CN1857380A - Method for detecting medicine material astragalus quality - Google Patents
Method for detecting medicine material astragalus quality Download PDFInfo
- Publication number
- CN1857380A CN1857380A CN 200610065283 CN200610065283A CN1857380A CN 1857380 A CN1857380 A CN 1857380A CN 200610065283 CN200610065283 CN 200610065283 CN 200610065283 A CN200610065283 A CN 200610065283A CN 1857380 A CN1857380 A CN 1857380A
- Authority
- CN
- China
- Prior art keywords
- peak
- finger
- finger printing
- peaks
- minutes
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Dairy Products (AREA)
Abstract
The present invention discloses the fingerprint method for detecting the quality of astragalus medicine material and its extract. The fingerprint method includes: adopting octodecyl silane bonded silicon gel as filler, acetoitrile-water as flow phase for gradient elution and astragalin A dissolved in methanol as contrast; taking detected astragalus sample through crushing astragalus root, methanol extracting and other steps; detecting the astragalus sample in high efficiency liquid phase chromatographic process to obtain the fingerprint of the detected astragalus sample; and comparing the fingerprint of the detected astragalus sample and the standard fingerprint for similarity degree over 0.90.
Description
Technical field
The present invention relates to a kind of quality determining method of Chinese crude drug, particularly the finger print quality detecting method of Milkvetch Root and extract thereof.
Background technology
Chinese medicine fingerprint is meant that a kind of Chinese crude drug or Chinese patent medicine are common, has the chromatograph or the spectrographic collection of illustrative plates of the distinctive element of the first species.Fingerprint pattern technology is a key means of estimating Chinese medicine quality, helps the modernization of Chinese medicine.States such as Japan, the U.S., Germany, France have successively brought into use finger printing that natural drug is carried out quality control, can effectively control the quality of medicine, guarantee the safe and effective of medicine, are known together by international at present.Today, some pharmacy corporations of China have carried out finger printing research to some tcm products under the advocating of country.Yet, now less for the research of Milkvetch Root and extract finger printing thereof.Radix Astragali crude drug and extract thereof also need be set up finger print quality detecting method.
Summary of the invention
The object of the invention is to provide the quality determining method of a kind of Milkvetch Root and extract Radix Astragali saponin thereof.
The present invention seeks to be achieved through the following technical solutions.
The finger print quality detecting method of Milkvetch Root of the present invention, this method comprises the steps:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With the ratio of acetonitrile-water is 0.1～0.5: 1 as mobile phase, and carry out gradient elution: 0 to 20 minute, acetonitrile concentration was 10～30%, continue after 15 minutes, acetonitrile concentration from 10～30% to 30～40%, 30～40% acetonitrile concentrations are maintained until 60 minutes; Flow velocity 0.5～1.0ml/min; 20～40 ℃ of column temperatures; Detector is an evaporative light scattering detector, 95～125 ℃ of drift tube temperatures, gas flow rate 2.5～3.2SLPM; With reference to the preparation of product solution, it is an amount of that precision takes by weighing the astragaloside reference substance, adds dissolve with methanol and make the solution that every 1ml contains 0.5mg, as reference product solution; The preparation of need testing solution, it is an amount of to get Milkvetch Root, pulverizes, get 1.5g, the accurate title, decide, and puts in the apparatus,Soxhlet's, add methanol 50～200ml, refluxed 2～8 hours, put cold, filter, filtrate is reclaimed methanol to doing, and residue adds water 20ml makes dissolving, extract 2～5 times with water saturated n-butyl alcohol jolting, each 10～40ml merges n-butanol extracting liquid, extracts 1～4 time with ammonia solution, each 5～30ml, discard ammonia solution, n-butyl alcohol liquid evaporate to dryness, residue is with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol and be diluted to scale, shake up,, get subsequent filtrate and detect test liquid as the Milkvetch Root finger printing with the microporous filter membrane filtration of 0.45 μ m; The test liquid finger printing detects, and with high performance liquid chromatography the Milkvetch Root finger printing is detected test liquid and detects, and sample size is 5～50 μ l, writes down 60 minutes chromatogram, gets the finger printing of Milkvetch Root; The test sample finger printing should should be greater than 0.90 with the standard finger-print similarity; The Milkvetch Root finger printing has 7 total fingerprint peakses, with reference to peak S is the astragaloside chromatographic peak, the relative retention time of 7 total fingerprint peakses is respectively: No. 1 peak 0.387 ± 0.039, No. 2 peaks 0.802 ± 0.080,0.875 ± 0.088, No. 5 peaks 0.909 ± 0.091,0.852 ± 0.085, No. 4 peaks, No. 3 peaks, 1.000 ± 0.000, No. 6 peaks 1.030 ± 0.010, S peak.
The finger print quality detecting method of Milkvetch Root of the present invention is preferably as follows detection method:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-water=0.23: 1 is a mobile phase, and carry out gradient elution: 0 to 20 minute, acetonitrile concentration was 23%, continue after 15 minutes, acetonitrile concentration from 23% to 35%, 35% acetonitrile concentration is maintained until 60 minutes; Flow velocity 0.7ml/min; 35 ℃ of column temperatures; Detector is an evaporative light scattering detector, 105 ℃ of drift tube temperatures, gas flow rate 2.95SLPM; With reference to the preparation of product solution, it is an amount of that precision takes by weighing the astragaloside reference substance, adds dissolve with methanol and make the solution that every 1ml contains 0.5mg, as reference product solution; The preparation of need testing solution, it is an amount of to get Milkvetch Root, pulverizes, get 1.5g, the accurate title, decide, and puts in the apparatus,Soxhlet's, add methanol 120ml, refluxed 6 hours, put cold, filter, filtrate is reclaimed methanol to doing, and residue adds water 20ml makes dissolving, extract 3 times with water saturated n-butyl alcohol jolting, each 15ml merges n-butanol extracting liquid, extracts 2 times with ammonia solution, each 15ml, discard ammonia solution, n-butyl alcohol liquid evaporate to dryness, residue is with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol and be diluted to scale, shake up,, get subsequent filtrate and detect test liquid as the Milkvetch Root finger printing with the microporous filter membrane filtration of 0.45 μ m; The test liquid finger printing detects, and with high performance liquid chromatography the Milkvetch Root finger printing is detected test liquid and detects, and sample size is 20 μ l, writes down 60 minutes chromatogram, gets the finger printing of Milkvetch Root; The test sample finger printing should should be greater than 0.90 with the standard finger-print similarity; The Milkvetch Root finger printing has 7 total fingerprint peakses, is the astragaloside chromatographic peak with reference to peak S, and the preferred relative retention time of 7 total fingerprint peakses is respectively: No. 1 peak 0.387,0.852, No. 4 peak 0.875,0.802, No. 3 peak, No. 2 peaks, No. 5 peaks 0.909,1.000, No. 6 peaks 1.030, S peak; 0.788, No. 5 peak 0.999,0.936, No. 4 peak, 0.723, No. 3 peak, 0.425, No. 2 peak, No. 1 peak, 1.000, No. 6 peaks 1.021, S peak or 0.962, No. 5 peak 0.909 ± 0.819,0.768, No. 4 peak, 0.881, No. 3 peak, 0.349, No. 2 peak, No. 1 peak, 1.000, No. 6 peaks 1.039, S peak.
The quality determining method of the finger printing of the extract Radix Astragali saponin in the Milkvetch Root, this method comprises the steps:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With the acetonitrile-water ratio is 0.1～0.5: 1 as mobile phase, and carry out gradient elution: 0 to 20 minute, acetonitrile concentration was 10～30%, continue after 15 minutes, acetonitrile concentration from 10～30% to 30～40%, 30～40% acetonitrile concentrations are maintained until 60 minutes; Flow velocity 0.5～1.0ml/min; 20～40 ℃ of column temperatures; Detector is an evaporative light scattering detector, 95～125 ℃ of drift tube temperatures, gas flow rate 2.5～3.2SLPM; With reference to the preparation of product solution, it is an amount of that precision takes by weighing the astragaloside reference substance, adds dissolve with methanol and make the solution that every 1ml contains 0.5mg, as reference product solution; Radix Astragali saponin 20mg is got in the preparation of need testing solution, and accurate the title decides, and puts in the 5ml measuring bottle, adds dissolve with methanol and is diluted to scale, shakes up; Microporous filter membrane with 0.45 μ m filters, and gets subsequent filtrate, promptly; The test liquid finger printing detects, and with high performance liquid chromatography the Radix Astragali saponin finger printing is detected test liquid and detects, and sample size is 5～50 μ l, writes down 60 minutes chromatogram, gets the finger printing of Radix Astragali saponin; The test sample finger printing should should be greater than 0.90 with the standard finger-print similarity; The Radix Astragali saponin finger printing has 6 total fingerprint peakses, with reference to peak S is the astragaloside chromatographic peak, the relative retention time of 6 total fingerprint peakses is respectively: No. 1 peak 0.797 ± 0.080, No. 2 peaks 0.847 ± 0.085, No. 3 peaks 0.870 ± 0.087, No. 4 peaks 0.905 ± 0.090,1.000 ± 0.000, No. 5 peaks 1.029 ± 0.010, S peak.
The finger print quality detecting method of Radix Astragali saponin is preferably as follows detection method:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With the ratio of acetonitrile-water be 0.23: 1 as mobile phase, carry out gradient elution: 0 to 20 minute, acetonitrile concentration was 23%, continue after 15 minutes, acetonitrile concentration from 23% to 35%, 35% acetonitrile concentration is maintained until 60 minutes; Flow velocity 0.7ml/min; 35 ℃ of column temperatures; Detector is an evaporative light scattering detector, 105 ℃ of drift tube temperatures, gas flow rate 2.95SLPM; With reference to the preparation of product solution, it is an amount of that precision takes by weighing the astragaloside reference substance, adds dissolve with methanol and make the solution that every 1ml contains 0.5mg, as reference product solution; Radix Astragali saponin 20mg is got in the preparation of need testing solution, and accurate the title decides, and puts in the 5ml measuring bottle, adds dissolve with methanol and is diluted to scale, shakes up; Microporous filter membrane with 0.45 μ m filters, and gets subsequent filtrate, promptly; The test liquid finger printing detects, and with high performance liquid chromatography the Radix Astragali saponin finger printing is detected test liquid and detects, and sample size is 20 μ l, writes down 60 minutes chromatogram, gets the finger printing of Radix Astragali saponin; The test sample finger printing should should be greater than 0.90 with the standard finger-print similarity; The Radix Astragali saponin finger printing has 6 total fingerprint peakses, is the astragaloside chromatographic peak with reference to peak S, and the preferred relative retention time of 6 total fingerprint peakses is respectively: No. 1 peak 0.797,0.870, No. 4 peak 0.905,0.847, No. 3 peak, No. 2 peaks, 1.000, No. 5 peaks 1.029, S peak; 0.956, No. 4 peak 0.994,0.931, No. 3 peak, 0.876, No. 2 peak, No. 1 peak, 0.784, No. 4 peak 0.816 in 1.000, No. 5 peaks 1.038, S peak or 0.763, No. 3 peak, 0.718, No. 2 peak, No. 1 peak, 1.000, No. 5 peaks 1.020, S peak.
The present invention uses fingerprint pattern technology effectively to control the quality of Milkvetch Root and Radix Astragali saponin thereof; The present invention uses fingerprint pattern technology to begin raw material is effectively controlled from Milkvetch Root, guaranteed under certain preparation technology's situation, gained Radix Astragali saponin steady quality, thus the quality of preparations such as radix astragali saponin injection, astragalus root saponin can further effectively be controlled; Fingerprint pattern technology provided by the invention can be used as the key means of estimating Chinese medicine quality, helps the modernization of Chinese medicine.
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
Determining of the total peak of experimental example 1 Milkvetch Root finger printing
1. finger printing
According to 10 batches of given relevant parameters of test sample HPLC collection of illustrative plates, the main chromatographic peak that Milkvetch Root is measured gained by aforementioned preparation method all occurred in 60 minutes; 2 hours need testing solution chromatogram shows 60 minutes and does not occur chromatographic peak later on.Relatively the chromatogram of each batch sample finds that it is that each batch is total that 7 peaks are arranged, and sets up standard finger-print thus.
2. the demarcation of total fingerprint peaks
Result of calculation according to 10 batches of test sample finger printing relevant datas, the average relative retention time in total peak (peak number) is followed successively by 0.387 (1), 0.802 (2), 0.852 (3), 0.875 (4), 0.909 (5), 1.000 (S), 1.030 (6), as the foundation that total fingerprint peaks is demarcated, allowing relative deviation is ± 10% with this.
3. total fingerprint peaks relative retention time
The relative retention time table 1 of total fingerprint peaks in the 10 batches of test sample finger printing.
Table 1 Milkvetch Root has fingerprint peaks relative retention time (n=10)
| Total peak-to-peak number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | On average | RSD(％) |
| 1 2 3 4 5 S 6 | 0.387 0.802 0.853 0.877 0.910 1.000 1.031 | 0.388 0.803 0.854 0.877 0.910 1.000 1.030 | 0.387 0.801 0.852 0.876 0.909 1.000 1.030 | 0.388 0.801 0.852 0.875 0.908 1.000 1.029 | 0.388 0.802 0.852 0.876 0.909 1.000 1.029 | 0.387 0.802 0.853 0.876 0.909 1.000 1.029 | 0.388 0.802 0.851 0.874 0.907 1.000 1.030 | 0.387 0.801 0.852 0.875 0.909 1.000 1.030 | 0.386 0.800 0.851 0.874 0.908 1.000 1.029 | 0.386 0.801 0.852 0.876 0.909 1.000 1.030 | 0.387 0.802 0.852 0.875 0.909 1.000 1.030 | 0.21 0.10 0.11 0.12 0.09 0.00 0.06 |
The RSD of the relative retention time at 10 batches of total peaks of medical material shows that all less than 2% the concordance of each batch sample is better.
4. non-total peak area
Remove the peak that keeps without post, the non-total peak gross area that has calculated 10 batch samples accounts for the ratio of total peak area, the results are shown in Table 2.
The non-total peak gross area of table 2 Radix Astragali sample accounts for the percentage ratio (n=10) of total peak area
| Sample number into spectrum | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | On average |
| Proportion % | 0.70 | 2.30 | 0.53 | 0.62 | 8.88 | 1.05 | 2.72 | 0.93 | 4.72 | 0.80 | 2.33 |
The ratio that the non-total peak of each batch medical material gross area accounts for the gross area meets the regulation of " specification requirement (provisional) of Chinese medicine finger printing research " all less than 10%.
5, Milkvetch Root finger printing similarity evaluation
Get ten batches of Milkvetch Roots, detect as stated above, draw the finger printing of ten batch samples, the area of computer aided similarity evaluation software (Central South University's modernization of cmm center establishment) that adopts Chinese Pharmacopoeia committee to recommend calculates, and similarity sees Table 3.
Table 3
| Lot number | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Similarity | 0.994 | 0.996 | 0.992 | 0.988 | 0.996 | 0.992 | 0.986 | 0.982 | 0.978 | 0.998 |
Determining of the total peak of experimental example 2 Radix Astragali saponin finger printing
1, finger printing
According to 3 batches of given relevant parameters of test sample HPLC collection of illustrative plates, the main chromatographic peak that Radix Astragali saponin is measured gained by aforementioned preparation method all occurred in 60 minutes; 2 hours need testing solution chromatogram shows 60 minutes and does not occur chromatographic peak later on.Relatively the chromatographic peak of each batch sample finds that wherein 6 peaks are that each batch is total, sets up standard finger-print thus.
2, the demarcation of total fingerprint peaks
Result of calculation according to 3 batches of test sample finger printing relevant datas, each average relative retention time in total peak (peak number) is followed successively by 0.797 (1), 0.847 (2), 0.870 (3), 0.905 (4), 1.000 (S), 1.029 (5), as the foundation that total fingerprint peaks is demarcated, allowing relative deviation is ± 10% with this.
3, total fingerprint peaks relative retention time
Total fingerprint peaks relative retention time table 4 in 3 batches of test sample finger printing.
Table 4 Radix Astragali saponin has fingerprint peaks relative retention time (n=3)
| Total peak-to-peak number | 1 | 2 | 3 | On average | RSD(％) |
| 1 2 3 4 S 5 | 0.798 0.849 0.872 0.906 1.000 1.029 | 0.796 0.847 0.870 0.905 1.000 1.029 | 0.796 0.847 0.870 0.905 1.000 1.030 | 0.797 0.847 0.870 0.905 1.000 1.029 | 0.11 0.13 0.12 0.07 0.00 0.03 |
By above result as can be seen, the relative standard deviation of total peak relative retention time is less than 1%, and concordance is very good.
4, non-total peak area
Remove the peak that keeps without post, the non-total peak gross area that has calculated 3 batch samples accounts for the ratio of total peak area, the results are shown in Table 5.
The non-total peak gross area of table 5 Radix Astragali saponin sample accounts for the percentage ratio (n=3) of total peak area
| Sample number into spectrum | 1 | 2 | 3 | On average |
| Proportion (%) | 4.26 | 2.01 | 1.73 | 2.7 |
The ratio that the non-total peak of each batch intermediate gross area accounts for total peak area meets the regulation of " specification requirement (provisional) of Chinese medicine finger printing research " all less than 5%.
5, Radix Astragali saponin finger printing similarity evaluation
Get three batches of Radix Astragali saponins, detect as stated above, draw the finger printing of three batch samples, the area of computer aided similarity evaluation software (Central South University's modernization of cmm center establishment) that adopts Chinese Pharmacopoeia committee to recommend calculates, and similarity sees Table 6.
Table 6
| Lot number | 1 | 2 | 3 |
| Similarity | 0.995 | 0.992 | 0.993 |
Experimental example 3 Radix Astragali need testing solution stability tests
Getting Radix Astragali need testing solution of the present invention is determination object, the same day, second day, the 4th day measured (4 ℃ of preservations) in preparation respectively according to aforementioned chromatographic condition, write down each total chromatographic peak retention time and peak area, retention time with the object of reference astragaloside is reference, converse the ratio of the relative retention time at each total peak, as a result table 1～2.The result shows the relative standard deviation of each total peak relative retention time less than 2%, and is very stable; With reference to the relative standard deviation of peak-to-peak area percentage less than 2%.Above result shows that need testing solution is stable in 4 days.See Table 7 and 8.
Table 7 stability test relative retention time
| Total peak numbering | 0 day | 2 days | 4 days | On average | RSD(％) |
| 1 2 3 4 5 S 6 | 0.386 0.801 0.852 0.876 0.909 1.000 1.030 | 0.384 0.799 0.849 0.873 0.908 1.000 1.030 | 0.391 0.796 0.846 0.870 0.905 1.000 1.030 | 0.387 0.798 0.849 0.873 0.907 1.000 1.030 | 1.00 0.35 0.38 0.33 0.20 0.00 0.03 |
Table 8 stability test accounts for total peak area percentage ratio with reference to the peak
| Experimental period | 0 day | 2 days | 4 days | On average | RSD(％) |
| Peak area % | 88.594 | 90.610 | 88.891 | 89.36 | 1.2 |
The test of experimental example 4 Radix Astragali finger printing repeatability
Get 5 parts of Radix Astragali test samples of the present invention, according to the method formation determination of experimental example 3, write down each total chromatographic peak retention time and integration peak area, be reference with the retention time of object of reference astragaloside, converse the ratio of the relative retention time at each total peak, statistical result sees the following form 9 and 10.
Table 9 repeatability relative retention time (n=5)
| Total peak numbering | 1 | 2 | 3 | 4 | 5 | On average | RSD(％) |
| 1 2 3 4 5 S 6 | 0.387 0.801 0.852 0.876 0.909 1.000 1.030 | 0.385 0.801 0.852 0.875 0.909 1.000 1.030 | 0.386 0.801 0.852 0.876 0.909 1.000 1.030 | 0.394 0.799 0.850 0.873 0.907 1.000 1.030 | 0.394 0.799 0.849 0.873 0.907 1.000 1.030 | 0.389 0.800 0.851 0.875 0.908 1.000 1.030 | 1.20 0.12 0.18 0.17 0.12 0.00 0.02 |
The test of table 10 precision accounts for total peak area percentage ratio with reference to the peak
| Experiment number | 1 | 2 | 3 | 4 | 5 | On average | RSD(％) |
| Peak area % | 88.831 | 89.994 | 89.450 | 93.209 | 90.503 | 90.40 | 1.9 |
Experimental result shows that the relative standard deviation of each total peak relative retention time is all less than 2%; Relative standard deviation with reference to the peak area percentage ratio at peak is 1.9%, and the repeatability of result presentation method is good.
Experimental example 5 Radix Astragali saponin need testing solution stability tests
Getting Radix Astragali saponin need testing solution of the present invention is determination object, the same day, second day, the 3rd day measures (4 ℃ of preservations) according to aforementioned chromatographic condition in preparation respectively, writes down each total chromatographic peak retention time and peak area.Retention time with the object of reference astragaloside is reference, converses the ratio of the relative retention time at each total peak, the results are shown in Table 5～6.The result shows the relative standard deviation of each total peak relative retention time less than 1%, and is very stable; Relative standard deviation with reference to the peak area percentage ratio at peak is 1.3%, and the result shows need testing solution kept stable in three days.
Table 11 stability test relative retention time
| Total peak numbering | 0 day | 2 days | 3 days | On average | RSD(％) |
| 1 2 3 4 S 5 | 0.796 0.846 0.869 0.904 1.000 1.029 | 0.798 0.849 0.872 0.906 1.000 1.029 | 0.798 0.849 0.872 0.906 1.000 1.029 | 0.797 0.848 0.871 0.905 1.000 1.029 | 0.18 0.19 0.16 0.11 0.00 0.03 |
Table 12 stability test accounts for total peak area percentage ratio with reference to the peak
| Experimental period | 0 day | 2 days | 3 days | On average | RSD(％) |
| Peak area % | 90.058 | 89.866 | 92.003 | 90.64 | 1.3 |
The test of experimental example 6 Radix Astragali saponin finger printing repeatability
Get 5 parts of Radix Astragali saponin test samples,, write down each total chromatographic peak retention time and integration peak area according to experimental example 5 described method formation determinations.Retention time with the object of reference astragaloside is reference, converses the relative retention time at each total peak, and statistical result sees Table 13 and 14.
Table 13 repeatability test relative retention time (n=5)
| Total peak numbering | 1 | 2 | 3 | 4 | 5 | On average | RSD(％) |
| 1 2 3 4 S 5 | 0.795 0.846 0.869 0.904 1.000 1.029 | 0.797 0.847 0.870 0.905 1.000 1.030 | 0.796 0.847 0.870 0.905 1.000 1.029 | 0.796 0.847 0.870 0.905 1.000 1.030 | 0.796 0.846 0.869 0.904 1.000 1.029 | 0.796 0.846 0.870 0905 1.000 1.030 | 0.06 0.07 0.06 0.04 0.00 0.04 |
The test of table 14 precision accounts for total peak area percentage ratio with reference to the peak
| Experiment number | 1 | 2 | 3 | 4 | 5 | On average | RSD(％) |
| Peak area % | 91.696 | 89.566 | 89.131 | 91.388 | 91.477 | 90.65 | 1.3 |
Experimental result shows that the relative standard deviation of each total peak relative retention time is all less than 1%; Relative standard deviation with reference to the peak area percentage ratio at peak is 1.3%, and the repeatability of result presentation method is good.
Description of drawings:
Fig. 1 is the Radix Astragali saponin standard finger-print;
Fig. 2 is the Milkvetch Root standard finger-print.
Following embodiment all can realize the described effect of above-mentioned experimental example.
Embodiment 1: the quality determining method of Milkvetch Root
Chromatographic condition and system suitability are filler with octadecylsilane chemically bonded silica; Acetonitrile-water is mobile phase, carries out gradient elution: 0 to 20 minute, acetonitrile concentration was 23%, continue after 15 minutes, acetonitrile concentration from 23% to 35%, 35% acetonitrile concentration is maintained until 60 minutes; Flow velocity 0.7ml/min; 35 ℃ of column temperatures; Detector is EISD, 105 ℃ of drift tube temperatures, gas flow rate 2.95SLPM.
With reference to the preparation of product solution, it is an amount of that precision takes by weighing the Astragaloside IV reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 0.5mg, and get final product.
The preparation of need testing solution, it is an amount of to get Milkvetch Root, pulverizes, cross sieve No. two, get 1.5g, accurately weighed, put in the apparatus,Soxhlet's, add methyl alcohol 120ml, refluxed 6 hours, let cool, filter, filtrate is reclaimed methyl alcohol to doing, residue adds water 20ml makes dissolving, extracts 3 times with water saturated n-butanol jolting, each 15ml, merge n-butanol extracting liquid, extract 2 times with ammonia solution, each 15ml discards ammonia solution, n-butanol liquid evaporate to dryness, residue dissolves with methyl alcohol and is transferred in the 5ml measuring bottle, adds methyl alcohol and is diluted to scale, shakes up, filter with the miillpore filter of 0.45 μ m, get subsequent filtrate and get final product; The test liquid finger-print detects, and with high performance liquid chromatography the Milkvetch Root finger-print is detected test liquid and detects, and sample size is 20 μ l, records 60 minutes chromatogram, gets the finger-print of Milkvetch Root.
Embodiment 2: the quality determining method of Milkvetch Root
Chromatographic condition and system suitability are filler with octadecylsilane chemically bonded silica; Acetonitrile-water is mobile phase, carries out gradient elution: 0 to 20 minute, acetonitrile concentration was 22%, continue after 15 minutes, acetonitrile concentration from 22% to 33%, 33% acetonitrile concentration is maintained until 60 minutes; Flow velocity 0.9ml/min; 25 ℃ of column temperatures; Detector is EISD, 120 ℃ of drift tube temperatures, gas flow rate 2.60SLPM; With reference to the preparation of product solution, it is an amount of that precision takes by weighing the Astragaloside IV reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 0.5mg, as reference product solution; The preparation of need testing solution, it is an amount of to get Milkvetch Root, pulverizes, get 1.5g, accurately weighed, put in the apparatus,Soxhlet's, add methyl alcohol 80ml, refluxed 3 hours, let cool, filter, filtrate is reclaimed methyl alcohol to doing, and residue adds water 20ml makes dissolving, extract 4 times with water saturated n-butanol jolting, each 35ml merges n-butanol extracting liquid, extracts 3 times with ammonia solution, each 25ml, discard ammonia solution, n-butanol liquid evaporate to dryness, residue dissolves with methyl alcohol and is transferred in the 5ml measuring bottle, add methyl alcohol and be diluted to scale, shake up, with the miillpore filter filtration of 0.45 μ m, get subsequent filtrate and detect test liquid as the Milkvetch Root finger-print; The test liquid finger-print detects, and with high performance liquid chromatography the Milkvetch Root finger-print is detected test liquid and detects, and sample size is 10 μ l, records 60 minutes chromatogram, gets the finger-print of Milkvetch Root; The test sample finger-print should should be greater than 0.90 with the standard finger-print similarity; The Milkvetch Root finger-print has 7 total fingerprint peakses, is the Astragaloside IV chromatographic peak with reference to peak S, and the relative retention time of 7 total fingerprint peakses is respectively: No. 1 peak 0.425,0.936, No. 4 peak 0.788,0.723, No. 3 peak, No. 2 peaks, No. 5 peaks 0.999,1.000, No. 6 peaks 1.021, S peak.
Embodiment 3: the quality determining method of Milkvetch Root
Chromatographic condition and system suitability are filler with octadecylsilane chemically bonded silica; Acetonitrile-water=0.23: 1 is mobile phase, and carry out gradient elution: 0 to 20 minute, acetonitrile concentration was 23%, continue after 15 minutes, acetonitrile concentration from 23% to 35%, 35% acetonitrile concentration is maintained until 60 minutes; Flow velocity 0.7ml/min; 35 ℃ of column temperatures; Detector is EISD, 105 ℃ of drift tube temperatures, gas flow rate 2.95SLPM; With reference to the preparation of product solution, it is an amount of that precision takes by weighing the Astragaloside IV reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 0.5mg, as reference product solution; The preparation of need testing solution, it is an amount of to get Milkvetch Root, pulverizes, get 1.5g, accurately weighed, put in the apparatus,Soxhlet's, add methyl alcohol 120ml, refluxed 6 hours, let cool, filter, filtrate is reclaimed methyl alcohol to doing, and residue adds water 20ml makes dissolving, extract 3 times with water saturated n-butanol jolting, each 15ml merges n-butanol extracting liquid, extracts 2 times with ammonia solution, each 15ml, discard ammonia solution, n-butanol liquid evaporate to dryness, residue dissolves with methyl alcohol and is transferred in the 5ml measuring bottle, add methyl alcohol and be diluted to scale, shake up, with the miillpore filter filtration of 0.45 μ m, get subsequent filtrate and detect test liquid as the Milkvetch Root finger-print; The test liquid finger-print detects, and with high performance liquid chromatography the Milkvetch Root finger-print is detected test liquid and detects, and sample size is 20 μ l, records 60 minutes chromatogram, gets the finger-print of Milkvetch Root; The test sample finger-print should should be greater than 0.90 with the standard finger-print similarity; The Milkvetch Root finger-print has 7 total fingerprint peakses, is the Astragaloside IV chromatographic peak with reference to peak S, and the relative retention time of 7 total fingerprint peakses is respectively: No. 1 peak 0.387,0.852, No. 4 peak 0.875,0.802, No. 3 peak, No. 2 peaks, No. 5 peaks 0.909,1.000, No. 6 peaks 1.030, S peak.
Embodiment 4: the quality determining method of Milkvetch Root
Chromatographic condition and system suitability are filler with octadecylsilane chemically bonded silica; Acetonitrile-water (0.12: 1) is mobile phase, carries out gradient elution: 0 to 20 minute, acetonitrile concentration was 12%, continue after 15 minutes, acetonitrile concentration from 12% to 39%, 39% acetonitrile concentration is maintained until 60 minutes; Flow velocity 0.6ml/min; 30 ℃ of column temperatures; Detector is EISD, 110 ℃ of drift tube temperatures, gas flow rate 3.10SLPM; With reference to the preparation of product solution, it is an amount of that precision takes by weighing the Astragaloside IV reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 0.5mg, as reference product solution; The preparation of need testing solution, it is an amount of to get Milkvetch Root, pulverizes, get 1.5g, accurately weighed, put in the apparatus,Soxhlet's, add methyl alcohol 190ml, refluxed 5 hours, let cool, filter, filtrate is reclaimed methyl alcohol to doing, and residue adds water 20ml makes dissolving, extract 5 times with water saturated n-butanol jolting, each 25ml merges n-butanol extracting liquid, extracts 4 times with ammonia solution, each 6ml, discard ammonia solution, n-butanol liquid evaporate to dryness, residue dissolves with methyl alcohol and is transferred in the 5ml measuring bottle, add methyl alcohol and be diluted to scale, shake up, with the miillpore filter filtration of 0.45 μ m, get subsequent filtrate and detect test liquid as the Milkvetch Root finger-print; The test liquid finger-print detects, and with high performance liquid chromatography the Milkvetch Root finger-print is detected test liquid and detects, and sample size is 48 μ l, records 60 minutes chromatogram, gets the finger-print of Milkvetch Root; The test sample finger-print should should be greater than 0.90 with the standard finger-print similarity; The Milkvetch Root finger-print has 7 total fingerprint peakses, is the Astragaloside IV chromatographic peak with reference to peak S, and the relative retention time of 7 total fingerprint peakses is respectively: No. 1 peak 0.349,0.768, No. 4 peak 0.962,0.881, No. 3 peak, No. 2 peaks, No. 5 peaks 0.909 ± 0.819,1.000, No. 6 peaks 1.039, S peak
Embodiment 5: the quality determining method of astragaloside
Chromatographic condition and system suitability are filler with octadecylsilane chemically bonded silica; Acetonitrile-water is mobile phase, carries out gradient elution: 0 to 20 minute, acetonitrile concentration was 23%, continue after 15 minutes, acetonitrile concentration from 23% to 35%, 35% acetonitrile concentration is maintained until 60 minutes; Flow velocity 0.7ml/min; 35 ℃ of column temperatures; Detector is EISD, 105 ℃ of drift tube temperatures, gas flow rate 2.95SLPM.
With reference to the preparation of product solution, it is an amount of that precision takes by weighing the Astragaloside IV reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 0.5mg, and get final product.
Astragaloside 20mg is got in the preparation of need testing solution, and is accurately weighed, puts in the 5ml measuring bottle, adds the methyl alcohol dissolving and is diluted to scale, shakes up; Miillpore filter with 0.45 μ m filters, and gets subsequent filtrate, and get final product; The test liquid finger-print detects, and with high performance liquid chromatography the astragaloside finger-print is detected test liquid and detects, and sample size is 20 μ l, records 60 minutes chromatogram, gets the finger-print of astragaloside.
Embodiment 6: the quality determining method of astragaloside
Chromatographic condition and system suitability are filler with octadecylsilane chemically bonded silica; Acetonitrile-water is mobile phase, gradient elution: 0 to 20 minute, acetonitrile concentration was 25%, continue after 15 minutes, acetonitrile concentration from 25% to 32%, 32% acetonitrile concentration is maintained until 60 minutes; Flow velocity 0.7ml/min; 35 ℃ of column temperatures; Detector is EISD, 115 ℃ of drift tube temperatures, gas flow rate 3.00SLPM.
With reference to the preparation of product solution, it is an amount of that precision takes by weighing the Astragaloside IV reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 0.5mg, and get final product.
Astragaloside 20mg is got in the preparation of need testing solution, and is accurately weighed, puts in the 5ml measuring bottle, adds the methyl alcohol dissolving and is diluted to scale, shakes up; Miillpore filter with 0.45 μ m filters, and gets subsequent filtrate, and get final product.
The test liquid finger-print detects, and with high performance liquid chromatography the astragaloside finger-print is detected test liquid and detects, and sample size is 10 μ l, records 60 minutes chromatogram, gets the finger-print of astragaloside; The test sample finger-print should should be greater than 0.90 with the standard finger-print similarity; The astragaloside finger-print has 6 total fingerprint peakses, is the Astragaloside IV chromatographic peak with reference to peak S, and the relative retention time of 6 total fingerprint peakses is respectively: No. 1 peak 0.876,0.956, No. 4 peak 0.994,0.931, No. 3 peak, No. 2 peaks, 1.000, No. 5 peaks 1.038, S peak.
Embodiment 7: the quality determining method of astragaloside
Chromatographic condition and system suitability are filler with octadecylsilane chemically bonded silica; Acetonitrile-water=0.23: 1 is mobile phase, and carry out gradient elution: 0 to 20 minute, acetonitrile concentration was 23%, continue after 15 minutes, acetonitrile concentration from 23% to 35%, 35% acetonitrile concentration is maintained until 60 minutes; Flow velocity 0.7ml/min; 35 ℃ of column temperatures; Detector is EISD, 105 ℃ of drift tube temperatures, gas flow rate 2.95SLPM; With reference to the preparation of product solution, it is an amount of that precision takes by weighing the Astragaloside IV reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 0.5mg, as reference product solution; Astragaloside 20mg is got in the preparation of need testing solution, and is accurately weighed, puts in the 5ml measuring bottle, adds the methyl alcohol dissolving and is diluted to scale, shakes up; Miillpore filter with 0.45 μ m filters, and gets subsequent filtrate, and get final product; The test liquid finger-print detects, and with high performance liquid chromatography the astragaloside finger-print is detected test liquid and detects, and sample size is 20 μ l, records 60 minutes chromatogram, gets the finger-print of astragaloside; The test sample finger-print should should be greater than 0.90 with the standard finger-print similarity; The astragaloside finger-print has 6 total fingerprint peakses, is the Astragaloside IV chromatographic peak with reference to peak S, and the relative retention time of 6 total fingerprint peakses is respectively: No. 1 peak 0.797,0.870, No. 4 peak 0.905,0.847, No. 3 peak, No. 2 peaks, 1.000, No. 5 peaks 1.029, S peak.
Embodiment 8: the quality determining method of astragaloside
Chromatographic condition and system suitability are filler with octadecylsilane chemically bonded silica; Acetonitrile-water (0.15: 1) is mobile phase, carries out gradient elution: 0 to 20 minute, acetonitrile concentration was 15%, continue after 15 minutes, acetonitrile concentration from 15% to 49%, 49% acetonitrile concentration is maintained until 60 minutes; Flow velocity 0.6ml/min; 25 ℃ of column temperatures; Detector is EISD, 120 ℃ of drift tube temperatures, gas flow rate 2.60SLPM; With reference to the preparation of product solution, it is an amount of that precision takes by weighing the Astragaloside IV reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 0.5mg, as reference product solution; Astragaloside 20mg is got in the preparation of need testing solution, and is accurately weighed, puts in the 5ml measuring bottle, adds the methyl alcohol dissolving and is diluted to scale, shakes up; Miillpore filter with 0.45 μ m filters, and gets subsequent filtrate, and get final product; The test liquid finger-print detects, and with high performance liquid chromatography the astragaloside finger-print is detected test liquid and detects, and sample size is 40 μ l, records 60 minutes chromatogram, gets the finger-print of astragaloside; The test sample finger-print should should be greater than 0.90 with the standard finger-print similarity; The astragaloside finger-print has 6 total fingerprint peakses, is the Astragaloside IV chromatographic peak with reference to peak S, and the relative retention time of 6 total fingerprint peakses is respectively: No. 1 peak 0.718,0.784, No. 4 peak 0.816,0.763, No. 3 peak, No. 2 peaks, 1.000, No. 5 peaks 1.020, S peak.
Claims (4)
1, a kind of graph-spectrum quality detection method of Milkvetch Root fingerprint is characterized in that this method comprises the steps:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With acetonitrile-water ratio is 0.1～0.5: 1 as mobile phase, and carry out gradient elution: 0 to 20 minute, acetonitrile concentration was 10～30%, continue after 15 minutes, acetonitrile concentration from 10～30% to 30～40%, 30～40% acetonitrile concentrations are maintained until 60 minutes; Flow velocity 0.5～1.0ml/min; 20～40 ℃ of column temperatures; Detector is an evaporative light scattering detector, 95～125 ℃ of drift tube temperatures, gas flow rate 2.5～3.2SLPM; With reference to the preparation of product solution, it is an amount of that precision takes by weighing the astragaloside reference substance, adds dissolve with methanol and make the solution that every 1ml contains 0.5mg, as reference product solution; The preparation of need testing solution, it is an amount of to get Milkvetch Root, pulverizes, get 1.5g, the accurate title, decide, and puts in the apparatus,Soxhlet's, add methanol 50～200ml, refluxed 2～8 hours, put cold, filter, filtrate is reclaimed methanol to doing, and residue adds water 20ml makes dissolving, extract 2～5 times with water saturated n-butyl alcohol jolting, each 10～40ml merges n-butanol extracting liquid, extracts 1～4 time with ammonia solution, each 5～30ml, discard ammonia solution, n-butyl alcohol liquid evaporate to dryness, residue is with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol and be diluted to scale, shake up,, get subsequent filtrate and detect test liquid as the Milkvetch Root finger printing with the microporous filter membrane filtration of 0.45 μ m; The test liquid finger printing detects, and with high performance liquid chromatography the Milkvetch Root finger printing is detected test liquid and detects, and sample size is 5～50 μ l, writes down 60 minutes chromatogram, gets the finger printing of Milkvetch Root; The test sample finger printing should should be greater than 0.90 with the standard finger-print similarity; The Milkvetch Root finger printing has 7 total fingerprint peakses, with reference to peak S is the astragaloside chromatographic peak, the relative retention time of 7 total fingerprint peakses is respectively: No. 1 peak 0.387 ± 0.039, No. 2 peaks 0.802 ± 0.080,0.875 ± 0.088, No. 5 peaks 0.909 ± 0.091,0.852 ± 0.085, No. 4 peaks, No. 3 peaks, 1.000 ± 0.000, No. 6 peaks 1.030 ± 0.010, S peak.
2, the finger print quality detecting method of Milkvetch Root as claimed in claim 1 is characterized in that this method comprises the steps:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With the ratio of acetonitrile-water be 0.23: 1 as mobile phase, carry out gradient elution: 0 to 20 minute, acetonitrile concentration was 23%, continue after 15 minutes, acetonitrile concentration from 23% to 35%, 35% acetonitrile concentration is maintained until 60 minutes; Flow velocity 0.7ml/min; 35 ℃ of column temperatures; Detector is an evaporative light scattering detector, 105 ℃ of drift tube temperatures, gas flow rate 2.95SLPM; With reference to the preparation of product solution, it is an amount of that precision takes by weighing the astragaloside reference substance, adds dissolve with methanol and make the solution that every 1ml contains 0.5mg, as reference product solution; The preparation of need testing solution, it is an amount of to get Milkvetch Root, pulverizes, get 1.5g, the accurate title, decide, and puts in the apparatus,Soxhlet's, add methanol 120ml, refluxed 6 hours, put cold, filter, filtrate is reclaimed methanol to doing, and residue adds water 20ml makes dissolving, extract 3 times with water saturated n-butyl alcohol jolting, each 15ml merges n-butanol extracting liquid, extracts 2 times with ammonia solution, each 15ml, discard ammonia solution, n-butyl alcohol liquid evaporate to dryness, residue is with dissolve with methanol and be transferred in the 5ml measuring bottle, add methanol and be diluted to scale, shake up,, get subsequent filtrate and detect test liquid as the Milkvetch Root finger printing with the microporous filter membrane filtration of 0.45 μ m; The test liquid finger printing detects, and with high performance liquid chromatography the Milkvetch Root finger printing is detected test liquid and detects, and sample size is 20 μ l, writes down 60 minutes chromatogram, gets the finger printing of Milkvetch Root; The test sample finger printing should should be greater than 0.90 with the standard finger-print similarity; The Milkvetch Root finger printing has 7 total fingerprint peakses, is the astragaloside chromatographic peak with reference to peak S, and the relative retention time of 7 total fingerprint peakses is respectively: No. 1 peak 0.387,0.852, No. 4 peak 0.875,0.802, No. 3 peak, No. 2 peaks, No. 5 peaks 0.909,1.000, No. 6 peaks 1.030, S peak.
3, the finger print quality detecting method of the extract Radix Astragali saponin in the Milkvetch Root is characterized in that this method comprises the steps:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With the ratio of acetonitrile-water is 0.1～0.5: 1 as mobile phase, and carry out gradient elution: 0 to 20 minute, acetonitrile concentration was 10～30%, continue after 15 minutes, acetonitrile concentration from 10～30% to 30～40%, 30～40% acetonitrile concentrations are maintained until 60 minutes; Detector is an evaporative light scattering detector, 95～125 ℃ of drift tube temperatures, gas flow rate 2.5～3.2SLPM; With reference to the preparation of product solution, it is an amount of that precision takes by weighing the astragaloside reference substance, adds dissolve with methanol and make the solution that every 1ml contains 0.5mg, as reference product solution; Radix Astragali saponin 20mg is got in the preparation of need testing solution, and accurate the title decides, and puts in the 5ml measuring bottle, adds dissolve with methanol and is diluted to scale, shakes up; Microporous filter membrane with 0.45 μ m filters, and gets subsequent filtrate, promptly; The test liquid finger printing detects, and with high performance liquid chromatography the Radix Astragali saponin finger printing is detected test liquid and detects, and sample size is 5～50 μ l, writes down 60 minutes chromatogram, gets the finger printing of Radix Astragali saponin; The test sample finger printing should should be greater than 0.90 with the standard finger-print similarity; The Radix Astragali saponin finger printing has 6 total fingerprint peakses, with reference to peak S is the astragaloside chromatographic peak, the relative retention time of 6 total fingerprint peakses is respectively: No. 1 peak 0.797 ± 0.080, No. 2 peaks 0.847 ± 0.085, No. 3 peaks 0.870 ± 0.087, No. 4 peaks 0.905 ± 0.090,1.000 ± 0.000, No. 5 peaks 1.029 ± 0.010, S peak.
4, the finger print quality detecting method of Radix Astragali saponin as claimed in claim 3 is characterized in that this method comprises the steps:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; With the ratio of acetonitrile-water be 0.23: 1 as mobile phase, carry out gradient elution: 0 to 20 minute, acetonitrile concentration was 23%, continue after 15 minutes, acetonitrile concentration from 23% to 35%, 35% acetonitrile concentration is maintained until 60 minutes; Flow velocity 0.7ml/min; 35 ℃ of column temperatures; Detector is an evaporative light scattering detector, 105 ℃ of drift tube temperatures, gas flow rate 2.95SLPM; With reference to the preparation of product solution, it is an amount of that precision takes by weighing the astragaloside reference substance, adds dissolve with methanol and make the solution that every 1ml contains 0.5mg, as reference product solution; Radix Astragali saponin 20mg is got in the preparation of need testing solution, and accurate the title decides, and puts in the 5ml measuring bottle, adds dissolve with methanol and is diluted to scale, shakes up; Microporous filter membrane with 0.45 μ m filters, and gets subsequent filtrate, promptly; The test liquid finger printing detects, and with high performance liquid chromatography the Radix Astragali saponin finger printing is detected test liquid and detects, and sample size is 20 μ l, writes down 60 minutes chromatogram, gets the finger printing of Radix Astragali saponin; The test sample finger printing should should be greater than 0.90 with the standard finger-print similarity; The Radix Astragali saponin finger printing has 6 total fingerprint peakses, is the astragaloside chromatographic peak with reference to peak S, and the relative retention time of 6 total fingerprint peakses is respectively: 0.870, No. 4 peak 0.905,0.847, No. 3 peak, 0.797, No. 2 peak, No. 1 peak, 1.000, No. 5 peaks 1.029, S peak.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610065283 CN1857380A (en) | 2006-03-22 | 2006-03-22 | Method for detecting medicine material astragalus quality |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610065283 CN1857380A (en) | 2006-03-22 | 2006-03-22 | Method for detecting medicine material astragalus quality |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101809518A Division CN102353729A (en) | 2006-03-22 | 2006-03-22 | Quality detection method of radix astragali medicinal material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1857380A true CN1857380A (en) | 2006-11-08 |
Family
ID=37296368
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610065283 Pending CN1857380A (en) | 2006-03-22 | 2006-03-22 | Method for detecting medicine material astragalus quality |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1857380A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149300A (en) * | 2013-03-05 | 2013-06-12 | 贵州师范大学 | Measurement method of radix astragali granule fingerprint and characteristic fingerprint thereof |
| CN104569199A (en) * | 2014-12-30 | 2015-04-29 | 上海现代中医药股份有限公司 | Measuring method for astragalus membranaceus fingerprint spectrum |
| CN105954384A (en) * | 2016-04-22 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for extracting astragaloside in center-supplementing and qi-boosting pill by using rapid solvent extraction process |
| CN113109482A (en) * | 2021-04-29 | 2021-07-13 | 北京振东光明药物研究院有限公司 | Method for establishing fingerprint of astragalus membranaceus medicinal material, extract and single preparation |
| CN115792017A (en) * | 2022-12-06 | 2023-03-14 | 中国中医科学院眼科医院 | Quality detection method of traditional Chinese medicine composition for reducing recurrence of herpes simplex viral keratitis |
| CN118376710A (en) * | 2024-04-19 | 2024-07-23 | 贵州富华药业有限责任公司 | Method for constructing traditional Chinese medicine compound HPLC-ELSD fingerprint containing epimedium and application thereof |
-
2006
- 2006-03-22 CN CN 200610065283 patent/CN1857380A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149300A (en) * | 2013-03-05 | 2013-06-12 | 贵州师范大学 | Measurement method of radix astragali granule fingerprint and characteristic fingerprint thereof |
| CN103149300B (en) * | 2013-03-05 | 2014-06-18 | 贵州汉方制药有限公司 | Measurement method of radix astragali granule fingerprint and characteristic fingerprint thereof |
| CN104569199A (en) * | 2014-12-30 | 2015-04-29 | 上海现代中医药股份有限公司 | Measuring method for astragalus membranaceus fingerprint spectrum |
| CN104569199B (en) * | 2014-12-30 | 2016-08-24 | 上海现代中医药股份有限公司 | A kind of assay method of Radix Astragali finger printing |
| CN105954384A (en) * | 2016-04-22 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Method for extracting astragaloside in center-supplementing and qi-boosting pill by using rapid solvent extraction process |
| CN113109482A (en) * | 2021-04-29 | 2021-07-13 | 北京振东光明药物研究院有限公司 | Method for establishing fingerprint of astragalus membranaceus medicinal material, extract and single preparation |
| CN115792017A (en) * | 2022-12-06 | 2023-03-14 | 中国中医科学院眼科医院 | Quality detection method of traditional Chinese medicine composition for reducing recurrence of herpes simplex viral keratitis |
| CN118376710A (en) * | 2024-04-19 | 2024-07-23 | 贵州富华药业有限责任公司 | Method for constructing traditional Chinese medicine compound HPLC-ELSD fingerprint containing epimedium and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1857380A (en) | Method for detecting medicine material astragalus quality | |
| CN1707260A (en) | Angelica sinensis and ligusticum wallichii Chinese medicinal crop and establishing method for its preparation finger print and standard fingerprint | |
| CN107356684B (en) | Method for detecting fingerprint of cassia seed | |
| CN101049389A (en) | Method for controlling quality of granule preparation for treating chilly sensation type gastritis | |
| CN104458993B (en) | The method for building up of strong medicinal material blumea riparia HPLC finger-print | |
| CN102353729A (en) | Quality detection method of radix astragali medicinal material | |
| CN108254470B (en) | Method for simultaneously measuring saccharide components in rehmannia and establishing fingerprint spectrum of saccharide components | |
| CN1857589A (en) | Method of measuring icariin and epimedin c content in Xianlinggubao preparation | |
| CN1785255A (en) | Method for quality control of traditional Chinese medicine prepns. | |
| CN1991361A (en) | Method for checking quality of Chinese Jin wine by using fingerprint pattern technology | |
| CN101028388A (en) | Quality inspection of Chinese-medicinal preparation for treating shortsighness and asthenopia | |
| CN101028460A (en) | Method for inspecting throat-clearing Chinese medicinal pills | |
| CN101029889A (en) | Method for inspecting Chinese medicinal preparation quality in treatment of old man eyes dieases | |
| CN1872097A (en) | Method for controlling quality of spore oil, powder and preparation of ganoderma lucidum | |
| CN1844913A (en) | Quality detection method for fingerprint spectrum method of radix astragali saponin injection | |
| CN101040951A (en) | Method of controlling the quality of Ynxingchao dropping pills compound | |
| CN1900710A (en) | Establishment of lucid ganderma spore and lucid ganderma spore oil finger print atlas and standard finger print atlas | |
| CN1991360A (en) | Method for identifying Korea barren wort medicinal material by using traditional medicine fingerprint pattern technology | |
| CN101028487A (en) | Chinese-medicinal preparation for treating eyeground bleeding and method for inspecting vision-improving prescription quality | |
| CN1785294A (en) | Quality control method of eucommia bark blood pressure lowering preparation for treating high blood pressure | |
| CN108982738B (en) | Construction method and detection method of intermediate characteristic spectrum of Zhenqi Fuzheng granule or Zhenqi Fuzheng granule fingerprint | |
| CN1785347A (en) | Quality control method of Chinese medicinal preparation for treating child hyperpyrexia | |
| CN1844911A (en) | Leech fingerprint spectrum establishment method and medicinal leech identification method | |
| CN1844912A (en) | Earthworm fingerprint spectrum establishment method and medicinal earthworm identification method | |
| CN1857445A (en) | Quality control method for Desheng preparation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20061108 |