CN102297922B - Fingerprint detecting method of volatile components in Guanxin seven-flavor dripping pills - Google Patents
Fingerprint detecting method of volatile components in Guanxin seven-flavor dripping pills Download PDFInfo
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Abstract
The invention discloses a fingerprint detecting method of volatile components in Guanxin seven-flavor dripping pills, comprising the following steps of: using Aiglent Innowax as a chromatographic column and nitrogen as a carrier gas with the column temperature being temperature programming and the split ratio being 1:1, directly sampling, calculating theoretical plate number according to ethyl p-methoxycinnamate peak with the theoretical plate number being no less than 300000; taking an ethyl p-methoxycinnamate reference substance, adding methanol to prepare a solution as a reference solution; taking a pharmaceutical composition provided by the invention, followed by fine grinding, adding methanol, shaking up, centrifuging, and taking a supernatant as a tested object solution; respectively taking two microliters of the reference solution and the tested object solution, injecting a gas chromatography, determining, and recording chromatogram; and comparing the tested object fingerprint with the reference fingerprint to show ten characteristic peaks corresponding to the reference fingerprint with the similarity of the tested object fingerprint and the reference fingerprint being not lower than 0.90. The invention has advantages of strong specialization, good stability and good reappearance.
Description
Technical field
The present invention relates to a kind of detection method, particularly relate to a kind of fingerprint atlas detection method of coronary disease seven flavor dripping pills.
Background technology
Coronary disease seven flavor dripping pills are 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 only has the coherence check of proterties and tablet general rule aspect quality control, substantially can not control the inherent quality of product.
Summary of the invention
The object of the present invention is to provide a kind of fingerprint atlas detection method of coronary disease seven flavor dripping pills.
The present invention is achieved through the following technical solutions:
The fingerprint atlas detection method of coronary disease seven flavor dripping pills of the present invention comprises the steps:
Chromatographic condition and system suitability are take Aiglent Innowax 30m * 0.32mm * 0.5 μ m as chromatographic column, and nitrogen buffer gas, detecting device are flame ionization ditector, and injector temperature is 150-350 ℃, and detector temperature is 150-350 ℃; Nitrogen flow rate is 1-3ml/min, and hydrogen flow rate is 25-45ml/min, and air velocity is 250-450ml/min; Column temperature is temperature programme, and initial temperature is 50-150 ℃, with the speed of 1-3 ℃/minute, is warming up to 150-290 ℃, keeps 5-15 minute, split ratio 1: 1, and direct injected, number of theoretical plate is pressed the ethyl ρ-methoxy cinnamate peak and is calculated, and should be not less than 300000;
It is appropriate that the ethyl ρ-methoxy cinnamate reference substance is got in the preparation of object of reference solution, accurately weighed, adds methyl alcohol and make every 1ml and contain the solution of 0.1-0.3mg;
Determination method is accurate object of reference solution and each 1-3 μ l of need testing solution of drawing respectively, and the injection gas chromatography view, measure, and records chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, present 10 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 fingerprint atlas detection method of coronary disease seven flavor dripping pills of the present invention comprises the steps:
Chromatographic condition and system suitability are take Aiglent Innowax 30m * 0.32mm * 0.5 μ m as chromatographic column, and nitrogen buffer gas, detecting device are flame ionization ditector, and injector temperature is 250 ℃, and detector temperature is 250 ℃; Nitrogen flow rate is 2ml/min, and hydrogen flow rate is 35ml/min, and air velocity is 350ml/min; Column temperature is temperature programme, and initial temperature is 100 ℃, with the speed of 2 ℃/minute, is warming up to 220 ℃, kept 10 minutes, and split ratio 1: 1, direct injected, number of theoretical plate is pressed the ethyl ρ-methoxy cinnamate peak and is calculated, and should be not less than 300000;
It is appropriate that the ethyl ρ-methoxy cinnamate reference substance is got in the preparation of object of reference solution, accurately weighed, adds methyl alcohol and make every 1ml and contain the solution of 0.2mg;
Drug regimen 1.0 weight portions of the present invention are got in the preparation of need testing solution, and porphyrize is put in 10 parts by volume volumetric flasks, adds appropriate methyl alcohol, and power is 280W, frequency is 40kHz, and ultrasonic processing 10 minutes, let cool, and is settled to scale, shake up, 5000 rev/mins centrifugal, centrifugal 5 minutes, gets supernatant;
Determination method is accurate object of reference solution and each 2 μ l of need testing solution of drawing respectively, and the injection gas chromatography view, measure, and records chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 10 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.
10 specific features peaks corresponding with reference fingerprint that present in coronary disease of the present invention seven flavor dripping pill finger-prints are: No. 3 peaks, No. 4 peaks and No. 6 peaks are the composition in dalbergia wood; No. 1 peak, No. 2 peaks, No. 5 peaks, No. 7 peaks and No. 10 peaks are the composition in nutmeg; No. 9 peaks are the composition in kaempferia galamga; No. 8 peaks are the composition in santal.
10 of the present invention with the relative retention time at reference fingerprint characteristic of correspondence peak and the Area Ratio that accounts for reference to peak are:
No. 1 peak: relative retention time 0.192-0.235, account for the Area Ratio 64.59%-134.16% with reference to peak;
No. 2 peak: relative retention time 0.371-0.454, account for the Area Ratio 1.90%-36.14% with reference to peak;
No. 3 peak: relative retention time 0.448-0.548, account for the Area Ratio 30.59%-71.38% with reference to peak;
No. 4 peak: relative retention time 0.468-0.572, account for the Area Ratio 38.76%-90.44% with reference to peak;
No. 5 peak: relative retention time 0.477-0.584, account for the Area Ratio 43.68%-101.93% with reference to peak;
No. 6 peak: relative retention time 0.497-0.607, account for the Area Ratio 86.70%-202.31% with reference to peak;
No. 7 peak: relative retention time 0.655-0.800, account for the Area Ratio 92.25%-191.59% with reference to peak;
No. 8 peak: relative retention time 0.822-1.004, account for the Area Ratio 2.99%-56.78% with reference to peak;
No. 9 peaks: be the reference peak;
No. 10 peak: relative retention time 0.956-1.169, account for the Area Ratio 161.06%-299.11% with reference to peak.
10 of the present invention with the relative retention time at reference fingerprint characteristic of correspondence peak and the Area Ratio that accounts for reference to peak are:
No. 1 peak: relative retention time 0.192-0.235, account for the Area Ratio 80.59%-120.16% with reference to peak;
No. 2 peak: relative retention time 0.371-0.454, account for the Area Ratio 10.90%-25.14% with reference to peak;
No. 3 peak: relative retention time 0.448-0.548, account for the Area Ratio 40.59%-60.38% with reference to peak;
No. 4 peak: relative retention time 0.468-0.572, account for the Area Ratio 50.76%-75.44% with reference to peak;
No. 5 peak: relative retention time 0.477-0.584, account for the Area Ratio 60.68%-80.93% with reference to peak;
No. 6 peak: relative retention time 0.497-0.607, account for the Area Ratio 120.70%-170.31% with reference to peak;
No. 7 peak: relative retention time 0.655-0.800, account for the Area Ratio 120.25%-170.59% with reference to peak;
No. 8 peak: relative retention time 0.822-1.004, account for the Area Ratio 15.99%-30.78% with reference to peak;
No. 9 peaks: be the reference peak;
No. 10 peak: relative retention time 0.956-1.169, account for the Area Ratio 190.06%-250.11% with reference to peak.
10 of the present invention with the relative retention time at reference fingerprint characteristic of correspondence peak and the Area Ratio that accounts for reference to peak are:
No. 1 peak: relative retention time 0.213 accounts for the Area Ratio 99.38% with reference to peak;
No. 2 peaks: relative retention time 0.412 accounts for the Area Ratio 19.02% with reference to peak;
No. 3 peaks: relative retention time 0.498 accounts for the Area Ratio 50.99% with reference to peak;
No. 4 peaks: relative retention time 0.520 accounts for the Area Ratio 64.60% with reference to peak;
No. 5 peaks: relative retention time 0.530 accounts for the Area Ratio 72.80% with reference to peak;
No. 6 peaks: relative retention time 0.552 accounts for the Area Ratio 144.51% with reference to peak;
No. 7 peaks: relative retention time 0.727 accounts for the Area Ratio 141.92% with reference to peak;
No. 8 peaks: relative retention time 0.913 accounts for the Area Ratio 29.88% with reference to peak;
No. 9 peaks: be the reference peak;
No. 10 peaks: relative retention time 1.062 accounts for the Area Ratio 230.08% with reference to peak.
Coronary disease seven flavor dripping pills of the present invention are made by the 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 of coronary disease seven flavor dripping pills of the present invention 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
The bulk drug of coronary disease seven flavor dripping pills of the present invention consists of:
The red sage root 21 weight portion santal 6 weight portion dalbergia wood 6 weight portions
Sea-buckthorn 8 weight portions
The bulk drug of coronary disease seven flavor dripping pills of the present invention consists of:
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 flavor dripping pills of the present invention is:
santal, dalbergia wood, Kaempferia galanga, nutmeg are extracted volatile oil 2-8 hour with 5-10 times of water gaging, and the another device of the aqueous solution after distillation is 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 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, relative density is 1.30～1.40 thick paste 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 15-35 weight portion, take dimethyl silicon oil as cooling medium, make dripping pill.
The preparation method of coronary disease seven flavor dripping pills of the present invention is preferably:
Santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 5 hours with 7.8 times of water gagings, and the another device of the aqueous solution after distillation is collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor 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, relative density is 1.30～1.40 thick paste during concentrated each extract to 60 ℃ respectively, merge each thick paste, 80 ℃ of drying under reduced pressure, be 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 pass of weight portion of the present invention and parts by volume is g/ml or kg/l.
The advantage of the fingerprint atlas detection method 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 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.Quality and the curative effect of controlling coronary disease seven flavor dripping pills are significant.
Description of drawings
Fig. 1 is reference fingerprint;
Fig. 2 is with reference to the product collection of illustrative plates;
Fig. 3 is the dalbergia wood medicinal materials fingerprint;
Fig. 4 is the nutmeg medicinal materials fingerprint;
Fig. 5 is the kaempferia galamga medicinal materials fingerprint;
Fig. 6 is the santal medicinal materials fingerprint;
Fig. 7 is sample 1 collection of illustrative plates;
Fig. 8 is sample 2 collection of illustrative plates;
Fig. 9 is sample 3 collection of illustrative plates;
Figure 10 is sample 4 collection of illustrative plates;
Figure 11 is sample 5 collection of illustrative plates;
Figure 12 is sample 6 collection of illustrative plates;
Figure 13 is sample 7 collection of illustrative plates.
Figure 14 is sample 8 collection of illustrative plates.
Figure 15 is sample 9 collection of illustrative plates.
Figure 16 is sample 10 collection of illustrative plates.
Figure 17 is sample 11 collection of illustrative plates.
Figure 18 is sample 12 collection of illustrative plates.
Figure 19 is sample 13 collection of illustrative plates.
Figure 20 is sample 14 collection of illustrative plates.
Figure 21 is sample 15 collection of illustrative plates
Figure 22 is sample 16 collection of illustrative plates.
Figure 23 is sample 17 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: the shaker test of chromatographic condition and system condition.
1, the selection of heating schedule selects three kinds of heating schedules to test.
The first heating schedule: column temperature is temperature programme, and initial temperature is 90 ℃, with the speed of 2 ℃/minute, is warming up to 200 ℃, keeps 12 minutes.
The second heating schedule: column temperature is temperature programme, and initial temperature is 110 ℃, with the speed of 2 ℃/minute, is warming up to 230 ℃, keeps 15 minutes.
The third heating schedule: column temperature is temperature programme, and initial temperature is 100 ℃, with the speed of 2 ℃/minute, is warming up to 220 ℃, keeps 10 minutes.
Test findings: finger-print peak type and the degree of separation of the third heating schedule gained are all best, and acquisition time is also less, so select the third heating schedule.
2, the selection of chromatographic column selects three kinds of chromatographic columns to test.
The first chromatographic column: AC-20 30m * 0.32mm * 0.5 μ m.
The second chromatographic column: DB-wax 30m * 0.32mm * 0.5 μ m.
The third chromatographic column: Aiglent Innowax 30m * 0.32mm * 0.5 μ m.
Test findings: finger-print peak type and the degree of separation of first and second kind chromatographic column gained are slightly poor, finger-print peak type and the degree of separation of the third chromatographic column gained are best, so final definite the third chromatographic column (Aiglent Innowax 30m * 0.32mm * 0.5 μ m) of using.
The fingerprint atlas detection method test of volatile ingredient in experimental example two, coronary disease of the present invention seven flavor dripping pills (according to embodiment 1 preparation method, making)
1, the finger print measuring method of coronary disease seven flavor dripping pills
(1), chromatographic condition and system suitability be take Aiglent Innowax 30m * 0.32mm * 0.5 μ m as chromatographic column, nitrogen buffer gas, detecting device are flame ionization ditector, injector temperature is 250 ℃, detector temperature is 250 ℃; Nitrogen flow rate is 2ml/min, and hydrogen flow rate is 35ml/min, and air velocity is 350ml/min; Column temperature is temperature programme, and initial temperature is 100 ℃, with the speed of 2 ℃/minute, is warming up to 220 ℃, kept 10 minutes, and split ratio 1: 1, direct injected, number of theoretical plate is pressed the ethyl ρ-methoxy cinnamate peak and is calculated, and should be not less than 300000.
(2), that the ethyl ρ-methoxy cinnamate reference substance is got in the preparation of object of reference solution is appropriate, accurately weighed, adds methyl alcohol and makes every 1ml and contain the solution of 0.2mg, obtain.
(3), need testing solution to prepare sample thief appropriate, porphyrize, get approximately 1.0g, accurately weighed, put in the 10ml volumetric flask, add appropriate methyl alcohol, ultrasonic processing (power 280W, frequency 40kHz) 10 minutes, let cool, be settled to scale, shake up, centrifugal (5000 rev/mins) 5 minutes, get supernatant, obtains.
(4), determination method accurate each 2 μ l of object of reference solution and need testing solution that draw respectively, the injection gas chromatography view, mensuration, record chromatogram, obtains.
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 10 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, reference fingerprint (seeing Fig. 1)
Wherein: instrument, chromatographic column and integral parameter: Agilent 6890N gas liqud chromatography instrument, Instrument chromatographic work station.Chromatographic column is Aiglent Innowax (30m * 0.32mm * 0.5 μ m).Slope: 30; Peak width: 0.03.
3, the explanation of reference fingerprint
Coronary disease seven flavor dripping pills are formed by seven flavor Chinese drug preparations, and with reference to the accompanying drawings as can be known, wherein four flavor Chinese medicine dalbergia woods, nutmeg, volatile ingredient that kaempferia galamga is relevant with santal all have embodiment in finger-print: No. 3 peaks, No. 4 peaks and No. 6 peaks are the composition in dalbergia wood; No. 1 peak, No. 2 peaks, No. 5 peaks, No. 7 peaks and No. 10 peaks are the composition in nutmeg; Composition in No. 9 peak kaempferia galamgas; No. 8 peaks are the composition in santal.So this method is significant to the quality control of coronary disease seven flavor dripping pills.
4, sample determining fingerprint pattern
(1), chromatographic condition and system suitability be take Aiglent Innowax 30m * 0.32mm * 0.5 μ m as chromatographic column, nitrogen buffer gas, detecting device are flame ionization ditector, injector temperature is 250 ℃, detector temperature is 250 ℃; Nitrogen flow rate is 2ml/min, and hydrogen flow rate is 35ml/min, and air velocity is 350ml/min; Column temperature is temperature programme, and initial temperature is 100 ℃, with the speed of 2 ℃/minute, is warming up to 220 ℃, kept 10 minutes, and split ratio 1: 1, direct injected, number of theoretical plate is pressed the ethyl ρ-methoxy cinnamate peak and is calculated, and should be not less than 300000.
(2), that the ethyl ρ-methoxy cinnamate reference substance is got in the preparation of object of reference solution is appropriate, accurately weighed, adds methyl alcohol and makes every 1ml and contain the solution of 0.2mg, obtain.
(3), need testing solution to prepare sample thief appropriate, porphyrize, get approximately 1.0g, accurately weighed, put in the 10ml volumetric flask, add appropriate methyl alcohol, ultrasonic processing (power 280W, frequency 40kHz) 10 minutes, let cool, be settled to scale, shake up, centrifugal (5000 rev/mins) 5 minutes, get supernatant, obtains.
(4), determination method accurate each 2 μ l of object of reference solution and need testing solution that draw respectively, the injection gas chromatography view, mensuration, record chromatogram, obtains.
5, discussion of results:
The finger-print of comparative sample 1～17, find: 1., 10 of total chromatographic peaks are all arranged in 17 batch samples; 2., the finger-print of sample 8 is the most representative, so determine that the finger-print of sample 8 is reference fingerprint.
The finger-print of other samples and reference fingerprint are compared, in the test sample chromatogram, 10 and reference fingerprint characteristic of correspondence peak are all arranged, 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 | 10 | 0.968 |
| |
10 | 0.967 |
| |
10 | 0.956 |
| |
10 | 0.977 |
| |
10 | 0.989 |
| |
10 | 0.994 |
| |
10 | 0.993 |
| |
10 | 1.000 |
| |
10 | 0.986 |
| |
10 | 0.989 |
| |
10 | 0.993 |
| |
10 | 0.994 |
| |
10 | 0.995 |
| |
10 | 0.968 |
| |
10 | 0.985 |
| |
10 | 0.985 |
| |
10 | 0.978 |
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
Santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 5 hours with 7.8 times of water gagings, and the another device of the aqueous solution after distillation is collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor 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, relative density is 1.30～1.40 thick paste during concentrated each extract to 60 ℃ respectively, merge each thick paste, 80 ℃ of drying under reduced pressure, be ground into fine powder, obtain extract powder, add the PEG400 of volatile oil, 5g, the Macrogol 4000 of 25g,, take dimethyl silicon oil as cooling medium, make dripping pill.
Detection method:
Chromatographic condition and system suitability are take Aiglent Innowax 30m * 0.32mm * 0.5 μ m as chromatographic column, and nitrogen buffer gas, detecting device are flame ionization ditector, and injector temperature is 250 ℃, and detector temperature is 250 ℃; Nitrogen flow rate is 2ml/min, and hydrogen flow rate is 35ml/min, and air velocity is 350ml/min; Column temperature is temperature programme, and initial temperature is 100 ℃, with the speed of 2 ℃/minute, is warming up to 220 ℃, kept 10 minutes, and split ratio 1: 1, direct injected, number of theoretical plate is pressed the ethyl ρ-methoxy cinnamate peak and is calculated, and should be not less than 300000;
It is appropriate that the ethyl ρ-methoxy cinnamate reference substance is got in the preparation of object of reference solution, accurately weighed, adds methyl alcohol and make every 1ml and contain the solution of 0.2mg;
Drug regimen 1.0g of the present invention is got in the preparation of need testing solution, and porphyrize is put in the 10ml volumetric flask, adds appropriate methyl alcohol, and power is 280W, frequency is 40kHz, and ultrasonic processing 10 minutes, let cool, and is settled to scale, shake up, 5000 rev/mins centrifugal, centrifugal 5 minutes, gets supernatant;
Determination method is accurate object of reference solution and each 2 μ l of need testing solution of drawing respectively, and the injection gas chromatography view, measure, and records chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 10 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;
10 specific features peaks corresponding with reference fingerprint that present in described coronary disease seven flavor dripping pill finger-prints are: No. 3 peaks, No. 4 peaks and No. 6 peaks are the composition in dalbergia wood; No. 1 peak, No. 2 peaks, No. 5 peaks, No. 7 peaks and No. 10 peaks are the composition in nutmeg; No. 9 peaks are the composition in kaempferia galamga; No. 8 peaks are the composition in santal;
Described 10 with the relative retention time at reference fingerprint characteristic of correspondence peak and the Area Ratio that accounts for reference to peak are:
No. 1 peak: relative retention time 0.213 accounts for the Area Ratio 99.38% with reference to peak;
No. 2 peaks: relative retention time 0.412 accounts for the Area Ratio 19.02% with reference to peak;
No. 3 peaks: relative retention time 0.498 accounts for the Area Ratio 50.99% with reference to peak;
No. 4 peaks: relative retention time 0.520 accounts for the Area Ratio 64.60% with reference to peak;
No. 5 peaks: relative retention time 0.530 accounts for the Area Ratio 72.80% with reference to peak;
No. 6 peaks: relative retention time 0.552 accounts for the Area Ratio 144.51% with reference to peak;
No. 7 peaks: relative retention time 0.727 accounts for the Area Ratio 141.92% with reference to peak;
No. 8 peaks: relative retention time 0.913 accounts for the Area Ratio 29.88% with reference to peak;
No. 9 peaks: be the reference peak;
No. 10 peaks: relative retention time 1.062 accounts for the Area Ratio 230.08% with reference to peak.
Embodiment 2:
Red sage root 21g santal 6g dalbergia wood 6g Kaempferia galanga 8g
Nutmeg 8g fructus choerospondiatis 18g sea-buckthorn 8g
Santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 7 hours with 6 times of water gagings, and the another device of the aqueous solution after distillation is collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor medicinal materials extract 1 time with 3 times of amount 80% alcohol refluxs, each 0.7 hour, filter, collect filtrate, the dregs of a decoction decoct 3 times with 9 times of water gagings, each 1 hour, filter, collect filtrate, relative density is 1.30～1.40 thick paste 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 the PEG400 of volatile oil, 3 weight portions, the Macrogol 4000 of 30 weight portions,, take dimethyl silicon oil as cooling medium, make dripping pill;
Detection method:
Chromatographic condition and system suitability are take Aiglent Innowax 30m * 0.32mm * 0.5 μ m as chromatographic column, and nitrogen buffer gas, detecting device are flame ionization ditector, and injector temperature is 200 ℃, and detector temperature is 300 ℃; Nitrogen flow rate is 1.5ml/min, and hydrogen flow rate is 40ml/min, and air velocity is 300ml/min; Column temperature is temperature programme, and initial temperature is 130 ℃, with the speed of 1.5 ℃/minute, is warming up to 270 ℃, kept 7 minutes, and split ratio 1: 1, direct injected, number of theoretical plate is pressed the ethyl ρ-methoxy cinnamate peak and is calculated, and should be not less than 300000;
It is appropriate that the ethyl ρ-methoxy cinnamate reference substance is got in the preparation of object of reference solution, accurately weighed, adds methyl alcohol and make every 0.8ml and contain the solution of 0.25mg;
Pharmaceutical composition 0.7g of the present invention is got in the preparation of need testing solution, and porphyrize is put in the 15ml volumetric flask, adds methyl alcohol, power is 240W, and frequency is the ultrasonic processing of 55kHz 7 minutes, lets cool, and is settled to scale, shake up, 4000 rev/mins centrifugal, centrifugal 6 minutes, gets supernatant;
Determination method is accurate object of reference solution and each 1 μ l of need testing solution of drawing respectively, and the injection gas chromatography view, measure, and records chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, present 10 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.
10 specific features peaks corresponding with reference fingerprint that present in described coronary disease seven flavor dripping pill finger-prints are: No. 3 peaks, No. 4 peaks and No. 6 peaks are the composition in dalbergia wood; No. 1 peak, No. 2 peaks, No. 5 peaks, No. 7 peaks and No. 10 peaks are the composition in nutmeg; No. 9 peaks are the composition in kaempferia galamga; No. 8 peaks are the composition in santal.
Described 10 with the relative retention time at reference fingerprint characteristic of correspondence peak and the Area Ratio that accounts for reference to peak are:
No. 1 peak: relative retention time 0.202 accounts for the Area Ratio 124.66% with reference to peak;
No. 2 peaks: relative retention time 0.385 accounts for the Area Ratio 33.13% with reference to peak;
No. 3 peaks: relative retention time 0.465 accounts for the Area Ratio 65.18% with reference to peak;
No. 4 peaks: relative retention time 0.483 accounts for the Area Ratio 85.22% with reference to peak;
No. 5 peaks: relative retention time 0.489 accounts for the Area Ratio 95.93% with reference to peak;
No. 6 peaks: relative retention time 0.513 accounts for the Area Ratio 185.22% with reference to peak;
No. 7 peaks: relative retention time 0.685 accounts for the Area Ratio 181.33% with reference to peak;
No. 8 peaks: relative retention time 0.924 accounts for the Area Ratio 50.18% with reference to peak;
No. 9 peaks: be the reference peak;
No. 10 peaks: relative retention time 0.987 accounts for the Area Ratio 260.21% with reference to peak.
Red sage root 50g santal 3g dalbergia wood 11g Kaempferia galanga 4g
Nutmeg 18g fructus choerospondiatis 8g sea-buckthorn 18g
Santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 3 hours with 9 times of water gagings, and the another device of the aqueous solution after distillation is collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor medicinal materials extract 3 times with 7 times of amount 90% alcohol refluxs, each 1.3 hours, filter, collect filtrate, the dregs of a decoction decoct 1 time with 5 times of water gagings, each 1.5 hours, filter, collect filtrate, relative density is 1.30～1.40 thick paste during concentrated each extract to 60 ℃ respectively, merge above-mentioned aqueous solution and filtrate, 110 ℃ of drying under reduced pressure, be ground into fine powder, obtain extract powder, add the PEG400 of volatile oil, 9g, the Macrogol 4000 of 30g,, take dimethyl silicon oil as cooling medium, make dripping pill.
Detection method
Chromatographic condition and system suitability are take Aiglent Innowax 30m * 0.32mm * 0.5 μ m as chromatographic column, and nitrogen buffer gas, detecting device are flame ionization ditector, and injector temperature is 300 ℃, and detector temperature is 200 ℃; Nitrogen flow rate is 3ml/min, and hydrogen flow rate is 30ml/min, and air velocity is 400ml/min; Column temperature is temperature programme, and initial temperature is 70 ℃, with the speed of 2.5 ℃/minute, is warming up to 180 ℃, kept 12 minutes, and split ratio 1: 1, direct injected, number of theoretical plate is pressed the ethyl ρ-methoxy cinnamate peak and is calculated, and should be not less than 300000;
It is appropriate that the ethyl ρ-methoxy cinnamate reference substance is got in the preparation of object of reference solution, accurately weighed, adds methyl alcohol and make every 1.2ml and contain the solution of 0.15mg;
Pharmaceutical composition 1.3 weight portions of the present invention are got in the preparation of need testing solution, and porphyrize is put in 5 parts by volume volumetric flasks, adds methyl alcohol, power is 320W, and frequency is the ultrasonic processing of 30kHz 13 minutes, lets cool, and is settled to scale, shake up, 6000 rev/mins centrifugal, centrifugal 4 minutes, gets supernatant;
Determination method is accurate object of reference solution and each 3 μ l of need testing solution of drawing respectively, and the injection gas chromatography view, measure, and records chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, present 10 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.
10 specific features peaks corresponding with reference fingerprint that present in described coronary disease seven flavor dripping pill finger-prints are: No. 3 peaks, No. 4 peaks and No. 6 peaks are the composition in dalbergia wood; No. 1 peak, No. 2 peaks, No. 5 peaks, No. 7 peaks and No. 10 peaks are the composition in nutmeg; No. 9 peaks are the composition in kaempferia galamga; No. 8 peaks are the composition in santal.
Described 10 with the relative retention time at reference fingerprint characteristic of correspondence peak and the Area Ratio that accounts for reference to peak are:
No. 1 peak: relative retention time 0.205 accounts for the Area Ratio 84.69%% with reference to peak;
No. 2 peaks: relative retention time 0.424 accounts for the Area Ratio 7.30% with reference to peak;
No. 3 peaks: relative retention time 0.528 accounts for the Area Ratio 65.33% with reference to peak;
No. 4 peaks: relative retention time 0.532 accounts for the Area Ratio 45.66% with reference to peak;
No. 5 peaks: relative retention time 0.514 accounts for the Area Ratio 63.38% with reference to peak;
No. 6 peaks: relative retention time 0.537 accounts for the Area Ratio 98.70%% with reference to peak;
No. 7 peaks: relative retention time 0.685 accounts for the Area Ratio 112.25% with reference to peak;
No. 8 peaks: relative retention time 0.924 accounts for the Area Ratio 8.69% with reference to peak;
No. 9 peaks: be the reference peak;
No. 10 peaks: relative retention time 1.151 accounts for the Area Ratio 191.16% 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
Santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 5 hours with 7.8 times of water gagings, and the another device of the aqueous solution after distillation is collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor 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, relative density is 1.30～1.40 thick paste during concentrated each extract to 60 ℃ respectively, merge each thick paste, 80 ℃ of drying under reduced pressure, be ground into fine powder, obtain extract powder, add the PEG400 of volatile oil, 5g, the Macrogol 4000 of 25g,, take dimethyl silicon oil as cooling medium, make dripping pill.
Detection method:
Chromatographic condition and system suitability are take Aiglent Innowax 30m * 0.32mm * 0.5 μ m as chromatographic column, and nitrogen buffer gas, detecting device are flame ionization ditector, and injector temperature is 250 ℃, and detector temperature is 250 ℃; Nitrogen flow rate is 2ml/min, and hydrogen flow rate is 35ml/min, and air velocity is 350ml/min; Column temperature is temperature programme, and initial temperature is 100 ℃, with the speed of 2 ℃/minute, is warming up to 220 ℃, kept 10 minutes, and split ratio 1: 1, direct injected, number of theoretical plate is pressed the ethyl ρ-methoxy cinnamate peak and is calculated, and should be not less than 300000;
It is appropriate that the ethyl ρ-methoxy cinnamate reference substance is got in the preparation of object of reference solution, accurately weighed, adds methyl alcohol and make every 1ml and contain the solution of 0.2mg;
Drug regimen 1.0g of the present invention is got in the preparation of need testing solution, and porphyrize is put in the 10ml volumetric flask, adds appropriate methyl alcohol, and power is 280W, frequency is 40kHz, and ultrasonic processing 10 minutes, let cool, and is settled to scale, shake up, 5000 rev/mins centrifugal, centrifugal 5 minutes, gets supernatant;
Determination method is accurate object of reference solution and each 2 μ l of need testing solution of drawing respectively, and the injection gas chromatography view, measure, and records chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 10 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;
10 specific features peaks corresponding with reference fingerprint that present in described coronary disease seven flavor dripping pill finger-prints are: No. 3 peaks, No. 4 peaks and No. 6 peaks are the composition in dalbergia wood; No. 1 peak, No. 2 peaks, No. 5 peaks, No. 7 peaks and No. 10 peaks are the composition in nutmeg; No. 9 peaks are the composition in kaempferia galamga; No. 8 peaks are the composition in santal.
Red sage root 21g santal 6g dalbergia wood 6g Kaempferia galanga 8g
Nutmeg 8g fructus choerospondiatis 18g sea-buckthorn 8g
Santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 7 hours with 6 times of water gagings, and the another device of the aqueous solution after distillation is collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor medicinal materials extract 1 time with 3 times of amount 80% alcohol refluxs, each 0.7 hour, filter, collect filtrate, the dregs of a decoction decoct 3 times with 9 times of water gagings, each 1 hour, filter, collect filtrate, relative density is 1.30～1.40 thick paste 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 the PEG400 of volatile oil, 3 weight portions, the Macrogol 4000 of 30 weight portions,, take dimethyl silicon oil as cooling medium, make dripping pill;
Detection method:
Chromatographic condition and system suitability are take Aiglent Innowax 30m * 0.32mm * 0.5 μ m as chromatographic column, and nitrogen buffer gas, detecting device are flame ionization ditector, and injector temperature is 200 ℃, and detector temperature is 300 ℃; Nitrogen flow rate is 1.5ml/min, and hydrogen flow rate is 40ml/min, and air velocity is 300ml/min; Column temperature is temperature programme, and initial temperature is 130 ℃, with the speed of 1.5 ℃/minute, is warming up to 270 ℃, kept 7 minutes, and split ratio 1: 1, direct injected, number of theoretical plate is pressed the ethyl ρ-methoxy cinnamate peak and is calculated, and should be not less than 300000;
It is appropriate that the ethyl ρ-methoxy cinnamate reference substance is got in the preparation of object of reference solution, accurately weighed, adds methyl alcohol and make every 0.8ml and contain the solution of 0.25mg;
Pharmaceutical composition 0.7g of the present invention is got in the preparation of need testing solution, and porphyrize is put in the 15ml volumetric flask, adds methyl alcohol, power is 240W, and frequency is the ultrasonic processing of 55kHz 7 minutes, lets cool, and is settled to scale, shake up, 4000 rev/mins centrifugal, centrifugal 6 minutes, gets supernatant;
Determination method is accurate object of reference solution and each 1 μ l of need testing solution of drawing respectively, and the injection gas chromatography view, measure, and records chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, present 10 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.
10 specific features peaks corresponding with reference fingerprint that present in described coronary disease seven flavor dripping pill finger-prints are: No. 3 peaks, No. 4 peaks and No. 6 peaks are the composition in dalbergia wood; No. 1 peak, No. 2 peaks, No. 5 peaks, No. 7 peaks and No. 10 peaks are the composition in nutmeg; No. 9 peaks are the composition in kaempferia galamga; No. 8 peaks are the composition in santal.
Red sage root 50g santal 3g dalbergia wood 11g Kaempferia galanga 4g
Nutmeg 18g fructus choerospondiatis 8g sea-buckthorn 18g
Santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 3 hours with 9 times of water gagings, and the another device of the aqueous solution after distillation is collected; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor medicinal materials extract 3 times with 7 times of amount 90% alcohol refluxs, each 1.3 hours, filter, collect filtrate, the dregs of a decoction decoct 1 time with 5 times of water gagings, each 1.5 hours, filter, collect filtrate, relative density is 1.30～1.40 thick paste during concentrated each extract to 60 ℃ respectively, merge above-mentioned aqueous solution and filtrate, 110 ℃ of drying under reduced pressure, be ground into fine powder, obtain extract powder, add the PEG400 of volatile oil, 9g, the Macrogol 4000 of 30g,, take dimethyl silicon oil as cooling medium, make dripping pill.
Detection method
Chromatographic condition and system suitability are take Aiglent Innowax 30m * 0.32mm * 0.5 μ m as chromatographic column, and nitrogen buffer gas, detecting device are flame ionization ditector, and injector temperature is 300 ℃, and detector temperature is 200 ℃; Nitrogen flow rate is 3ml/min, and hydrogen flow rate is 30ml/min, and air velocity is 400ml/min; Column temperature is temperature programme, and initial temperature is 70 ℃, with the speed of 2.5 ℃/minute, is warming up to 180 ℃, kept 12 minutes, and split ratio 1: 1, direct injected, number of theoretical plate is pressed the ethyl ρ-methoxy cinnamate peak and is calculated, and should be not less than 300000;
It is appropriate that the ethyl ρ-methoxy cinnamate reference substance is got in the preparation of object of reference solution, accurately weighed, adds methyl alcohol and make every 1.2ml and contain the solution of 0.15mg;
Pharmaceutical composition 1.3 weight portions of the present invention are got in the preparation of need testing solution, and porphyrize is put in 5 parts by volume volumetric flasks, adds methyl alcohol, power is 320W, and frequency is the ultrasonic processing of 30kHz 13 minutes, lets cool, and is settled to scale, shake up, 6000 rev/mins centrifugal, centrifugal 4 minutes, gets supernatant;
Determination method is accurate object of reference solution and each 3 μ l of need testing solution of drawing respectively, and the injection gas chromatography view, measure, and records chromatogram;
Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, present 10 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.
10 specific features peaks corresponding with reference fingerprint that present in described coronary disease seven flavor dripping pill finger-prints are: No. 3 peaks, No. 4 peaks and No. 6 peaks are the composition in dalbergia wood; No. 1 peak, No. 2 peaks, No. 5 peaks, No. 7 peaks and No. 10 peaks are the composition in nutmeg; No. 9 peaks are the composition in kaempferia galamga; No. 8 peaks are the composition in santal.
Claims (13)
1. the fingerprint atlas detection method of volatile ingredient in a coronary disease seven flavor dripping pills, it is characterized in that the method comprises the steps: that chromatographic condition and system suitability are take Aiglent Innowax 30m * 0.32mm * 0.5 μ m as chromatographic column, nitrogen buffer gas, detecting device is flame ionization ditector, injector temperature is 150-350 ℃, and detector temperature is 150-350 ℃; Nitrogen flow rate is 1-3ml/min, and hydrogen flow rate is 25-45ml/min, and air velocity is 250-450ml/min; Column temperature is temperature programme, and initial temperature is 50-150 ℃, with the speed of 1-3 ℃/minute, is warming up to 150-290 ℃, keeps 5-15 minute, split ratio 1: 1, and direct injected, number of theoretical plate is pressed the ethyl ρ-methoxy cinnamate peak and is calculated, and should be not less than 300000; It is appropriate that the ethyl ρ-methoxy cinnamate reference substance is got in the preparation of object of reference solution, accurately weighed, adds methyl alcohol and make every 1ml and contain the solution of 0.1-0.3mg; The preparation of the need testing solution compositions 0.5-1.5 weight portion of getting it filled, porphyrize, put in 5-15 parts by volume volumetric flask, adds methyl alcohol, power is 220-340W, frequency is the ultrasonic processing of 20-60kHz 5-15 minute, lets cool, and is settled to scale, shake up, 3000-7000 rev/min centrifugal, and centrifugal 3-7 minute, get supernatant; Determination method is accurate object of reference solution and each 1-3 μ l of need testing solution of drawing respectively, and the injection gas chromatography view, measure, and records chromatogram; Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, present 10 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 fingerprint atlas detection method of volatile ingredient in coronary disease as claimed in claim 1 seven flavor dripping pills, it is characterized in that the method comprises the steps: that chromatographic condition and system suitability are take Aiglent Innowax 30m * 0.32mm * 0.5 μ m as chromatographic column, nitrogen buffer gas, detecting device is flame ionization ditector, injector temperature is 250 ℃, and detector temperature is 250 ℃; Nitrogen flow rate is 2ml/min, and hydrogen flow rate is 35ml/min, and air velocity is 350ml/min; Column temperature is temperature programme, and initial temperature is 100 ℃, with the speed of 2 ℃/minute, is warming up to 220 ℃, kept 10 minutes, and split ratio 1: 1, direct injected, number of theoretical plate is pressed the ethyl ρ-methoxy cinnamate peak and is calculated, and should be not less than 300000; It is appropriate that the ethyl ρ-methoxy cinnamate reference substance is got in the preparation of object of reference solution, accurately weighed, adds methyl alcohol and make every 1ml and contain the solution of 0.2mg; The preparation of need testing solution compositions 1.0 weight portions of getting it filled, porphyrize, put in 10 parts by volume volumetric flasks, adds appropriate methyl alcohol, and power is 280W, frequency is 40kHz, and ultrasonic processing 10 minutes, let cool, and is settled to scale, shake up, 5000 rev/mins centrifugal, centrifugal 5 minutes, gets supernatant; Determination method is accurate object of reference solution and each 2 μ l of need testing solution of drawing respectively, and the injection gas chromatography view, measure, and records chromatogram; Test sample finger-print and reference fingerprint are compared, in the test sample chromatogram, should present 10 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 fingerprint atlas detection method of volatile ingredient in coronary disease as claimed in claim 1 or 2 seven flavor dripping pills, it is characterized in that 10 specific features peaks corresponding with reference fingerprint that present in these coronary disease seven flavor dripping pill finger-prints are: No. 1 peak: relative retention time 0.192-0.235 accounts for the Area Ratio 64.59%-134.16% with reference to peak; No. 2 peak: relative retention time 0.371-0.454, account for the Area Ratio 1.90%-36.14% with reference to peak; No. 3 peak: relative retention time 0.448-0.548, account for the Area Ratio 30.59%-71.38% with reference to peak; No. 4 peak: relative retention time 0.468-0.572, account for the Area Ratio 38.76%-90.44% with reference to peak; No. 5 peak: relative retention time 0.477-0.584, account for the Area Ratio 43.68%-101.93% with reference to peak; No. 6 peak: relative retention time 0.497-0.607, account for the Area Ratio 86.70%-202.31% with reference to peak; No. 7 peak: relative retention time 0.655-0.800, account for the Area Ratio 92.25%-191.59% with reference to peak; No. 8 peak: relative retention time 0.822-1.004, account for the Area Ratio 2.99%-56.78% with reference to peak; No. 9 peaks: be the reference peak; No. 10 peak: relative retention time 0.956-1.169, account for the Area Ratio 161.06%-299.11% with reference to peak; No. 3 peaks, No. 4 peaks and No. 6 peaks are the composition in dalbergia wood; No. 1 peak, No. 2 peaks, No. 5 peaks, No. 7 peaks and No. 10 peaks are the composition in nutmeg; No. 9 peaks are the composition in kaempferia galamga; No. 8 peaks are the composition in santal.
4. the fingerprint atlas detection method of volatile ingredient in coronary disease as claimed in claim 3 seven flavor dripping pills, it is characterized in that described 10 with the relative retention time at reference fingerprint characteristic of correspondence peak and the Area Ratio that accounts for reference to peak are: No. 1 peak: relative retention time 0.192-0.235 accounts for the Area Ratio 80.59%-120.16% with reference to peak; No. 2 peak: relative retention time 0.371-0.454, account for the Area Ratio 10.90%-25.14% with reference to peak; No. 3 peak: relative retention time 0.448-0.548, account for the Area Ratio 40.59%-60.38% with reference to peak; No. 4 peak: relative retention time 0.468-0.572, account for the Area Ratio 50.76%-75.44% with reference to peak; No. 5 peak: relative retention time 0.477-0.584, account for the Area Ratio 60.68%-80.93% with reference to peak; No. 6 peak: relative retention time 0.497-0.607, account for the Area Ratio 120.70%-170.31% with reference to peak; No. 7 peak: relative retention time 0.655-0.800, account for the Area Ratio 120.25%-170.59% with reference to peak; No. 8 peak: relative retention time 0.822-1.004, account for the Area Ratio 15.99%-30.78% with reference to peak; No. 9 peaks: be the reference peak; No. 10 peak: relative retention time 0.956-1.169, account for the Area Ratio 190.06%-250.11% with reference to peak.
5. the fingerprint atlas detection method of volatile ingredient in coronary disease as claimed in claim 3 seven flavor dripping pills, it is characterized in that described 10 with the relative retention time at reference fingerprint characteristic of correspondence peak and the Area Ratio that accounts for reference to peak are: No. 1 peak: relative retention time 0.213 accounts for the Area Ratio 99.38% with reference to peak; No. 2 peaks: relative retention time 0.412 accounts for the Area Ratio 19.02% with reference to peak; No. 3 peaks: relative retention time 0.498 accounts for the Area Ratio 50.99% with reference to peak; No. 4 peaks: relative retention time 0.520 accounts for the Area Ratio 64.60% with reference to peak; No. 5 peaks: relative retention time 0.530 accounts for the Area Ratio 72.80% with reference to peak; No. 6 peaks: relative retention time 0.552 accounts for the Area Ratio 144.51% with reference to peak; No. 7 peaks: relative retention time 0.727 accounts for the Area Ratio 141.92% with reference to peak; No. 8 peaks: relative retention time 0.913 accounts for the Area Ratio 29.88% with reference to peak; No. 9 peaks: be the reference peak; No. 10 peaks: relative retention time 1.062 accounts for the Area Ratio 230.08% with reference to peak.
6., as the fingerprint atlas detection method of volatile ingredient in claim 1,2,4 or 5 described coronary disease seven flavor dripping pills, 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 fingerprint atlas detection method of volatile ingredient in coronary disease seven flavor dripping pills 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 fingerprint atlas detection method of volatile ingredient in coronary disease seven flavor dripping pills 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 santal 4.3 weight portion dalbergia wood 8.5 weight portion Kaempferia galanga 6.4 weight portion nutmeg 12.8 weight portion fructus choerospondiatis 12.8 weight portion sea-buckthorn 12.8 weight portions; Or the red sage root 21 weight portion santal 6 weight portion dalbergia wood 6 weight portion Kaempferia galanga 8 weight portion nutmeg 8 weight portion fructus choerospondiatis 18 weight portion sea-buckthorn 8 weight portions; Or the red sage root 50 weight portion santal 3 weight portion dalbergia wood 11 weight portion Kaempferia galanga 4 weight portion nutmeg 18 weight portion fructus choerospondiatis 8 weight portion sea-buckthorn 18 weight portions.
9. the fingerprint atlas detection method of volatile ingredient in coronary disease seven flavor dripping pills 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 santal 4.3 weight portion dalbergia wood 8.5 weight portion Kaempferia galanga 6.4 weight portion nutmeg 12.8 weight portion fructus choerospondiatis 12.8 weight portion sea-buckthorn 12.8 weight portions; Or the red sage root 21 weight portion santal 6 weight portion dalbergia wood 6 weight portion Kaempferia galanga 8 weight portion nutmeg 8 weight portion fructus choerospondiatis 18 weight portion sea-buckthorn 8 weight portions; Or the red sage root 50 weight portion santal 3 weight portion dalbergia wood 11 weight portion Kaempferia galanga 4 weight portion nutmeg 18 weight portion fructus choerospondiatis 8 weight portion sea-buckthorn 18 weight portions.
10. the fingerprint atlas detection method of volatile ingredient in coronary disease as claimed in claim 6 seven flavor dripping pills, it is characterized in that described coronary disease seven flavor dripping pills make by the following method: santal, dalbergia wood, Kaempferia galanga, nutmeg are extracted volatile oil 2-8 hour with 5-10 times of water gaging, and the another device of the aqueous solution after distillation is 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 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, relative density is 1.30～1.40 thick paste 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 15-35 weight portion, take dimethyl silicon oil as cooling medium, make dripping pill.
11. the fingerprint atlas detection method of volatile ingredient in coronary disease seven flavor dripping pills as described in one of claim 7-9, it is characterized in that described coronary disease seven flavor dripping pills make by the following method: santal, dalbergia wood, Kaempferia galanga, nutmeg are extracted volatile oil 2-8 hour with 5-10 times of water gaging, and the another device of the aqueous solution after distillation is 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 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, relative density is 1.30～1.40 thick paste 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 15-35 weight portion, take dimethyl silicon oil as cooling medium, make dripping pill.
12. the fingerprint atlas detection method of volatile ingredient in coronary disease seven flavor dripping pills as claimed in claim 10, it is characterized in that described coronary disease seven flavor dripping pills make by the following method: santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 5 hours with 7.8 times of water gagings, the another device collection of the aqueous solution after distillation; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor 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, relative density is 1.30～1.40 thick paste during concentrated each extract to 60 ℃ respectively, merge each thick paste, 80 ℃ of drying under reduced pressure, be 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.
13. the fingerprint atlas detection method of volatile ingredient in coronary disease seven flavor dripping pills as claimed in claim 11, it is characterized in that described coronary disease seven flavor dripping pills make by the following method: santal, dalbergia wood, Kaempferia galanga, nutmeg were extracted volatile oil 5 hours with 7.8 times of water gagings, the another device collection of the aqueous solution after distillation; The dregs of a decoction and all the other reds sage root, fructus choerospondiatis, sea-buckthorn three flavor 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, relative density is 1.30～1.40 thick paste during concentrated each extract to 60 ℃ respectively, merge each thick paste, 80 ℃ of drying under reduced pressure, be 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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| JP3028300B2 (en) * | 1996-09-18 | 2000-04-04 | 現代自動車株式会社 | Warning device when vehicle is overloaded |
| CN1616021A (en) * | 2004-09-15 | 2005-05-18 | 张平 | Chinese medicine drippling pill for treating coronary heart disease and its preparing method |
| CN101181589A (en) * | 2007-11-23 | 2008-05-21 | 包头中药有限责任公司 | Method for detecting the mass of tsunematsu 8-flavour agilawood tambac tablet |
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