CN108362809A - A kind of quality evaluating method of ginkgo leaf and its extract and preparation - Google Patents
A kind of quality evaluating method of ginkgo leaf and its extract and preparation Download PDFInfo
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- 235000008100 Ginkgo biloba Nutrition 0.000 title claims abstract description 49
- 241000218628 Ginkgo Species 0.000 title claims abstract description 48
- 235000011201 Ginkgo Nutrition 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000000284 extract Substances 0.000 title claims abstract description 21
- 239000013558 reference substance Substances 0.000 claims abstract description 46
- 238000012937 correction Methods 0.000 claims abstract description 27
- 238000001514 detection method Methods 0.000 claims abstract description 19
- 239000007791 liquid phase Substances 0.000 claims abstract description 15
- 238000005259 measurement Methods 0.000 claims abstract description 11
- 229930003935 flavonoid Natural products 0.000 claims abstract description 10
- 150000002215 flavonoids Chemical class 0.000 claims abstract description 10
- 235000017173 flavonoids Nutrition 0.000 claims abstract description 10
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 claims description 40
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 claims description 34
- 239000012071 phase Substances 0.000 claims description 34
- 229930003944 flavone Natural products 0.000 claims description 28
- 235000011949 flavones Nutrition 0.000 claims description 28
- IYRMWMYZSQPJKC-UHFFFAOYSA-N kaempferol Chemical compound C1=CC(O)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 IYRMWMYZSQPJKC-UHFFFAOYSA-N 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 21
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 claims description 21
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 claims description 20
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 claims description 20
- 229930182470 glycoside Natural products 0.000 claims description 20
- 235000005875 quercetin Nutrition 0.000 claims description 20
- 229960001285 quercetin Drugs 0.000 claims description 20
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 claims description 18
- 150000002212 flavone derivatives Chemical class 0.000 claims description 18
- 150000001875 compounds Chemical class 0.000 claims description 16
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 239000000047 product Substances 0.000 claims description 15
- UBSCDKPKWHYZNX-UHFFFAOYSA-N Demethoxycapillarisin Natural products C1=CC(O)=CC=C1OC1=CC(=O)C2=C(O)C=C(O)C=C2O1 UBSCDKPKWHYZNX-UHFFFAOYSA-N 0.000 claims description 14
- 235000008777 kaempferol Nutrition 0.000 claims description 14
- UXOUKMQIEVGVLY-UHFFFAOYSA-N morin Natural products OC1=CC(O)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 UXOUKMQIEVGVLY-UHFFFAOYSA-N 0.000 claims description 14
- 239000000523 sample Substances 0.000 claims description 12
- 229930182478 glucoside Natural products 0.000 claims description 11
- 239000012085 test solution Substances 0.000 claims description 11
- 239000009429 Ginkgo biloba extract Substances 0.000 claims description 10
- 150000002213 flavones Chemical class 0.000 claims description 10
- 235000020686 ginkgo biloba extract Nutrition 0.000 claims description 10
- 229940068052 ginkgo biloba extract Drugs 0.000 claims description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- 239000004615 ingredient Substances 0.000 claims description 8
- 239000012488 sample solution Substances 0.000 claims description 7
- GQODBWLKUWYOFX-UHFFFAOYSA-N Isorhamnetin Natural products C1=C(O)C(C)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 GQODBWLKUWYOFX-UHFFFAOYSA-N 0.000 claims description 6
- 238000004364 calculation method Methods 0.000 claims description 6
- 150000002338 glycosides Chemical class 0.000 claims description 6
- IZQSVPBOUDKVDZ-UHFFFAOYSA-N isorhamnetin Chemical compound C1=C(O)C(OC)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 IZQSVPBOUDKVDZ-UHFFFAOYSA-N 0.000 claims description 6
- 235000008800 isorhamnetin Nutrition 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000010828 elution Methods 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 2
- 238000010276 construction Methods 0.000 claims description 2
- 238000007865 diluting Methods 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims 1
- 238000004811 liquid chromatography Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 7
- 239000003814 drug Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 238000003908 quality control method Methods 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000825 pharmaceutical preparation Substances 0.000 abstract description 2
- 230000014759 maintenance of location Effects 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 6
- 239000011550 stock solution Substances 0.000 description 5
- 238000001914 filtration Methods 0.000 description 4
- LKZDFKLGDGSGEO-UJECXLDQSA-N kaempferol 3-O-beta-D-glucosyl-(1->2)-beta-D-glucoside Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@H]1[C@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=CC(O)=CC=2)=O)O[C@H](CO)[C@@H](O)[C@@H]1O LKZDFKLGDGSGEO-UJECXLDQSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 3
- RTATXGUCZHCSNG-TYSPDFDMSA-N Kaempferol-3-O-rutinoside Natural products OC1[C@H](O)[C@@H](O)C(C)O[C@H]1OCC1[C@@H](O)[C@@H](O)C(O)[C@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=CC(O)=CC=2)=O)O1 RTATXGUCZHCSNG-TYSPDFDMSA-N 0.000 description 3
- RTATXGUCZHCSNG-QHWHWDPRSA-N Nicotiflorin Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=CC(O)=CC=2)=O)O1 RTATXGUCZHCSNG-QHWHWDPRSA-N 0.000 description 3
- IKGXIBQEEMLURG-UHFFFAOYSA-N Rutin Chemical compound OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-UHFFFAOYSA-N 0.000 description 3
- 238000010812 external standard method Methods 0.000 description 3
- CFYMYCCYMJIYAB-UHFFFAOYSA-N laricitrin Chemical compound OC1=C(O)C(OC)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 CFYMYCCYMJIYAB-UHFFFAOYSA-N 0.000 description 3
- 239000012982 microporous membrane Substances 0.000 description 3
- RTATXGUCZHCSNG-ZFDPGQBLSA-N nicotiflorin Natural products O(C[C@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](OC2=C(c3ccc(O)cc3)Oc3c(c(O)cc(O)c3)C2=O)O1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@H](C)O1 RTATXGUCZHCSNG-ZFDPGQBLSA-N 0.000 description 3
- RTATXGUCZHCSNG-UHFFFAOYSA-N nicotiflorine Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=CC(O)=CC=2)=O)O1 RTATXGUCZHCSNG-UHFFFAOYSA-N 0.000 description 3
- 238000003556 assay Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 244000194101 Ginkgo biloba Species 0.000 description 1
- 241000218791 Ginkgoaceae Species 0.000 description 1
- 244000062250 Kaempferia rotunda Species 0.000 description 1
- 235000013422 Kaempferia rotunda Nutrition 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 244000018633 Prunus armeniaca Species 0.000 description 1
- 235000009827 Prunus armeniaca Nutrition 0.000 description 1
- 241001093501 Rutaceae Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229930182486 flavonoid glycoside Natural products 0.000 description 1
- 150000007955 flavonoid glycosides Chemical class 0.000 description 1
- 150000008131 glucosides Chemical class 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000013441 quality evaluation Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- DKVBOUDTNWVDEP-NJCHZNEYSA-N teicoplanin aglycone Chemical compound N([C@H](C(N[C@@H](C1=CC(O)=CC(O)=C1C=1C(O)=CC=C2C=1)C(O)=O)=O)[C@H](O)C1=CC=C(C(=C1)Cl)OC=1C=C3C=C(C=1O)OC1=CC=C(C=C1Cl)C[C@H](C(=O)N1)NC([C@H](N)C=4C=C(O5)C(O)=CC=4)=O)C(=O)[C@@H]2NC(=O)[C@@H]3NC(=O)[C@@H]1C1=CC5=CC(O)=C1 DKVBOUDTNWVDEP-NJCHZNEYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The quality evaluating method of a kind of ginkgo leaf and its extract and preparation, belongs to the technical field of quality detection of Chinese medicine.The present invention surveys by one by the high-efficiency liquid-phase fingerprint of structure ginkgo chemical composition and comments method more, calculate correction factor, realize the measurement to a variety of flavonoids contents in ginkgo.This method is easy to operate, stability is good, both the quality of ginkgo leaf and its extract and preparation can objective, comprehensive, have accurately been evaluated, and it is used for its quality control, also solve the problem that due to reference substance lacks can not objective the problem of reasonably controlling medicinal material and its extract or the quality of the pharmaceutical preparations, to control quality and ensure that curative effect is of great significance.
Description
Technical field
The present invention relates to the technical field of quality detection of Chinese medicine, and in particular to one kind based on high-efficiency liquid-phase fingerprint and
One surveys the quality evaluating method of the ginkgo leaf of more evaluation amount methods and its extract and preparation.
Technical background
Ginkgo leaf is Ginkgoaceae plant Ginkgo bilobaGinkgo bilobaL. dried leaf, have it is promoting blood circulation and removing blood stasis, remove obstruction in channels to relieve pain,
The effect of astringing the lung and relieving asthma, changing turbid lipid-loweringing.Ginkgo chemical composition is abundant, including flavonoids, lactone and phenolic acid class etc., wherein ginkgo
Flavone component content is most, and composition is various, can improve each of cardio-cerebrovascular with the ginkgo biloba extract that general flavone content is 24%
Kind disease, and it is without side-effects.
The approval of domestic and international field of medicaments is obtained in ginkgo biloba extract and ginkgo agent Related product and obtains mass market
The quality evaluating method of today of demand, ginkgo are most important.Currently, at 2015 editions《Chinese Pharmacopoeia》Ginkgo leaf quality standard
In：General flavone content is evaluated and is controlled by the content of Quercetin, Kaempferol and Isorhamnetin after measurement sour water solution, should
Not only pre-treatment is cumbersome for method, and time-consuming, and cannot fully reflect the true and exact level of flavones ingredient.In addition, having
Research, which is reported, to be established the analyses of a variety of flavonoids in ginkgo leaf and its extract using HPLC-UV technologies and comments
Valence method, but institute's testing index reference substance separation preparation difficulty is big, analysis cost is high, not as ginkgo quality of medicinal material control method
Easily promote.Therefore, it in order to fully control the quality and clinical safety of ginkgo leaf medicinal material and its extract and its preparation, develops
It is a kind of it is simple and easy to do, testing cost is cheap, and can Simultaneous Quantitative Analysis a variety of active ingredients analysis method, for ginkgo and its
The quality control of extract and preparation has realistic meaning.
For this purpose, the present invention provides it is a kind of based on high-efficiency liquid-phase fingerprint and one survey more evaluation amount methods ginkgo leaf and its
The quality evaluating method of extract and preparation.A kind of flavone component in ginkgo is passed through into relative correction factor as internal reference object
It calculates, realizes the measurement to a variety of flavonoids contents in ginkgo.This method is easy to operate, and stability is good, both can be with
Quality that is objective, comprehensive, accurately evaluating ginkgo leaf and its extract and preparation, also solving the problem that can not visitor due to reference substance lacks
The problem of reasonably evaluating quality is seen, to control quality and ensures that curative effect is of great significance.
Invention content
Contain in view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a variety of flavone components in a kind of measurement ginkgo
Quantity measuring method, this method can accurately evaluate the quality of ginkgo leaf and its extract and general flavone in preparation, can also solve
It can not objective the problem of reasonably controlling Chinese medicine and its quality of the pharmaceutical preparations certainly due to reference substance lacks.
To achieve the goals above, the present invention adopts the following technical scheme that：
The quality evaluating method of a kind of ginkgo leaf and its extract and preparation is provided, this method is by using high performance liquid chromatography skill
Art and a survey comment method more, and multiple flavonoids in ginkgo are carried out with the measurement of content, realize ginkgo leaf and its carry
Objective, comprehensive, the accurately quality evaluation of object and preparation, the assay of flavonoids is taken to refer to ginkgo leaf and its carry
The assay of a variety of flavones reference substances in object and preparation is taken, the quantity of flavonoids is 8-16 kinds.
Specifically include following steps：
1）The preparation of reference substance solution：Precision weighs each flavones reference substance 1-5mg and is placed in volumetric flask respectively, with 80-100% first
Alcohol dissolves constant volume, then filters, and each single reference substance storing solution is made, and it is molten then to measure different volumes single standard product respectively
Liquid, the mixing sample of the flavone component containing there are many is made in mixed diluting, spare as mixed reference substance solution；
2）The preparation of test solution：Precision weighs ginkgo leaf, ginkgo biloba extract or ginkgo agent, and a concentration of 50- is added
100% methanol, ultrasound or heating extraction, filtering, take subsequent filtrate to cross 0.45um or 0.22um filter membranes, obtain sample solution；
3）The calculating of correction factor RCF：Take step 1）In mixed reference substance solution 2-20 μ L obtained, surveyed with high performance liquid chromatography
Fixation spectrogram simultaneously calculates peak area, selects one of compound as internal reference object, calculates separately the internal reference object and other chemical combination
Relative correction factor f between objectk/s。
Wherein, relative correction factor calculation formula is：fk/s=fk/fs=AkCs/(AsCk).In formula：AsFor internal reference object peak face
Product；CsFor internal reference object concentration；AkFor the peak area of certain component k to be measured；CkFor the concentration of certain component k to be measured.
4）The measurement of active constituent in sample：Take step 2）In test solution 2-20 μ L obtained, with using efficient liquid phase
Chromatographic determination chromatogram calculates separately out the quality of other flavone components as follows；
The formula is：Wk=（Ws╳Ak)/(fk/s╳As）, WkTo be tested the quality of component, WsFor the quality of internal reference object, AkFor quilt
Survey the peak area of component, fk/sFor correction factor, AsFor the peak area of internal reference object.
The present invention by measure ginkgo leaf and its middle 8-16 kinds content of extract and preparation are high, activity is good flavonoid glycoside and
The total amount of a variety of flavones reference substances of its aglycon ingredient, the content of accurate evaluation Total Ginkgo Flavone-Glycoides.
Flavones reference substance includes Quercetin -3-O- (- two-O- α-L- rhamnopyranosyls of 2'', 6 ")-β-D-Glucoses glycosides, kaempferia galamga
Phenol -3-0- (- two-O- α-L- rhamnopyranosyls of 2'', 6 ")-β-D-Glucoses glycosides, Kaempferol -3-O- β sophoroside, Quercetin -3-O-
Rutinose -7-O- glucosides, 3'- methyl-myricetin -3-O- rutinosides, Quercetin 3-O- glucosides, Quercetin 3-
O- (2- β-D-Glucose base-alpha-L-rhamnoside), kaempferol-3-O-rutinoside, Isorhamnetin -3-O- β-D- rutinoses
Glycosides, Kaempferol 3- (2''- β-D-Glucose glycosides)-alpha-L-rhamnoside, Quercetin 3-O- α-(6'''-p- coumaric acyls-Portugal
Polyglycoside-β -1,4- rhamnosides), Kaempferol 3-O- α-(6'''-p- coumaric acyls-glucoside-β -1,2- rhamnoses
Glycosides).
The present invention ensures that flavonoids compares ingredient by high-efficient liquid phase chromatogram technology construction feature liquid-phase fingerprint
With good separation degree（Separating degree >=1.2）.
High performance liquid chromatography detection condition is：The detector of high performance liquid chromatograph is using diode array detector or leads to
It is water-soluble with 0.1% formic acid using acetonitrile as mobile phase A using eight or octadecylsilane chemically bonded silica as filler with type detector
Liquid is Mobile phase B, gradient elution, and during gradient elution, mobile phase A, the variation of the ratio of B are：0-20min, A phase 15%-20%,
B phases 85%-80%；20-25min, A phase 20%-30%, B phase 80%-70%；25-30min, A phase 30%-35%, B phase 70%-65%； 30-
45min, A phase 35%-40%, B phase 65%-60%.It is Detection wavelength for 210nm-360nm to use UV detector.Flow velocity is
0.5ml/min-1.5ml/min keeps 20-45 DEG C of column temperature.
High-efficiency liquid-phase fingerprint is obtained using above-mentioned condition, each spectrogram similarity is not less than 0.90, the RSD of each peak area
It is not higher than 2%.
Performance liquid chromatographic column model is preferably Gemini C18 in the present invention（250mm × 4.6 mm, 5.0 μm）, flow velocity
Preferably 0.8mL/min, Detection wavelength are preferably 360nm, and column temperature is preferably 35oC.
The present invention surveys using one and comments method more, using one of which ingredient as internal reference object, passes through relative correction factor, respectively
Calculate the content of each compound.Wherein, relative correction factor calculation formula is：fk/s=fk/fs=AkCs/(AsCk).In formula：As
For internal reference object peak area；CsFor internal reference object concentration；AkFor the peak area of certain component k to be measured；CkFor the concentration of certain component k to be measured.
The present invention has the following advantages：
1）Compared with conventional method, the present invention solves Chinese medicine multicomponent quantitatively and operation present in multi objective quality control is numerous
The problems such as trivial, reference substance lacks, realizes the control of multi objective synchronizing quality, in accurately reflecting while reducing detection ingredient
Medicine product quality.
2）The present invention surveys high-efficient liquid phase chromatogram technology with one comments method to be combined more, has both met fingerprint similarity and has wanted
It asks and the dual product up to standard for meeting content requirement is confirmed to be qualified products, for the quality one between control different batches of product
Cause property is of great significance.
3）The method of the present invention is surveyed by one and is commented method simultaneous quantitative silver-colored more with a kind of product as a contrast of flavone component in ginkgo
In apricot Quercetin and its glycoside, Kaempferol and its glycoside, Isorhamnetin and its a variety of flavones such as glycoside and ginkegetin at
Point content, the content of general flavone in accurate evaluation ginkgo leaf and its extract and preparation.
4）Provided by the present invention one survey comments method easy to operate, and multi objective quality evaluating method stability is good, can be with
Quality that is objective, comprehensive, accurately evaluating ginkgo leaf and its extract and preparation, avoids in conventional method by measuring flavones
The evaluation method of ingredient hydrolysate content can effectively prevent product fraud, change the problems such as technique.
Description of the drawings
Fig. 1 is the high-efficient liquid phase chromatogram of ginkgo biloba p.e.
Fig. 2 is the high-efficient liquid phase chromatogram of the ginkgo leaf hybrid standard product of 8 kinds of chromocor compounds composition.
Fig. 3 is the high-efficient liquid phase chromatogram of the ginkgo leaf hybrid standard product of 10 kinds of chromocor compounds composition.
Fig. 4 is the high-efficient liquid phase chromatogram of the ginkgo leaf hybrid standard product of 12 kinds of chromocor compounds composition.
Specific implementation mode
With reference to specific embodiment, the present invention is furture elucidated, it should be understood that these embodiments be merely to illustrate the present invention and
It is not used in the range for first heading direct for invention, modification bacterium colony and this Shen of the those skilled in the art for the various equivalent forms of the present invention
It please claim of ownership limited range.
Chromatographic condition used in following embodiment：
1）Instrument：High performance liquid chromatograph（China spectrum S6000, Dalian Hua Pu developments in science and technology Co., Ltd）；
2）Analyze chromatographic column：Gemini C18（250mm × 4.6 mm, 5.0 μm, U.S.'s phenomenex company）；
3）Mobile phase：Using acetonitrile as mobile phase A, using 0.1% aqueous formic acid as Mobile phase B,
4）Gradient condition：Mobile phase A, the variation of the ratio of B are：0-23min, 16-17%A, 23-25min, 17-20%A,
25-40min, 20%A, 40-45min, 20-28%A, 45-48m in, 28-35%A, 48-60min, 35%A
5）Detector condition：UV detector, Detection wavelength 360nm
6）Flow velocity is 0.8ml/min；
7）35 DEG C of column temperature.
Embodiment 1
It is described in detail with reference to Fig. 2 and embodiment：
1）Reference substance
Quercetin -3-O- (- two-O- α-L- rhamnopyranosyls of 2'', 6 ")-β-D-Glucose glycosides（1）, Kaempferol -3-0- (2'', 6 " -
Two-O- α-L- rhamnopyranosyls)-β-D-Glucose glycosides（2）, Quercetin -3-O- rutinose -7-O- glucosides（3）, Quercetin
3-O- glucosides（4）, Isorhamnetin -3-O- β-D- rutinosides（5）, Kaempferol 3- (2''- β-D-Glucose glycosides)-α-L-
Rhamnoside（6）, Quercetin 3-O- α-(6'''-p- coumaric acyls-glucoside-β -1,4- rhamnosides)（7）, Kaempferol
3-O- α-(6'''-p- coumaric acyls-glucoside-β -1,2- rhamnosides)（8）.
2）The preparation of sample solution
Precision weighs ginkgo biloba extract powder 5.0mg in volumetric flask, and methanol dissolving is added, and ultrasonic 5min is settled to 20mL, shakes
It is even, with 0.22 μm of filtering with microporous membrane, it is test solution, analysis detection is carried out using high performance liquid chromatography.
3）The preparation of reference substance solution
Precision weighs 8 kinds of each 1.0mg of GINKGO BILOBA EXTRACT monomeric compound in step 1), respectively in volumetric flask, methanol is added to dissolve and determine
Hold to 2ml, shakes up, the stock solution of each reference substance, a concentration of 0.5mg/mL is made.Precision measures the stock solution of each reference substance
2.0mL is placed in the volumetric flask of same 25mL, is added methanol to dissolve and is diluted to scale, is shaken up to get reference substance mixed solution,
Filter membrane enters high performance liquid chromatograph.
4）The calculating of correction factor
Take step 3）In 10 μ L of mixed reference substance solution obtained, measure chromatogram with high performance liquid chromatography and calculate peak area,
It selects No. 4 reference substances as internal reference object, calculates separately the relative correction factor f between the internal reference object and other compoundsk/s.Phase
It is to correction factor calculation formula：fk/s=fk/fs=AkCs/(AsCk).In formula：AsFor internal standard compound peak area；CsIt is dense for internal standard compound
Degree；AkFor the peak area of certain component k to be measured；CkFor the concentration of certain component k to be measured.
4）The measurement of other flavone components
Take step 2）In 10 μ L of test solution obtained, with high performance liquid chromatography measure chromatogram, count respectively as follows
Calculate the quality of other flavone components；
The formula is：Wk=（Ws╳Ak)/(fk/s╳As）, WkTo be tested the quality of component, WsFor the quality of internal reference object, AkFor quilt
Survey the peak area of component, fk/sFor correction factor, AsFor the peak area of internal reference object.
Its gradient condition：Mobile phase A, the variation of the ratio of B are：0-23min, 16-17%A, 23-25min, 17-
20%A, 25-40min, 20%A, 40-45min, 20-28%A, 45-48m in, 28-35%A, 48-60min, 35%
A;
Embodiment 2
It is described in detail with reference to Fig. 3 and embodiment：
1）Reference substance
Quercetin -3-O- (- two-O- α-L- rhamnopyranosyls of 2'', 6 ")-β-D-Glucose glycosides（1）, Kaempferol -3-0- (2'', 6 " -
Two-O- α-L- rhamnopyranosyls)-β-D-Glucose glycosides（2）, Quercetin -3-O- rutinose -7-O- glucosides（3）, 3'- methyl-
Myricetin -3-O- rutinosides（4）, Quercetin 3-O- glucosides（5）, kaempferol-3-O-rutinoside（6）, different sandlwood
Element -3-O- β-D- rutinosides（7）, Kaempferol 3- (2''- β-D-Glucose glycosides)-alpha-L-rhamnoside（8）, Quercetin 3-
O- α-(6'''-p- coumaric acyls-glucoside-β -1,4- rhamnosides)（9）, Kaempferol 3-O- α-(6'''-p- coumaric acyls
Base-glucoside-β -1,2- rhamnosides)（10）.
2）The preparation of sample solution
Precision weighs ginkgo biloba extract powder 5.0mg in volumetric flask, and methanol dissolving is added, and ultrasonic 5min is settled to 20mL, shakes
It is even, with 0.22 μm of filtering with microporous membrane, it is test solution, analysis detection is carried out using high performance liquid chromatography.
3）The preparation of reference substance solution
Precision weighs 10 kinds of each 1.0mg of GINKGO BILOBA EXTRACT monomeric compound in step 1), respectively in volumetric flask, methanol is added to dissolve and determine
Hold to 2.0ml, shakes up, the stock solution of each reference substance, a concentration of 0.5mg/mL is made.The reserve that precision measures each reference substance is molten
Liquid 2.0mL is placed in the volumetric flask of same 25mL, is added methanol to dissolve and is diluted to scale, is shaken up molten to get reference substance mixing
Liquid, filter membrane enter high performance liquid chromatograph.
4）The calculating of correction factor
Take step 3）In 10 μ L of mixed reference substance solution obtained, measure chromatogram with high performance liquid chromatography and calculate peak area,
It selects No. 5 reference substances as internal reference object, calculates separately the relative correction factor f between the internal reference object and other compoundsk/s.Phase
It is to correction factor calculation formula：fk/s=fk/fs=AkCs/(AsCk).In formula：AsFor internal standard compound peak area；CsIt is dense for internal standard compound
Degree；AkFor the peak area of certain component k to be measured；CkFor the concentration of certain component k to be measured.
4）The measurement of other flavone components
Take step 2）In 10 μ L of test solution obtained, with high performance liquid chromatography measure chromatogram, count respectively as follows
Calculate the quality of other flavone components；
The formula is：Wk=（Ws╳Ak)/(fk/s╳As）, WkTo be tested the quality of component, WsFor the quality of internal reference object, AkFor quilt
Survey the peak area of component, fk/sFor correction factor, AsFor the peak area of internal reference object.
Its gradient condition：Mobile phase A, the variation of the ratio of B are：0-23min, 16-17%A, 23-25min, 17-
20%A, 25-40min, 20%A, 40-45min, 20-28%A, 45-48m in, 28-35%A, 48-60min, 35%
A;
Embodiment 3
It is described in detail with reference to Fig. 4 and embodiment：
1）Reference substance
Quercetin -3-O- (- two-O- α-L- rhamnopyranosyls of 2'', 6 ")-β-D-Glucose glycosides（1）, Kaempferol -3-0- (2'', 6 " -
Two-O- α-L- rhamnopyranosyls)-β-D-Glucose glycosides（2）, Kaempferol -3-O- β sophoroside（3）, Quercetin -3-O- rutinoses -7-
O- glucosides（4）, 3'- methyl-myricetin -3-O- rutinosides（5）, Quercetin 3-O- glucosides（6）, Quercetin 3-
O- (2- β-D-Glucose base-alpha-L-rhamnoside)（7）, kaempferol-3-O-rutinoside（8）, Isorhamnetin -3-O- β-D- rues
Fragrant glucosides（9）, Kaempferol 3- (2''- β-D-Glucose glycosides)-alpha-L-rhamnoside（10）, Quercetin 3-O- α-(6'''-p-
Coumaric acyl-glucoside-β -1,4- rhamnosides)（11）, Kaempferol 3-O- α-(6'''-p- coumaric acyls-glucoside-
β -1,2- rhamnosides)（12）.
2）The preparation of sample solution
Precision weighs ginkgo biloba extract powder 5.0mg in volumetric flask, and methanol dissolving is added, and ultrasonic 5min is settled to 20mL, shakes
It is even, with 0.22 μm of filtering with microporous membrane, it is test solution, analysis detection is carried out using high performance liquid chromatography.
3）The preparation of reference substance solution
Precision weighs 12 kinds of each 1.0mg of GINKGO BILOBA EXTRACT monomeric compound in step 1), respectively in volumetric flask, methanol is added to dissolve and determine
Hold to 2ml, shakes up, the stock solution of each reference substance, a concentration of 0.5mg/mL is made.Precision measures the stock solution of each reference substance
1.5mL is placed in the volumetric flask of same 25mL, is added methanol to dissolve and is diluted to scale, is shaken up to get reference substance mixed solution,
Filter membrane enters high performance liquid chromatograph.
4）The calculating of correction factor
Take step 3）In 10 μ L of mixed reference substance solution obtained, measure chromatogram with high performance liquid chromatography and calculate peak area,
It selects No. 6 reference substances as internal reference object, calculates separately the relative correction factor f between the internal reference object and other compoundsk/s.Phase
It is to correction factor calculation formula：fk/s=fk/fs=AkCs/(AsCk).In formula：AsFor internal standard compound peak area；CsIt is dense for internal standard compound
Degree；AkFor the peak area of certain component k to be measured；CkFor the concentration of certain component k to be measured.
4）The measurement of other flavone components
Take step 2）In 10 μ L of test solution obtained, with high performance liquid chromatography measure chromatogram, count respectively as follows
Calculate the quality of other flavone components；
The formula is：Wk=（Ws╳Ak)/(fk/s╳As）, WkTo be tested the quality of component, WsFor the quality of internal reference object, AkFor quilt
Survey the peak area of component, fk/sFor correction factor, AsFor the peak area of internal reference object.
Its gradient condition：Mobile phase A, the variation of the ratio of B are：0-23min, 16-17%A, 23-25min, 17-
20%A, 25-40min, 20%A, 40-45min, 20-28%A, 45-48m in, 28-35%A, 48-60min, 35%
A;
Embodiment 4
With reference to the present invention is further described with Fig. 3
The case study on implementation of the investigation of methodology
1）Linear relationship, minimum detection limit (LOD) and minimum quantitative limit (LOQ) experiment
Precision draws the standard solution solution 8 that reference substance is 10 kinds of compounds, 20,40,80,160,320,640ug/ml, sample introduction
10 uL are measured, liquid chromatograph is injected, record peak area, with a concentration of abscissa of each reference substance, peak area is ordinate, is drawn
Standard curve, with S/N=3 determine method detection limit, with S/N=10 determine method quantitative limit, detection limit, quantitative limit and
The parameters such as equation of linear regression, the linear relationship (r as a result shown2More than or equal to 0.9993), detection limit 0.13-1.11 determines
Amount limit 0.43-3.69, the RSD of relative correction factor is in 0.23-1.34, and relative retention time is in 0.05-0.72.
Regression equation, the range of linearity and minimum detection limit and minimum quantitative limit
2）Precision, repeatability, stability and accuracy test：
Precision：Reference substance solution is taken, repeats sample introduction in one day respectively under determining chromatographic condition 6 times and at continuous 3 days
It is interior repeat sample introduction 6 times, day is evaluated with the relative standard deviation (RSD) and retention time (RT) of each Component peak area analyzed
Interior and day to day precision, precision result show in a few days the RSD of A (peak area) and RT (retention time) are respectively lower than 0.89,
0.75, in the daytime the RSD of A (peak area) and RT (retention time) be respectively lower than 1.86,0.6, indicate that precision is good.
Stability test：It takes with a hybrid standard product solution, injects liquid phase when 0,2,4,6,8,12,24,48
Chromatograph investigates its stability with each composition swarming area RSD and retention time (RT), and stability A (peak area) and RT (retain
Time) RSD be respectively 0.66-1.92,0.13-1.18, indicate that sample solution is stablized in 48h.
Repetitive test：Hybrid standard product solution (parallel 6 parts) is taken, sample introduction is analyzed under above-mentioned chromatographic condition, with sample
In RSD retention times (RT) value of each component content evaluate its stability, repeated A (peak area) and RT's (retention time)
RSD is respectively 0.67-1.96,0.05-0.51, indicates that sample solution repeatability is good.
Precision, repeatability and stability test
Accuracy is tested：By the accuracy of sample recovery rate experimental evaluation method, precision weighs the ginkgo of appropriate known content
Medicinal powder 1g, is added a certain amount of reference substance solution, and sample is prepared by test solution, and basic, normal, high three concentration is made
(50%, 80%, 100%) it measures, calculates sample recovery rate, the standard value of the rate of recovery=(measured value-original value)/addition, the rate of recovery
In 98.8-102.1, RSD is in 0.32-1.76, the results showed that, this method has good accuracy.
The applicability of method is investigated:
For new detecting method, experiment investigated the existing different liquid chromatograph in laboratory, different chromatographic columns and other
Influence factor (wavelength, flow velocity, column temperature, the gradient of mobile phase, gradient timetable program), the relative correction factor (RPF) of gained
And its relative retention time (RSD).
It is the premise for ensureing " one surveys comment more " method application that chromatographic peak, which is accurately positioned, is joined using relative retention time value (RRT)
Number is positioned in conjunction with chromatogram global feature.RRT=RTx/RTs, RTx:Other chromatographic peak retention times RTs：The chromatography of internal standard compound
The retention time at peak, the RSD ranges of the RCF of different liquid chromatographs are in 0.12-1.18, and the range of the RSD of RRT is in 0.2-
1.36, so influence very little of the different liquid chromatographs to method.The range of the RSD of the RCF of different wave length in 0.26-2.03,
The RSD ranges of RRT are in 0.53-1.83.The range of the RSD of RCF different in flow rate exists in 0.53-1.72, the RSD ranges of RRT
The range of the RSD of the RCF of 0.33-1.65. difference column temperatures is in 0.65-2.02, and the RSD ranges of RRT are in 0.50-1.67 mobile phase acid
RCF between 0.65-1.77, RRT between 0.46-2.30, on method influence very little.
One survey comments method and external standard method results contrast (mg/g)
Note：No. 5 peaks are Quercetin 3-O- glucosides
The method of the present invention is characterized with the correlation of external standard method acquired results with Pearson correlation coefficient it is found that the side of the present invention
Method is with external standard method acquired results without significant difference.
Claims (5)
1. the quality evaluating method of a kind of ginkgo leaf and its extract and preparation, which is characterized in that this method is by using efficient
Liquid chromatography technology and a survey comment method more, and multiple flavonoids in ginkgo are carried out with the measurement of content, specific to wrap
Include following step：
1）The preparation of reference substance solution：
Precision weighs each flavones reference substance 1-5mg and is placed in volumetric flask respectively, dissolves constant volume with 80-100% methanol, then mistake
Each single reference substance solution is made in filter；Then the single reference substance solution of different volumes is measured respectively, and mixed diluting is made containing more
The mixing sample of kind flavone component, it is spare as mixed reference substance solution；
The flavones reference substance is that Quercetin and its glycoside, Kaempferol and its glycoside, Isorhamnetin and its glycoside and ginkgo are double yellow
Ketone；The quantity of flavones reference substance is 8-16 kinds；
2）The preparation of test solution：
Precision weighs ginkgo leaf, ginkgo biloba extract or ginkgo agent, and a concentration of 50-100% methanol is added, and ultrasound or heating carry
It takes, filter, take filtrate to cross 0.45um or 0.22um filter membranes, obtain sample solution；
3）The calculating of correction factor RCF：
Take step 1）In mixed reference substance solution 2-20 μ L obtained, measured with high performance liquid chromatography and chromatogram and calculate peak face
Product, selects one of compound as internal reference object, calculate separately relative correction between the internal reference object and other compounds because
Sub- fk/s；
The relative correction factor calculation formula is：fk/s=fk/fs=AkCs/(AsCk), in formula：AsFor internal reference object peak area；Cs
For internal reference object concentration；AkFor the peak area of certain component k to be measured；CkFor the concentration of certain component k to be measured；
4）The measurement of active constituent in sample：
Take step 2）In test solution 2-20 μ L obtained, with high performance liquid chromatography measure chromatogram, divide as follows
The quality of other flavone components is not calculated；
The formula is：Wk=（Ws╳Ak)/(fk/s╳As）, WkTo be tested the quality of component, WsFor the quality of internal reference object, AkFor quilt
Survey the peak area of component, fk/sFor correction factor, As is the peak area of internal reference object.
2. the quality evaluating method of a kind of ginkgo leaf according to claim 1 and its extract and preparation, it is characterised in that：
Step 3）Described in internal reference object be Quercetin 3-O- glucosides.
3. the quality evaluating method of a kind of ginkgo leaf according to claim 1 and its extract and preparation, it is characterised in that：
It is, by relative correction factor, to calculate separately each compound using one of which ingredient as internal reference object that one survey comments method more
Content；The high-efficient liquid phase chromatogram technology is used for construction feature liquid-phase fingerprint, and ensures flavonoids control ingredient
Separating degree >=1.2；In finger-print, each spectrogram similarity is not less than 0.90, and the RSD of each peak area is not higher than 2%.
4. the quality evaluating method of a kind of ginkgo leaf according to claim 1 and its extract and preparation, it is characterised in that：
High performance liquid chromatography detection condition is：The detector of high performance liquid chromatograph uses diode array detector or universal detection
Device, using acetonitrile as mobile phase A, is flowing with 0.1% aqueous formic acid using eight or octadecylsilane chemically bonded silica as filler
Phase B, gradient elution, during gradient elution, mobile phase A, the variation of the ratio of B are：0-20min, A phase 15%-20%, B phase 85%-
80%；20-25min, A phase 20%-30%, B phase 80%-70%；25-30min, A phase 30%-35%, B phase 70%-65%；30-45min, A
Phase 35%-40%, B phase 65%-60%；It is Detection wavelength for 210nm-360nm to use UV detector；Flow velocity is 0.5ml/min-
1.5ml/min keeps 20-45 DEG C of column temperature.
5. the quality evaluating method of a kind of ginkgo leaf according to claim 4 and its extract and preparation, it is characterised in that：
The column model is Gemini C18, and specification is 250mm × 4.6 mm, 5.0 μm；Flow velocity is 0.8ml/min, Detection wavelength
For 360nm, column temperature 35oC.
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