CN102399252A - Preparation method of cowherb seed flavonoid glycoside monomer - Google Patents
Preparation method of cowherb seed flavonoid glycoside monomer Download PDFInfo
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- CN102399252A CN102399252A CN2011104200855A CN201110420085A CN102399252A CN 102399252 A CN102399252 A CN 102399252A CN 2011104200855 A CN2011104200855 A CN 2011104200855A CN 201110420085 A CN201110420085 A CN 201110420085A CN 102399252 A CN102399252 A CN 102399252A
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- 229930182486 flavonoid glycoside Natural products 0.000 title claims abstract description 41
- 150000007955 flavonoid glycosides Chemical class 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000178 monomer Substances 0.000 title claims abstract description 11
- 244000178320 Vaccaria pyramidata Species 0.000 title abstract 4
- 235000010587 Vaccaria pyramidata Nutrition 0.000 title abstract 4
- 239000011347 resin Substances 0.000 claims abstract description 26
- 229920005989 resin Polymers 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000007791 liquid phase Substances 0.000 claims abstract description 8
- 238000005191 phase separation Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000012071 phase Substances 0.000 claims abstract description 5
- 238000000605 extraction Methods 0.000 claims abstract description 3
- 210000000582 semen Anatomy 0.000 claims description 48
- 101100400378 Mus musculus Marveld2 gene Proteins 0.000 claims description 14
- 238000004262 preparative liquid chromatography Methods 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 230000004913 activation Effects 0.000 claims description 8
- 230000000274 adsorptive effect Effects 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 8
- 239000012141 concentrate Substances 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 235000012054 meals Nutrition 0.000 claims description 4
- 239000012982 microporous membrane Substances 0.000 claims description 4
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 4
- 238000012856 packing Methods 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 239000013076 target substance Substances 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical group O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 18
- 239000002904 solvent Substances 0.000 abstract description 5
- 239000003814 drug Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 229940126680 traditional chinese medicines Drugs 0.000 abstract description 2
- 238000009835 boiling Methods 0.000 abstract 1
- 238000001514 detection method Methods 0.000 abstract 1
- 239000000945 filler Substances 0.000 abstract 1
- 238000011027 product recovery Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 241000219321 Caryophyllaceae Species 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 2
- 241001530119 Vaccaria Species 0.000 description 2
- OTAFHZMPRISVEM-UHFFFAOYSA-N chromone Chemical compound C1=CC=C2C(=O)C=COC2=C1 OTAFHZMPRISVEM-UHFFFAOYSA-N 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000010898 silica gel chromatography Methods 0.000 description 2
- 206010013935 Dysmenorrhoea Diseases 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- GYIKGLVKALOGDP-DSBKMWIDSA-N Isovitexin 4'-O-glucoside 2''-O-arabinoside Natural products O([C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1c1c(O)c2C(=O)C=C(c3ccc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)cc3)Oc2cc1O)[C@@H]1[C@H](O)[C@H](O)[C@H](O)CO1 GYIKGLVKALOGDP-DSBKMWIDSA-N 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 229920005654 Sephadex Polymers 0.000 description 1
- 244000058569 Vaccaria hispanica Species 0.000 description 1
- 235000004877 Vaccaria hispanica subsp hispanica Nutrition 0.000 description 1
- GYIKGLVKALOGDP-HLEFUGOVSA-N Vaccarin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC=C(C=2OC3=CC(O)=C([C@H]4[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O4)O[C@H]4[C@@H]([C@@H](O)[C@@H](O)CO4)O)C(O)=C3C(=O)C=2)C=C1 GYIKGLVKALOGDP-HLEFUGOVSA-N 0.000 description 1
- GYIKGLVKALOGDP-UHFFFAOYSA-N Vaccarin Natural products OC1C(O)C(O)C(CO)OC1OC1=CC=C(C=2OC3=CC(O)=C(C4C(C(O)C(O)C(CO)O4)OC4C(C(O)C(O)CO4)O)C(O)=C3C(=O)C=2)C=C1 GYIKGLVKALOGDP-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000037006 agalactosis Effects 0.000 description 1
- 125000002351 beta-D-glucopyranosyloxy group Chemical group 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000035619 diuresis Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 208000004396 mastitis Diseases 0.000 description 1
- 230000002175 menstrual effect Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000002953 preparative HPLC Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a method for quickly separating high-purity cowherb seed flavonoid glycoside monomers from a traditional Chinese medicine cowherb seed, belonging to the technical field of traditional Chinese medicines. The process steps of the invention are as follows: A. raw material extraction: boiling in water; B. enriching macroporous resin; C. high-efficiency preparation and liquid phase separation: c18 filler, the detection wavelength is 280nm, and the mobile phase is a methanol solution with the volume fraction of 30%; D. and product recovery: the prepared solution is enriched by macroporous resin, desorbed by ethanol, concentrated and dried to obtain the cowherb seed flavonoid glycoside monomer with the purity of more than 99 percent. The method is simple and rapid, has less solvent consumption, high yield, economy and environmental protection, can prepare a large amount of products at one time, and has higher economic value and academic value.
Description
Technical field
The present invention relates to the monomeric preparation method of a kind of Chemistry for Chinese Traditional Medicine, belong to technical field of traditional Chinese medicines, particularly, the present invention relates to a kind of from the Chinese medicinal materials Semen Vaccariae sharp separation high purity Semen Vaccariae flavonoid glycoside monomer methods.
Background technology
Chinese medicinal materials Semen Vaccariae (Vaccariae Semen); It is the dry mature seed of Caryophyllaceae (Caryophyllaceae) Vaccaria (Vaccaria Medic.) plant cow-fat (Vaccaria segetalis (Neck.) Garcke); Has promoting blood circulation to restore menstrual flow; The lactogenesis detumescence, the effect of inducing diuresis for treating stranguria syndrome.Be used for through closing, dysmenorrhoea, agalactia, acute mastitis swells and ache, the puckery pain of stranguria." Chinese pharmacopoeia is recorded, and is lactagogue good medicine in order to go through portion.
Semen Vaccariae flavonoid glycoside (Vaccarin); Chemistry 4H-1-Benzopyran-4-one by name; 6-(2-O-α-L-arabinopyranosyl-β-D-glucopyranosyl)-2-[4-(phenyl of β-D-glucopyranosyloxy)]-5,7-dihydroxy-, molecular formula is C
32H
38O
19, structural formula is following:
The Semen Vaccariae flavonoid glycoside is the main active ingredient of Semen Vaccariae, also is characteristic chemical constituent, is used for the quality control of Semen Vaccariae medicinal material.At present seldom about the bibliographical information of Semen Vaccariae flavonoid glycoside separation and purification; The Meng, report such as he, Qin Wenjie utilized silica gel column chromatography to combine dextran gel column chromatography to separate, and can obtain Semen Vaccariae flavonoid glycoside crystalline particulate (" herbal medicine " in May, 2011).Through repeatedly practising, Semen Vaccariae flavonoid glycoside water-soluble very strong is difficult for silica gel column chromatography and separates and crystallization purifying, thereby be difficult to obtain its high-purity monomer.The author finds to adopt the preparative high performance liquid chromatography post to separate through a large amount of practices of groping, and through once preparation, product purity can reach more than 99%.High performance preparative liquid chromatography is used for the monomeric separation and purification of Semen Vaccariae flavonoid glycoside and belongs to reported first.
Summary of the invention
The present invention is intended to overcome the defective of prior art, provide a kind of from the Semen Vaccariae medicinal material method of separating high-purity Semen Vaccariae flavonoid glycoside.Should method is simple, consume that solvent is few, yield is high, safety non-toxic, environmental protection, and product purity can reach more than 99%, can satisfy scale operation and suitability for industrialized production needs fully.
For realizing the foregoing invention purpose, the technical scheme that the present invention adopts is following:
The monomeric preparation method of a kind of Semen Vaccariae flavonoid glycoside is characterized in that being undertaken by following process step:
A. raw material extracts: Semen Vaccariae is ground into meal, adds the water that 8-10 doubly measures according to mass volume ratio (kg/L), boil to boil to filter in 2 hours and extract, extract altogether 3 times, united extraction liquid is cooled to room temperature;
B. macroporous resin enrichment: the cooled extracting solution of steps A is adsorbed through the good AB-8 macroporous adsorptive resins of activation with the speed of 2 ~ 5BV; Then respectively with the water of 3 times of amount column volumes and the volume(tric)fraction 30% ethanolic soln wash-out impurity of 2 times of amount column volumes; Again with 2 times of volume(tric)fraction 50% ethanolic soln wash-out target substances of measuring column volumes; Collect elutriant, be concentrated into 1/10 of original volume;
C. efficient production liquid phase separation: behind the filtering with microporous membrane of step B gained enriching soln with the 0.45um aperture; Obtain the Semen Vaccariae flavonoid glycoside through the separation of high performance preparative liquid chromatography post again and prepare solution, get the Semen Vaccariae flavonoid glycoside aqueous solution behind the recovery organic solvent;
D. product reclaims: the step C gained Semen Vaccariae flavonoid glycoside aqueous solution is adsorbed through the good AB-8 macroporous adsorptive resins of activation with the speed of 2 ~ 5BV; Then with 2 times of volume(tric)fraction 95% ethanol elutions of measuring column volumes; Concentrate eluant is to doing; Solid got Semen Vaccariae flavonoid glycoside monomer product in 80 ℃ times dry 6 hours.
Said high performance preparative liquid chromatography column packing is octadecylsilane chemically bonded silica (C18), and the post specification is 50cm * 10cm, 50cm * 8cm or 50cm * 5cm etc.
The chromatographic condition of said efficient production liquid phase is: detect wavelength 280nm, moving phase is methanol-water, and its volume ratio is 3:7.
The invention has the advantages that:
1, step is few, weak point consuming time, and yield is high, and is easy and simple to handle, is easy to suitability for industrialized production.
2, solvent consumption is few, and the solvent in the preparative liquid chromatography separating step is all recyclable to be utilized again.
3, solvent toxicity is little, used organic solvent methyl alcohol, ethanol etc., and environmental pollution is little.
4, good in economic efficiency, can carry out scale operation, and operation is easy, only comprise 4 steps, be easy to control, separation efficiency is high.
5, has high academic value.At present domestic bibliographical information about the separation and purification of Semen Vaccariae flavonoid glycoside seldom, high performance preparative liquid chromatography is used for the monomeric separation and purification of Semen Vaccariae flavonoid glycoside and belongs to first.Products obtained therefrom of the present invention not only can be used as Semen Vaccariae flavonoid glycoside reference substance, also can be suitability for industrialized production Semen Vaccariae flavonoid glycoside preparation highly purified raw material is provided.
Description of drawings
Fig. 1 is the embodiment of the invention 1 a step C efficient production liquid phase separation on-line monitoring collection of illustrative plates
Fig. 2 is that the monomeric HPLC of the embodiment of the invention 1 Semen Vaccariae flavonoid glycoside detects collection of illustrative plates.
Embodiment
Embodiment 1
The monomeric preparation method of a kind of Semen Vaccariae flavonoid glycoside is characterized in that being undertaken by following process step:
A. raw material extracts: 5kg is ground into meal with the Semen Vaccariae medicinal material, adds 50L water, and heating is boiled and boiled 2 hours, filters; Add 50L water in the filter residue again, boil with method and boil 2 hours, filter; Add 50L water in the filter residue once more, boil with method and boil 2 hours, filter, merging filtrate is placed and is cooled to room temperature;
B. macroporous resin enrichment: take by weighing 2kg AB-8 macroporous adsorbent resin, load resin post, the about 6L of resin bed volume with diameter 15cm glass column; The cooled filtrating of steps A is adsorbed through the good macroporous adsorptive resins of activation with the speed of 4BV; Use 18L water and 12L volume(tric)fraction 30% ethanolic soln wash-out impurity then respectively; Use 12L volume(tric)fraction 50% ethanolic soln wash-out target substance again, collect elutriant, be concentrated into about 1L;
C. efficient production liquid phase separation: with the filtering with microporous membrane of step B gained enriching soln with the 0.45um aperture; Separate through the high performance preparative liquid chromatography post; Collect Semen Vaccariae flavonoid glycoside section and prepare solution, the preparation solution decompression that will collect then concentrate recovery methyl alcohol to do not have alcohol distinguish the flavor of the Semen Vaccariae flavonoid glycoside aqueous solution.
Said high performance preparative liquid chromatography column packing is octadecylsilane chemically bonded silica (C
18), the post specification is 50cm * 8cm; Detect wavelength 280nm, moving phase is volume(tric)fraction 30% methanol solution.
D. product reclaims: take by weighing 500g AB-8 macroporous adsorbent resin, load resin post, the about 1.5L of resin bed volume with diameter 10cm glass column; The step C gained Semen Vaccariae flavonoid glycoside aqueous solution is adsorbed through the good macroporous adsorptive resins of activation with the speed of 4BV; Use 3L volume(tric)fraction 95% ethanol elution then; Concentrate eluant is to doing, and 80 ℃ of dryings of solid 6 hours get Semen Vaccariae flavonoid glycoside monomer.
The heavy 22g of gained Semen Vaccariae flavonoid glycoside monomer, the HPLC purity check is 99.3%.
Embodiment 2
The monomeric preparation method of a kind of Semen Vaccariae flavonoid glycoside is characterized in that being undertaken by following process step:
A. raw material extracts: 10kg is ground into meal with the Semen Vaccariae medicinal material, adds 80L water, and heating is boiled and boiled 2 hours, filters; Add 80L water in the filter residue again, boil with method and boil 2 hours, filter; Add 80L water in the filter residue once more, boil with method and boil 2 hours, filter, merging filtrate is placed and is cooled to room temperature;
B. macroporous resin enrichment: take by weighing 4kg AB-8 macroporous adsorbent resin, load resin post, the about 12L of resin bed volume with diameter 20cm glass column; Cooled extracting solution is adsorbed through the good macroporous adsorptive resins of activation with the speed of 3BV; Use 36L water and 24L volume(tric)fraction 30% ethanolic soln wash-out impurity then respectively; Use 24L volume(tric)fraction 50% ethanolic soln wash-out target substance again, collect elutriant, be concentrated into about 2.5L;
C. efficient production liquid phase separation: with the filtering with microporous membrane of step B gained enriching soln with the 0.45um aperture; Separate through the high performance preparative liquid chromatography post; Collect Semen Vaccariae flavonoid glycoside section and prepare solution, the preparation solution decompression that will collect then concentrate recovery methyl alcohol to do not have alcohol distinguish the flavor of the Semen Vaccariae flavonoid glycoside aqueous solution.
Said high performance preparative liquid chromatography column packing is octadecylsilane chemically bonded silica (C
18), the post specification is 50cm * 10cm; Detect wavelength 280nm, moving phase is volume(tric)fraction 30% methanol solution.
D. product reclaims: take by weighing 1kg AB-8 macroporous adsorbent resin, load resin post, the about 3L of resin bed volume with diameter 10cm glass column; The step C gained Semen Vaccariae flavonoid glycoside aqueous solution is adsorbed through the good macroporous adsorptive resins of activation with the speed of 3BV; Use 6L volume(tric)fraction 95% ethanol elution then; Concentrate eluant is to doing, and 80 ℃ of dryings of solid 6 hours get Semen Vaccariae flavonoid glycoside monomer.
The heavy 43.5g of gained Semen Vaccariae flavonoid glycoside monomer, the HPLC purity check is 99.2%.
Claims (3)
1. monomeric preparation method of Semen Vaccariae flavonoid glycoside is characterized in that being undertaken by following process step:
A. raw material extracts: Semen Vaccariae is ground into meal, adds the water that 8-10 doubly measures according to mass volume ratio kg/L, boil to boil to filter in 2 hours and extract, extract altogether 3 times, united extraction liquid is cooled to room temperature;
B. macroporous resin enrichment: the cooled extracting solution of steps A is adsorbed through the good AB-8 macroporous adsorptive resins of activation with the speed of 2 ~ 5BV; Then respectively with the water of 3 times of amount column volumes and the volume(tric)fraction 30% ethanolic soln wash-out impurity of 2 times of amount column volumes; Again with 2 times of volume(tric)fraction 50% ethanolic soln wash-out target substances of measuring column volumes; Collect elutriant, be concentrated into 1/10 of original volume;
C. efficient production liquid phase separation: behind the filtering with microporous membrane of step B gained enriching soln with the 0.45um aperture; Obtain the Semen Vaccariae flavonoid glycoside through the separation of high performance preparative liquid chromatography post again and prepare solution, get the Semen Vaccariae flavonoid glycoside aqueous solution behind the recovery organic solvent;
D. product reclaims: the step C gained Semen Vaccariae flavonoid glycoside aqueous solution is adsorbed through the good AB-8 macroporous adsorptive resins of activation with the speed of 2 ~ 5BV; Then with 2 times of volume(tric)fraction 95% ethanol elutions of measuring column volumes; Concentrate eluant is to doing; Solid got Semen Vaccariae flavonoid glycoside monomer product in 80 ℃ times dry 6 hours.
2. according to the monomeric preparation method of the said Semen Vaccariae flavonoid glycoside of claim 1, it is characterized in that said high performance preparative liquid chromatography column packing is an octadecylsilane chemically bonded silica, the post specification is 50cm * 10cm, 50cm * 8cm or 50cm * 5cm.
3. according to the monomeric preparation method of claim 1 Semen Vaccariae flavonoid glycoside, it is characterized in that the chromatographic condition of said efficient production liquid phase is: detect wavelength 280nm, moving phase is methanol-water, and its volume ratio is 3:7.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102376A (en) * | 2012-12-05 | 2013-05-15 | 江南大学 | Separation method for simultaneously separating cowherb seed flavonoid glycoside and cowherb seed total saponin |
| CN103304611A (en) * | 2013-06-18 | 2013-09-18 | 聊城大学 | Method for separating and purifying three flavonoid glycosides from trichosanthes bark |
| CN109632994A (en) * | 2018-12-21 | 2019-04-16 | 广东方制药有限公司 | The method for building up of the UPLC map of the seed of cowherb and Semen Vaccariae (parched) and application |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102376A (en) * | 2012-12-05 | 2013-05-15 | 江南大学 | Separation method for simultaneously separating cowherb seed flavonoid glycoside and cowherb seed total saponin |
| CN103102376B (en) * | 2012-12-05 | 2016-08-31 | 江南大学 | A kind of separation method concurrently separating Vaccarin and Semen Vaccariae total saponins |
| CN103304611A (en) * | 2013-06-18 | 2013-09-18 | 聊城大学 | Method for separating and purifying three flavonoid glycosides from trichosanthes bark |
| CN103304611B (en) * | 2013-06-18 | 2016-06-15 | 山东中医药大学 | A kind of method of separation and purification 3 kinds of flavonoid glycosides from Snakegourd Peel |
| CN109632994A (en) * | 2018-12-21 | 2019-04-16 | 广东方制药有限公司 | The method for building up of the UPLC map of the seed of cowherb and Semen Vaccariae (parched) and application |
| CN109632994B (en) * | 2018-12-21 | 2022-05-03 | 广东一方制药有限公司 | Method for establishing UPLC (ultra Performance liquid chromatography) spectrum of cowherb seed and fried cowherb seed and application of UPLC spectrum |
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Application publication date: 20120404 |