 0.00013g, obtain;
Need testing solution preparation: get coronary disease seven taste dripping pills, porphyrize, gets 0.2g, accurately weighed, to put in conical flask, precision adds 70% methyl alcohol 30ml, weighed weight, power 250W, the ultrasonic processing of frequency 30kHz 20 minutes, let cool, more weighed weight, with 80% methyl alcohol, supply less loss weight, shake up, filter, get subsequent filtrate, obtain;
Determination method: precision is drawn with reference to product solution and each 7 μ l of need testing solution respectively, injection liquid chromatography, UV-detector detects, and mensuration wavelength is 280nm, records chromatogram;
Test sample finger-print and reference fingerprint are compared, in test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press similarity evaluation and calculate, 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
Above seven tastes, Tan Xiang ﹑ falls fragrant ﹑ mountain a kind of apple ﹑ nutmeg and extracts volatile oil 5 hours with 7.8 times of water gagings, and the another device of aqueous solution after distillation is collected; The three taste medicinal materials such as the dregs of a decoction and all the other reds sage root extract secondary with 5 times of amount 95% alcohol refluxs, each 1 hour, filter, collect filtrate, the dregs of a decoction decoct secondary, each 1.5 hours with 7 times of water gagings, filter, collect filtrate, concentrated each extract to relative density is 1.30 ~ 1.40(60 ℃ respectively) thick paste, merge each thick paste, 80 ℃ of drying under reduced pressure, are ground into fine powder, extract powder, add volatile oil and PEG400, Macrogol 4000 appropriate, take dimethyl silicon oil as cooling medium, make dripping pill, obtain.
Detection method:
Chromatographic condition and system suitability: chromatographic column Inertsil ODS-3150 * 4.6mm, 5 μ m; 40 ℃ of column temperatures; Take octadecylsilane chemically bonded silica as filling agent; Take 0.5% formic acid solution as mobile phase A, and acetonitrile is Mobile phase B, flow velocity 1.2ml/min; By following program, carry out gradient elution: since 0 minute to 45 minutes, mobile phase A became 20% from 85%, since 45 minutes to 55 minutes, mobile phase A became 85% from 20%, and is maintained until 65 minutes, and gradient is linear gradient;
With reference to peak, prepare: get tanshin polyphenolic acid B reference substance 0.012g, accurately weighed, add 70% methyl alcohol and make every 1.3ml containing the solution of 0.00007g, obtain.
Need testing solution preparation: get coronary disease seven taste dripping pills, porphyrize, gets 0.4g, accurately weighed, to put in conical flask, precision adds 80% methyl alcohol 70ml, weighed weight, power 320W, the ultrasonic processing of frequency 50kHz 10 minutes, let cool, more weighed weight, with 70% methyl alcohol, supply less loss weight, shake up, filter, get subsequent filtrate, obtain;
Determination method: precision is drawn with reference to product solution and each 12 μ l of need testing solution respectively, injection liquid chromatography, UV-detector detects, and mensuration wavelength is 280nm, records chromatogram;
Test sample finger-print and reference fingerprint are compared, in test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press similarity evaluation and calculate, the similarity of test sample finger-print and reference fingerprint must not be lower than 0.90.
Claims (13)
1. a detection method for coronary disease seven taste dripping pill finger-prints, is characterized in that the method comprises the steps:
Chromatographic condition and system suitability: chromatographic column Inertsil ODS-3 150 * 4.6mm, 5 μ m; 25～45 ℃ of column temperatures; Take octadecylsilane chemically bonded silica as filling agent; Take 0.1～3.0% formic acid solution as mobile phase A, and acetonitrile is Mobile phase B, flow velocity 0.5～1.5ml/min; By following program, carry out gradient elution: since 0 minute to 45 minutes, mobile phase A became 20% from 85%, since 45 minutes to 55 minutes, mobile phase A became 85% from 20%, and is maintained until 65 minutes, and gradient is linear gradient;
With reference to product solution, prepare: get tanshin polyphenolic acid B reference substance 0.005-0.015 weight portion, accurately weighed, add 65～85% methyl alcohol and make every 0.5-1.5 parts by volume containing the solution of 0.00005-0.00015 weight portion, obtain;
Need testing solution preparation: get coronary disease seven taste dripping pills, porphyrize, gets 0.2～0.4 weight portion, accurately weighed, to put in conical flask, precision adds 65～85% methyl alcohol 20～80 parts by volume, weighed weight, power 220～350W, the ultrasonic processing of frequency 20-60kHz 7～23 minutes, let cool, more weighed weight, with 65～85% methyl alcohol, supply less loss weight, shake up, filter, get subsequent filtrate, obtain;
Determination method: precision is drawn with reference to product solution and each 5～15 μ l of need testing solution respectively, injection liquid chromatography, UV-detector detects, and mensuration wavelength is 280nm, records chromatogram;
Test sample finger-print and reference fingerprint are compared, in test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press similarity evaluation and calculate, 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 taste dripping pill finger-prints as claimed in claim 1, is characterized in that the method comprises the steps:
Chromatographic condition and system suitability: chromatographic column Inertsil ODS-3 150 * 4.6mm, 5 μ m; 35 ℃ of column temperatures; Take octadecylsilane chemically bonded silica as filling agent; Take 1.0% formic acid solution as mobile phase A, and acetonitrile is Mobile phase B, flow velocity 1.0ml/min; By following program, carry out gradient elution: since 0 minute to 45 minutes, mobile phase A became 20% from 85%, since 45 minutes to 55 minutes, mobile phase A became 85% from 20%, and is maintained until 65 minutes, and gradient is linear gradient;
With reference to product solution, prepare: get tanshin polyphenolic acid B reference substance 0.01 weight portion, accurately weighed, add 75% methyl alcohol and make every 1 parts by volume containing the solution of 0.0001 weight portion, obtain;
Need testing solution preparation: get coronary disease seven taste dripping pills, porphyrize, gets 0.3 weight portion, accurately weighed, to put in conical flask, precision adds 75% methyl alcohol 50 parts by volume, weighed weight, power 280W, the ultrasonic processing of frequency 40kHz 15 minutes, let cool, more weighed weight, with 75% methyl alcohol, supply less loss weight, shake up, filter, get subsequent filtrate, obtain;
Determination method: precision is drawn with reference to product solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, UV-detector detects, and mensuration wavelength is 280nm, records chromatogram;
Test sample finger-print and reference fingerprint are compared, in test sample chromatogram, should present 14 and reference fingerprint characteristic of correspondence peak, press similarity evaluation and calculate, 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 taste dripping pill finger-prints as claimed in claim 1 or 2, is characterized in that 14 characteristic peaks corresponding in described coronary disease seven taste dripping pill finger-prints are:
No. 1 peak: relative retention time 0.170-0.208, accounts for the Area Ratio 1.48%-28.03% with reference to peak;
No. 2 peak: relative retention time 0.199-0.243, account for the Area Ratio 1.33%-25.29% with reference to peak;
No. 3 peak: relative retention time 0.332-0.406, account for the Area Ratio 0.40%-7.63% with reference to peak;
No. 4 peak: relative retention time 0.772-0.943, account for the Area Ratio 1.26%-23.94% with reference to peak;
No. 5 peak: relative retention time 0.811-0.991, account for the Area Ratio 1.18%-22.46% with reference to peak;
No. 6 peaks: for reference to peak;
No. 7 peak: relative retention time 0.965-1.180, account for the Area Ratio 18.69%-43.61% with reference to peak;
No. 8 peak: relative retention time 1.544-1.887, account for the Area Ratio 1.33%-25.22% with reference to peak;
No. 9 peak: relative retention time 1.614-1.973, account for the Area Ratio 33.20%-68.96% with reference to peak;
No. 10 peak: relative retention time 1.802-2.203, account for the Area Ratio 1.22%-23.21% with reference to peak;
No. 11 peak: relative retention time 2.087-2.550, account for the Area Ratio 20.10%-46.90% with reference to peak;
No. 12 peak: relative retention time 2.493-3.047, account for the Area Ratio 0.50%-9.48% with reference to peak;
No. 13 peak: relative retention time 2.540-3.104, account for the Area Ratio 1.50%-28.44% with reference to peak;
No. 14 peak: relative retention time 2.958-3.616, account for the Area Ratio 13.56%-31.64% with reference to peak.
4. the detection method of coronary disease seven taste dripping pill finger-prints as claimed in claim 3, is characterized in that 14 characteristic peaks corresponding in described coronary disease seven taste dripping pill finger-prints are:
No. 1 peak: relative retention time 0.170-0.208, accounts for the Area Ratio 8.48%-20.03% with reference to peak;
No. 2 peak: relative retention time 0.199-0.243, account for the Area Ratio 7.33%-20.29% with reference to peak;
No. 3 peak: relative retention time 0.332-0.406, account for the Area Ratio 2.40%-5.63% with reference to peak;
No. 4 peak: relative retention time 0.772-0.943, account for the Area Ratio 8.26%-19.94% with reference to peak;
No. 5 peak: relative retention time 0.811-0.991, account for the Area Ratio 8.18%-18.46% with reference to peak;
No. 6 peaks: for reference to peak;
No. 7 peak: relative retention time 0.965-1.180, account for the Area Ratio 25.69%-35.61% with reference to peak;
No. 8 peak: relative retention time 1.544-1.887, account for the Area Ratio 8.33%-20.22% with reference to peak;
No. 9 peak: relative retention time 1.614-1.973, account for the Area Ratio 45.20%-60.96% with reference to peak;
No. 10 peak: relative retention time 1.802-2.203, account for the Area Ratio 8.22%-18.21% with reference to peak;
No. 11 peak: relative retention time 2.087-2.550, account for the Area Ratio 30.10%-40.90% with reference to peak;
No. 12 peak: relative retention time 2.493-3.047, account for the Area Ratio 3.50%-6.48% with reference to peak;
No. 13 peak: relative retention time 2.540-3.104, account for the Area Ratio 10.50%-20.44% with reference to peak;
No. 14 peak: relative retention time 2.958-3.616, account for the Area Ratio 18.56%-28.64% with reference to peak.
5. the detection method of coronary disease seven taste dripping pill finger-prints as claimed in claim 3, is characterized in that 14 characteristic peaks corresponding in described coronary disease seven taste dripping pill finger-prints are:
No. 1 peak: relative retention time 0.189, accounts for the Area Ratio 14.75% with reference to peak;
No. 2 peaks: relative retention time 0.221, accounts for the Area Ratio 13.31% with reference to peak;
No. 3 peaks: relative retention time 0.369, accounts for the Area Ratio 4.02% with reference to peak;
No. 4 peaks: relative retention time 0.857, accounts for the Area Ratio 12.60% with reference to peak;
No. 5 peaks: relative retention time 0.901, accounts for the Area Ratio 11.82% with reference to peak;
No. 6 peaks: for reference to peak;
No. 7 peaks: relative retention time 1.073, accounts for the Area Ratio 31.15% with reference to peak;
No. 8 peaks: relative retention time 1.716, accounts for the Area Ratio 13.27% with reference to peak;
No. 9 peaks: relative retention time 1.793, accounts for the Area Ratio 51.08% with reference to peak;
No. 10 peaks: relative retention time 2.002, accounts for the Area Ratio 12.22% with reference to peak;
No. 11 peaks: relative retention time 2.318, accounts for the Area Ratio 33.50% with reference to peak;
No. 12 peaks: relative retention time 2.770, accounts for the Area Ratio 4.99% with reference to peak;
No. 13 peaks: relative retention time 2.822, accounts for the Area Ratio 14.97% with reference to peak;
No. 14 peaks: relative retention time 3.287, accounts for the Area Ratio 22.60% with reference to peak.
6. the detection method of the coronary disease seven taste dripping pill finger-prints as described in claim 1,2,4 or 5, is characterized in that the bulk drug of described coronary disease seven taste 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 taste dripping pill finger-prints as claimed in claim 3, is characterized in that the bulk drug of described coronary disease seven taste 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 taste dripping pill finger-prints as claimed in claim 6, is characterized in that the bulk drug of described coronary disease seven taste dripping pills consists of:
The red sage root 38.4 weight portion santal 4.3 weight portion dalbergia wood 8.5 weight portions
Kaempferia galanga 6.4 weight portion nutmeg 12.8 weight portion fructus choerospondiatis 12.8 weight portions
Sea-buckthorn 12.8 weight portions;
Or the red sage root 21 weight portion santal 6 weight portion dalbergia wood 6 weight portions
Kaempferia galanga 8 weight portion nutmeg 8 weight portion fructus choerospondiatis 18 weight portions
Sea-buckthorn 8 weight portions;
Or the red sage root 50 weight portion santal 3 weight portion dalbergia wood 11 weight portions
Kaempferia galanga 4 weight portion nutmeg 18 weight portion fructus choerospondiatis 8 weight portions
Sea-buckthorn 18 weight portions.
9. the detection method of coronary disease seven taste dripping pill finger-prints as claimed in claim 7, is characterized in that the bulk drug of described coronary disease seven taste dripping pills consists of:
The red sage root 38.4 weight portion santal 4.3 weight portion dalbergia wood 8.5 weight portions
Kaempferia galanga 6.4 weight portion nutmeg 12.8 weight portion fructus choerospondiatis 12.8 weight portions
Sea-buckthorn 12.8 weight portions;
Or the red sage root 21 weight portion santal 6 weight portion dalbergia wood 6 weight portions
Kaempferia galanga 8 weight portion nutmeg 8 weight portion fructus choerospondiatis 18 weight portions
Sea-buckthorn 8 weight portions;
Or the red sage root 50 weight portion santal 3 weight portion dalbergia wood 11 weight portions
Kaempferia galanga 4 weight portion nutmeg 18 weight portion fructus choerospondiatis 8 weight portions
Sea-buckthorn 18 weight portions.
10. the detection method of coronary disease seven taste dripping pill finger-prints as claimed in claim 6, is characterized in that the preparation method of described coronary disease seven taste dripping pills is:
Santal, dalbergia wood, Kaempferia galanga, nutmeg are extracted to volatile oil 2-8 hour with 5-10 times of water gaging, and the another device of aqueous solution after distillation is collected, the dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three taste medicinal materials are doubly measured 75-95% alcohol reflux with 2-8 and are extracted 1-3 time, 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, the thick paste that relative density is 1.30～1.40 during concentrated each extract to 60 ℃ respectively, merge above-mentioned aqueous solution and filtrate, 80 ℃ of drying under reduced pressure, be ground into fine powder, obtain extract powder, add volatile oil, the PEG400 of 2-10 weight portion, the Macrogol 4000 of 20-28 weight portion, take dimethyl silicon oil as cooling medium, make dripping pill.
The detection method of 11. coronary disease seven taste dripping pill finger-prints as described in one of claim 7-9, is characterized in that the preparation method of described coronary disease seven taste dripping pills is:
Santal, dalbergia wood, Kaempferia galanga, nutmeg are extracted to volatile oil 2-8 hour with 5-10 times of water gaging, and the another device of aqueous solution after distillation is collected, the dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three taste medicinal materials are doubly measured 75-95% alcohol reflux with 2-8 and are extracted 1-3 time, 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, the thick paste that relative density is 1.30～1.40 during concentrated each extract to 60 ℃ respectively, merge above-mentioned aqueous solution and filtrate, 80 ℃ of drying under reduced pressure, be ground into fine powder, obtain extract powder, add volatile oil, the PEG400 of 2-10 weight portion, the Macrogol 4000 of 20-28 weight portion, take dimethyl silicon oil as cooling medium, make dripping pill.
The detection method of 12. coronary disease seven taste dripping pill finger-prints as claimed in claim 10, is characterized in that the preparation method of described coronary disease seven taste dripping pills is:
Santal, dalbergia wood, Kaempferia galanga, nutmeg are extracted to volatile oil 5 hours with 7.8 times of water gagings, and the another device of aqueous solution after distillation is collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three taste medicinal materials extract secondary with 5 times of amount 95% alcohol refluxs, 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, the thick paste that relative density is 1.30～1.40 during concentrated each extract to 60 ℃ respectively, merge each thick paste, 80 ℃ of drying under reduced pressure, are ground into fine powder, obtain extract powder, add the PEG400 of volatile oil, 5 weight portions, the Macrogol 4000 of 25 weight portions, take dimethyl silicon oil as cooling medium, make dripping pill.
The detection method of 13. coronary disease seven taste dripping pill finger-prints as claimed in claim 11, is characterized in that the preparation method of described coronary disease seven taste dripping pills is:
Santal, dalbergia wood, Kaempferia galanga, nutmeg are extracted to volatile oil 5 hours with 7.8 times of water gagings, and the another device of aqueous solution after distillation is collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three taste medicinal materials extract secondary with 5 times of amount 95% alcohol refluxs, 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, the thick paste that relative density is 1.30～1.40 during concentrated each extract to 60 ℃ respectively, merge each thick paste, 80 ℃ of drying under reduced pressure, are ground into fine powder, obtain extract powder, add the PEG400 of volatile oil, 5 weight portions, the Macrogol 4000 of 25 weight portions, take dimethyl silicon oil as cooling medium, make dripping pill.
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| 《冠心七味片的质量标准研究》;黄鸣清 等;《广州中医药大学学报》;20060131;第23卷(第1期);59-61页 * |
| 《冠心七味片鉴别方法研究》;李卓明 等;《中国实验方剂学杂志》;20060331;第12卷(第3期);29-31页 * |
| 李卓明 等.《冠心七味片鉴别方法研究》.《中国实验方剂学杂志》.2006,第12卷(第3期), |
| 黄鸣清 等.《冠心七味片的质量标准研究》.《广州中医药大学学报》.2006,第23卷(第1期), |
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