CN1333248C - Chinese medicine quality control method - Google Patents
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- CN1333248C CN1333248C CNB031460348A CN03146034A CN1333248C CN 1333248 C CN1333248 C CN 1333248C CN B031460348 A CNB031460348 A CN B031460348A CN 03146034 A CN03146034 A CN 03146034A CN 1333248 C CN1333248 C CN 1333248C
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- 238000003908 quality control method Methods 0.000 title claims abstract description 10
- 239000003814 drug Substances 0.000 title abstract description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 63
- 230000014759 maintenance of location Effects 0.000 claims abstract description 22
- 239000013558 reference substance Substances 0.000 claims abstract description 14
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 66
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- 244000111489 Gardenia augusta Species 0.000 claims description 44
- 235000018958 Gardenia augusta Nutrition 0.000 claims description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 41
- 239000000243 solution Substances 0.000 claims description 39
- 238000012360 testing method Methods 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 17
- 238000002360 preparation method Methods 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- XJMPAUZQVRGFRE-SCHFUKFYSA-N Gardenoside Natural products O=C(OC)C=1[C@H]2[C@H]([C@H](O[C@H]3[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O3)OC=1)[C@@](O)(CO)C=C2 XJMPAUZQVRGFRE-SCHFUKFYSA-N 0.000 claims description 16
- XJMPAUZQVRGFRE-AYDWLWLASA-N methyl (1s,4as,7s,7as)-7-hydroxy-7-(hydroxymethyl)-1-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy-4a,7a-dihydro-1h-cyclopenta[c]pyran-4-carboxylate Chemical compound O([C@@H]1OC=C([C@@H]2[C@H]1[C@](C=C2)(O)CO)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O XJMPAUZQVRGFRE-AYDWLWLASA-N 0.000 claims description 16
- 238000010828 elution Methods 0.000 claims description 14
- 238000004519 manufacturing process Methods 0.000 claims description 14
- 239000003480 eluent Substances 0.000 claims description 13
- 239000006071 cream Substances 0.000 claims description 8
- 230000006837 decompression Effects 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 235000012054 meals Nutrition 0.000 claims description 8
- 238000010790 dilution Methods 0.000 claims description 7
- 239000012895 dilution Substances 0.000 claims description 7
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 claims description 6
- 238000003556 assay Methods 0.000 claims description 6
- 238000011003 system suitability test Methods 0.000 claims description 6
- 238000005325 percolation Methods 0.000 claims description 5
- 229940023032 activated charcoal Drugs 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000005374 membrane filtration Methods 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000002137 ultrasound extraction Methods 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 239000012453 solvate Substances 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims 2
- 238000004811 liquid chromatography Methods 0.000 claims 2
- 241000157835 Gardenia Species 0.000 abstract 3
- 239000007788 liquid Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 239000012847 fine chemical Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 150000002338 glycosides Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention discloses a quality control method for Chinese medicine, which particularly relates to a fingerprint map of gardenia as a Chinese medicine. The standard of the fingerprint map uses gardenia as a reference substance, and methanol is made into a solution as a solution of the reference substance. The retention time and the peak area of a chromatographic peak (S peak) of the gardenia are set as 1, and thus, the ratio of the relative retention time to the peak area is calculated.
Description
Invention field
The present invention relates to a kind of traditional Chinese medicine quality control method, particularly the method for quality control of Chinese medicine cape jasmine.
Background technology
Science and technology development provides condition for the Chinese medicine basic research, provides technical support for improving constantly traditional Chinese medicine quality.Traditional Chinese medicine fingerprint is a notion of using for reference the medical jurisprudence fingerprint, comprises Chinese medicine dna fingerprinting, protein fingerprint pattern and chemical fingerprint etc.; Usually said finger-print is meant chemical fingerprint; Traditional Chinese medicine fingerprint refers to that Chinese medicine is after suitably handling, adopt certain analysis means, obtain to indicate the total peak collection of illustrative plates of this Chinese medicine feature, by holding the feature of Chinese medicine fingerprint, differentiate the quality of Chinese medicine effectively, guarantee that Chinese crude drug and Chinese patent drug quality are relatively stable.
The research of traditional Chinese medicine fingerprint and application, not only can solve the difficult problem that China's traditional Chinese medicine authenticity of products difficulty is debated, also for strengthening the systematization and the standardization of Chinese crude drug plantation and processing specificationization, the inherent composition research of Chinese medicine, accelerate the development of the modernization of Chinese medicine, realize the assurance that science is provided in line with international standards.
Summary of the invention
The object of the invention is the finger-print that open cape jasmine is new.
The present invention is achieved by the following technical solutions:
Cape jasmine medicinal materials fingerprint examination criteria:
The preparation of need testing solution: get the meal 0.5g that cape jasmine crosses 24 mesh sieves, the accurate title, decide, and puts in the 100ml triangular flask, add methyl alcohol 100ml ultrasonic Extraction 15-30min, filter, get subsequent filtrate 50ml, water bath method, residue is separated with about 5ml is water-soluble, the granular activated carbon post of last 5g, wash with water near colourless after, add 30ml 60-80% ethanol elution, the ethanol eluate evaporate to dryness, the residue dissolve with methanol, constant volume becomes 10ml, shakes up, use membrane filtration, promptly get need testing solution;
The preparation of reference substance solution: get the Gardenoside reference substance, make solution that 1mg contains 0.5mg product solution in contrast with methyl alcohol; Assay method: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000); Chromatographic condition and system suitability test detect wavelength 238nm, and the acetonitrile-water gradient elution sees Table 1; Theoretical cam curve is calculated, and should not hang down 30000; Setting the need testing solution sample size is 10 μ l, writes down 60 minutes chromatogram, promptly; Is 1 calculating relative retention time and peak area ratio with Cape jasmine in the retention time and the peak area of the chromatographic peak (S peak) of glycosides; Finger-print and technical parameter: adopt high performance liquid chromatography, detect 10 batches of cape jasmine medicinal materials, be 1 hour writing time; The demarcation of total fingerprint peaks, (relative retention time): 1, (0.400) 2, (0.458) 3, (0.511) 4, (0.588) 5, (0.618) 6, (0.666) 7, (0.722) 8, (0.800) S, (1.000) 9, (1.084) 10, (1.109) 11, (1.195) 12, (1.235) 13, (1.290) 14, (1.815) 15, (1.832) 16, (1.850) 17, (1.864) 18, (1.889) 19, (1.905) 20, (1.918) 21, (1.940) 22, (1.950) 23, (1.962) 24, (1.972) 25, (1.991) 26, (2.019); Total fingerprint peaks area ratio: except that the Gardenoside peak, the peak area at other peak accounts for the number percent of total peak area all less than 10%, so peak area ratio is not done requirement; The part peak shape is described: the 14-26 peak is not for reaching the group peak of baseline separation, and what have is broad peak;
Non-total peak area: test sample collection of illustrative plates and reference fingerprint compare, and the non-total peak total area must not be greater than 10% of total peak area.
Cape jasmine semi-manufacture finger-print examination criteria: cape jasmine semi-manufacture preparation: get cape jasmine, be ground into meal, the 65-80% ethanol percolation of doubly measuring with 7-9, collect percolate, reclaim ethanol, be concentrated into the clear cream that 55-70 ℃ of relative density is 1.00-1.20, add 3-5 times of water gaging dilution, stir evenly, 0-4 ℃ refrigerates 45-50 hour, filters, 55-70 ℃ of relative density of filtrate decompression simmer down to is the clear cream of 1.00-1.20, last activated-charcoal column is used the distilled water wash-out earlier, and is colourless to eluent, doubly measure the 65-80% ethanol elution with 9-11 again, collect eluent, decompression recycling ethanol also concentrates, and gets the cape jasmine semi-manufacture;
The preparation of need testing solution: get cape jasmine semi-manufacture 1ml, water bath method adds methanol solvate, and the dilution constant volume becomes 2ml, crosses 0.45 μ m filter membrane, makes need testing solution;
The preparation of Gardenoside reference substance solution: get the Gardenoside reference substance, make the solution that every 1ml contains 0.5mg with methyl alcohol and compare product solution;
Assay method: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000); Chromatographic condition and system suitability test: detect wavelength 238nm, the acetonitrile-water gradient elution sees Table 1; Theoretical cam curve is calculated, and should not hang down 30000; Setting the need testing solution sample size is 10 μ l, writes down 60 minutes chromatograms, promptly; With the retention time of the chromatographic peak (S peak) of Gardenoside and peak area is 1 to calculate relative retention time and peak area ratio; Finger-print and technical parameter thereof: the peak number (relative retention time) of total fingerprint peaks: 1 (0.404) 2 (0.463) 3 (0.511) 4 (0.589) 5 (0.618) 6 (0.667) 7 (0.723) 8 (0.800) S (1.000) 9 (1.084) 10 (1.110) 11 (1.195) 12 (1.236) 13 (1.275); Peak area ratio: 1: 7: S=(0.121-0.153): (0.124-0.137): (1.000); Non-total peak area: test sample collection of illustrative plates and reference fingerprint are relatively; The non-total peak total area must not be greater than 5% of peak area;
The used instrument reagent of the half-finished finger-print of above cape jasmine and cape jasmine:
High performance liquid chromatograph: Waters2695 pump; Waters 2996 UV-detector; The Millcnnium32 chromatographic work station; Diamonsil C18 post (5 μ m, 4.6mm * 150mm); Acetonitrile is chromatographically pure (U.S. J.T.Baker); The Wahaha pure water; Methyl alcohol is chromatographically pure (Beijing prosperousization Fine Chemical Works);
Table 1 eluent gradient wash-out table
| Time (min) | Flow velocity (ml/min) | Water % | Acetonitrile % |
| 0 | 0.8 | 95 | 5 |
| 8 | 0.8 | 92 | 8 |
| 21 | 0.8 | 88 | 12 |
| 35 | 0.8 | 88 | 12 |
| 40 | 0.8 | 70 | 30 |
| 45 | 0.8 | 40 | 60 |
| 50 | 0.8 | 0 | 100 |
| 60 | 0.8 | 0 | 100 |
The present invention discloses cape jasmine and the half-finished finger-print of cape jasmine first, and this makes cape jasmine and the half-finished quality control of cape jasmine, and more science is accurate.
Embodiment
The preparation of embodiment 1 cape jasmine semi-manufacture
Get cape jasmine, be ground into meal, according to the percolation under the liquid extract item (" appendix IO of Chinese pharmacopoeia version in 2000),, collect percolate with 70% ethanol percolation of 8 times of amounts, reclaim ethanol, being concentrated into relative density is the clear cream of 1.10 (60 ℃ of mensuration), adds 4 times of water gaging dilutions, stirs evenly, 0-4 ℃ refrigerates 48 hours, filter, filtrate decompression simmer down to relative density is the clear cream of 1.10 (60 ℃ of mensuration), last activated-charcoal column, use earlier the distilled water wash-out, colourless to eluent, with 10 times of amount 70% ethanol elutions, collect eluent again, decompression recycling ethanol also concentrates, and gets the cape jasmine semi-manufacture.
Cape jasmine semi-manufacture finger-print examination criteria: the preparation of need testing solution: get cape jasmine semi-manufacture 1ml, water bath method adds methanol solvate, and the dilution constant volume becomes 2ml, crosses 0.45 μ m filter membrane, makes need testing solution;
The preparation of Gardenoside reference substance solution: get the Gardenoside reference substance, make the solution that every 1ml contains 0.5mg with methyl alcohol and compare product solution;
Assay method: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000); Chromatographic condition and system suitability test: detect wavelength 238nm, the acetonitrile-water gradient elution sees Table 1; Theoretical cam curve is calculated, and should not hang down 30000; Setting the need testing solution sample size is 10 μ l, writes down 60 minutes chromatograms, promptly; With the retention time of the chromatographic peak (S peak) of Gardenoside and peak area is 1 to calculate relative retention time and peak area ratio; Finger-print and technical parameter thereof: the peak number (relative retention time) of total fingerprint peaks: 1 (0.404) 2 (0.463) 3 (0.511) 4 (0.589) 5 (0.618) 6 (0.667) 7 (0.723) 8 (0.800) S (1.000) 9 (1.084) 10 (1.110) 11 (1.195) 12 (1.236) 13 (1.275); Peak area ratio: 1: 7: S=(0.121-0.153): (0.124-0.137): (1.000); Non-total peak area: test sample collection of illustrative plates and reference fingerprint are relatively; The non-total peak total area must not be greater than 5% of peak area;
The used instrument reagent of the half-finished finger-print of cape jasmine:
High performance liquid chromatograph: Waters2695 pump; Waters 2996 UV-detector; The Millcnnium32 chromatographic work station; Diamonsil C18 post (5 μ m, 4.6mm * 150mm); Acetonitrile is chromatographically pure (U.S. J.T.Baker); The Wahaha pure water; Methyl alcohol is chromatographically pure (Beijing prosperousization Fine Chemical Works);
Table 1 eluent gradient wash-out table
| Time (min) | Flow velocity (ml/min) | Water % | Acetonitrile % |
| 0 | 0.8 | 95 | 5 |
| 8 | 0.8 | 92 | 8 |
| 21 | 0.8 | 88 | 12 |
| 35 | 0.8 | 88 | 12 |
| 40 | 0.8 | 70 | 30 |
| 45 | 0.8 | 40 | 60 |
| 50 | 0.8 | 0 | 100 |
| 60 | 0.8 | 0 | 100 |
Embodiment 2 cape jasmine medicinal materials fingerprint examination criterias
The preparation of need testing solution: get the meal 0.5g that cape jasmine crosses 24 mesh sieves, the accurate title, decide, and puts in the 100ml triangular flask, add methyl alcohol 100ml ultrasonic Extraction 20min, filter, get subsequent filtrate 50ml, water bath method, residue is separated with about 5ml is water-soluble, the granular activated carbon post of last 5g, wash with water near colourless after, add 30ml 70% ethanol elution, the ethanol eluate evaporate to dryness, the residue dissolve with methanol, constant volume becomes 10ml, shakes up, with 0.45 μ m membrane filtration, promptly get need testing solution;
The preparation of reference substance solution: get the Gardenoside reference substance, make solution that 1mg contains 0.5mg product solution in contrast with methyl alcohol; Assay method: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000); Chromatographic condition and system suitability test detect wavelength 238nm, and the acetonitrile-water gradient elution sees Table 1; Theoretical cam curve is calculated, and should not hang down 30000; Setting the need testing solution sample size is 10 μ l, writes down 60 minutes chromatogram, promptly; Is 1 calculating relative retention time and peak area ratio with Cape jasmine in the retention time and the peak area of the chromatographic peak (S peak) of glycosides; Finger-print and technical parameter: adopt high performance liquid chromatography, detect 10 batches of cape jasmine medicinal materials, be 1 hour writing time; The demarcation of total fingerprint peaks, (relative retention time): 1, (0.400) 2, (0.458) 3, (0.511) 4, (0.588) 5, (0.618) 6, (0.666) 7, (0.722) 8, (0.800) S, (1.000) 9, (1.084) 10, (1.109) 11, (1.195) 12, (1.235) 13, (1.290) 14, (1.815) 15, (1.832) 16, (1.850) 17, (1.864) 18, (1.889) 19, (1.905) 20, (1.918) 21, (1.940) 22, (1.950) 23, (1.962) 24, (1.972) 25, (1.991) 26, (2.019); Total fingerprint peaks area ratio: except that the Gardenoside peak, the peak area at other peak accounts for the number percent of total peak area all less than 10%, so peak area ratio is not done requirement; The part peak shape is described: the 14-26 peak is not for reaching the group peak of baseline separation, and what have is broad peak;
Non-total peak area: test sample collection of illustrative plates and reference fingerprint compare, and the non-total peak total area must not be greater than 10% of total peak area.
The used instrument reagent of cape jasmine finger-print:
High performance liquid chromatograph: Waters2695 pump; The Waters2996 UV-detector; The Millcnnium32 chromatographic work station; Diamonsil C18 post (5 μ m, 4.6mm * 150mm); Acetonitrile is chromatographically pure (U.S. J.T.Baker); The Wahaha pure water; Methyl alcohol is chromatographically pure (Beijing prosperousization Fine Chemical Works);
Table 1 eluent gradient wash-out table
| Time (min) | Flow velocity (ml/min) | Water % | Acetonitrile % |
| 0 | 0.8 | 95 | 5 |
| 8 | 0.8 | 92 | 8 |
| 21 | 0.8 | 88 | 12 |
| 35 | 0.8 | 88 | 12 |
| 40 | 0.8 | 70 | 30 |
| 45 | 0.8 | 40 | 60 |
| 50 | 0.8 | 0 | 100 |
| 60 | 0.8 | 0 | 100 |
Claims (4)
1, the method for quality control of cape jasmine medicinal materials fingerprint detection, it is characterized in that this method is: the preparation of need testing solution: get the meal 0.5g that cape jasmine crosses 24 mesh sieves, the accurate title, decide, put in the 100ml triangular flask, add methyl alcohol 100ml ultrasonic Extraction 15-30min, filter, get subsequent filtrate 50ml, water bath method, residue is separated with 5ml is water-soluble, the granular activated carbon post of last 5g, wash with water near colourless after, add 30ml 60-80% ethanol elution, ethanol eluate evaporate to dryness, residue dissolve with methanol, constant volume becomes 10ml, shake up, use membrane filtration, promptly get need testing solution; The preparation of reference substance solution: get the Gardenoside reference substance, make solution that 1mg contains 0.5mg product solution in contrast with methyl alcohol; Assay method: according to high effective liquid chromatography for measuring; Chromatographic condition and system suitability test detect wavelength 238nm, the acetonitrile-water gradient elution; Theoretical cam curve is calculated, and should not hang down 30000; Setting the need testing solution sample size is 10 μ l, writes down 60 minutes chromatogram, promptly; With the chromatographic peak of Gardenoside is that the retention time at S peak and peak area are 1 to calculate relative retention time and peak area ratio; Finger-print and technical parameter: adopt high performance liquid chromatography, detect 10 batches of cape jasmine medicinal materials, be 1 hour writing time; Demarcate total fingerprint peaks with relative retention time, the relative retention time at 1-26 peak is respectively 0.400,0.458,0.511,0.588,0.618,0.666,0.722,0.800,1.000,1.084,1.109,1.195,1.235,1.290,1.815,1.832,1.850,1.864,1.889,1.905,1.918,1.940,1.950,1.962,1.972,1.991,2.019; Total fingerprint peaks area ratio: except that the Gardenoside peak, the peak area at other peak accounts for the number percent of total peak area all less than 10%, so peak area ratio is not done requirement; The part peak shape is described: the 14-26 peak is not for reaching the group peak of baseline separation, and what have is broad peak; Non-total peak area: test sample collection of illustrative plates and reference fingerprint compare, and the non-total peak total area must not be greater than 10% of total peak area;
Wherein, the eluent gradient wash-out is: flow velocity is 0.8ml/min; 0 moment water and acetonitrile ratio are: 95: 5; In the time of the 8th minute, water and acetonitrile ratio are 92: 8; In the time of the 21st minute, water and acetonitrile ratio are 88: 12; In the time of the 35th minute, water and acetonitrile ratio are 88: 12; In the time of the 40th minute, water and acetonitrile ratio are 70: 30; In the time of the 45th minute, water and acetonitrile ratio are 40: 60; In the time of the 50th minute, water and acetonitrile ratio are 0: 100; In the time of the 60th minute, water and acetonitrile ratio are 0: 100.
2; the method of quality control that cape jasmine medicinal materials fingerprint as claimed in claim 1 detects; it is characterized in that the preparation of need testing solution in this method: get the meal 0.5g that cape jasmine crosses 24 mesh sieves; the accurate title, decide; put in the 100ml triangular flask, add methyl alcohol 100ml ultrasonic Extraction 20min, filter; get subsequent filtrate 50ml; water bath method, residue is separated with 5ml is water-soluble, the granular activated carbon post of last 5g; wash with water near colourless after; add 3,0m1 70% ethanol elution, ethanol eluate evaporate to dryness, residue dissolve with methanol; constant volume becomes 10ml; shake up,, promptly get need testing solution with 0.45 μ m membrane filtration.
3, the method for quality control of cape jasmine semi-manufacture finger-print detection, it is characterized in that this method is: the preparation of need testing solution: get cape jasmine semi-manufacture 1ml, water bath method adds methanol solvate, and the dilution constant volume becomes 2ml, crosses 0.45 μ m filter membrane, makes need testing solution; The preparation of Gardenoside reference substance solution: get the Gardenoside reference substance, make the solution that every 1ml contains 0.5mg with methyl alcohol and compare product solution; Assay method: according to high effective liquid chromatography for measuring; Chromatographic condition and system suitability test: detect wavelength 238nm, the acetonitrile-water gradient elution; Theoretical cam curve is calculated, and should not hang down 30000; Setting the need testing solution sample size is 10 μ l, writes down 60 minutes chromatograms, promptly; With the chromatographic peak of Gardenoside is that the retention time at S peak and peak area are 1 to calculate relative retention time and peak area ratio; Finger-print and technical parameter thereof: demarcate total fingerprint peaks with relative retention time, the relative retention time at 1-13 peak is respectively 0.404,0.463,0.511,0.589,0.618,0.667,0.723,0.800,1.000,1.084,1.1101.195,1.236,1.275; No. 1 peak and No. 7 peaks are respectively 0.121～0.153,0.124～0.137 and 1.000 with respect to the peak area ratio at S peak; Non-total peak area: test sample collection of illustrative plates and reference fingerprint are relatively; The non-total peak total area must not be greater than 5% of peak area;
Wherein, the eluent gradient wash-out is: flow velocity is 0.8ml/min; 0 moment water and acetonitrile ratio are: 95: 5; In the time of the 8th minute, water and acetonitrile ratio are 92: 8; In the time of the 21st minute, water and acetonitrile ratio are 88: 12; In the time of the 35th minute, water and acetonitrile ratio are 88: 12; In the time of the 40th minute, water and acetonitrile ratio are 70: 30; In the time of the 45th minute, water and acetonitrile ratio are 40: 60; In the time of the 50th minute, water and acetonitrile ratio are 0: 100; In the time of the 60th minute, water and acetonitrile ratio are 0: 100;
Wherein the half-finished preparation method of cape jasmine is: get cape jasmine, be ground into meal, the 65-80% ethanol percolation of doubly measuring with 7-9, collect percolate, reclaim ethanol, be concentrated into the clear cream that 55-70 ℃ of relative density is 1.00-1.20, add 3-5 times of water gaging dilution, stir evenly, 0-4 ℃ refrigerates 45-50 hour, filters, 55-70 ℃ of relative density of filtrate decompression simmer down to is the clear cream of 1.00-1.20, last activated-charcoal column is used the distilled water wash-out earlier, and is colourless to eluent, doubly measure the 65-80% ethanol elution with 9-11 again, collect eluent, decompression recycling ethanol also concentrates, and gets the cape jasmine semi-manufacture.
4, the method of quality control that cape jasmine semi-manufacture finger-print as claimed in claim 3 detects, it is characterized in that the half-finished preparation method of cape jasmine is in this method: get cape jasmine, be ground into meal,, collect percolate with 70% ethanol percolation of 8 times of amounts, reclaim ethanol, be concentrated into 60 ℃ of following relative densities and be 1.10 clear cream, add 4 times of water gagings dilutions, stir evenly, 0-4 ℃ refrigerates 48 hours, filter, 60 ℃ of following relative densities of filtrate decompression simmer down to are 1.10 clear cream, last activated-charcoal column, use earlier the distilled water wash-out, colourless to eluent, with 10 times of amount 70% ethanol elutions, collect eluent again, decompression recycling ethanol also concentrates, and gets the cape jasmine semi-manufacture.
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| CNB031460348A CN1333248C (en) | 2003-07-14 | 2003-07-14 | Chinese medicine quality control method |
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| CNB031460348A CN1333248C (en) | 2003-07-14 | 2003-07-14 | Chinese medicine quality control method |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100419423C (en) * | 2004-10-15 | 2008-09-17 | 成都优他制药有限责任公司 | Method for controlling quality of simply single drug |
| CN101343297B (en) * | 2008-07-08 | 2011-03-23 | 陕西科技大学 | Method for extracting and purifying gardenoside with absorbent charcoal |
| CN102692473B (en) * | 2011-03-22 | 2015-08-19 | 石家庄以岭药业股份有限公司 | A kind of assay method of Fructus Gardeniae finger-print |
| CN109164178B (en) * | 2018-08-23 | 2021-07-27 | 四川新绿色药业科技发展有限公司 | Quality detection and identification method for gardenia and processed products thereof |
| CN110554124A (en) * | 2019-09-24 | 2019-12-10 | 哈尔滨珍宝制药有限公司 | Method for measuring fingerprint spectrum of gardenia formula particles |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1322951A (en) * | 2001-06-29 | 2001-11-21 | 天津市金士力药物研究开发有限公司 | Red sage medicine fingerprint establishing method and standard fingerprint atlas |
| WO2002046739A1 (en) * | 2000-12-08 | 2002-06-13 | Council Of Scientific And Industrial Research | A novel method for chromatographic finger printing and standardization of single medicines and formulations |
| JP2002214215A (en) * | 2001-01-12 | 2002-07-31 | Council Scient Ind Res | Chromatograph finger print and novel method for standardizing single medicine and prescribed matter |
| CN1403809A (en) * | 2001-09-04 | 2003-03-19 | 洪筱坤 | Establishment and application of Chinese medicine chaacteristic fingerprint spectrum |
| CN1419124A (en) * | 2002-12-23 | 2003-05-21 | 北京采瑞医药有限公司 | Method for controlling quality of compound red sage root preparation used for treating cardio-cerebral vascualr disease |
-
2003
- 2003-07-14 CN CNB031460348A patent/CN1333248C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002046739A1 (en) * | 2000-12-08 | 2002-06-13 | Council Of Scientific And Industrial Research | A novel method for chromatographic finger printing and standardization of single medicines and formulations |
| JP2002214215A (en) * | 2001-01-12 | 2002-07-31 | Council Scient Ind Res | Chromatograph finger print and novel method for standardizing single medicine and prescribed matter |
| CN1322951A (en) * | 2001-06-29 | 2001-11-21 | 天津市金士力药物研究开发有限公司 | Red sage medicine fingerprint establishing method and standard fingerprint atlas |
| CN1403809A (en) * | 2001-09-04 | 2003-03-19 | 洪筱坤 | Establishment and application of Chinese medicine chaacteristic fingerprint spectrum |
| CN1419124A (en) * | 2002-12-23 | 2003-05-21 | 北京采瑞医药有限公司 | Method for controlling quality of compound red sage root preparation used for treating cardio-cerebral vascualr disease |
Non-Patent Citations (4)
| Title |
|---|
| "中药药效成分的指纹图谱分析思路与方法" 梁鑫淼等，中国天然药物，第1卷第1期 2003;"中药指纹图谱研究概况" 杨义芳等，中草药，第34卷第6期 2003;"栀子药材毛细管电泳指纹图谱的研究" 曹敏等，中国药科大学学报，第33卷第4期 2002 * |
| "中药指纹图谱研究概况" 杨义芳等，中草药，第34卷第6期 2003 * |
| "中药药效成分的指纹图谱分析思路与方法" 梁鑫淼等，中国天然药物，第1卷第1期 2003 * |
| "栀子药材毛细管电泳指纹图谱的研究" 曹敏等，中国药科大学学报，第33卷第4期 2002 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1475802A (en) | 2004-02-18 |
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