CN102818863B - Method for identifying proanthocyanidins in ginkgo leaf preparation - Google Patents
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Abstract
The invention provides an analytic identification method for identifying that whether samples comprising a ginkgo leaf preparation, foods, healthcare products, medicines and/or cosmetics containing ginkgo leaf extracts and the like contain proanthocyanidins having other sources. The method is characterized in that a sample to be detected and a standard substance are pretreated through purifying with an polyamide resin, extracting with an organic solvent and the like; normal phase-high performance liquid chromatograms of the solution sample of the ginkgo leaf preparation to be detected and the solution substandard substance of a standard ginkgo leaf preparation are respectively established by adopting a phenomenex dihydric alcohol as a stationary phase, adopting a column having parameters of 250*4.6mm and 5mum, adopting (A)acetonitrile-(B)methanol/water/acetic acid (95/3/2, V/V/V) as a mobile phase, and adopting gradient eluting; and the chromatograms are contrasted and analyzed. The identification method has the advantages of high sensitivity, good resolution and reappearance, and obvious identification characteristic, and can accurately identify if the ginkgo leaf is added with above 0.5% of the proanthocyanidins having the other sources.
Description
Technical field
The present invention relates to the method that contains procyanidin with discriminatory analysis thing or sample to be analyzed for analyzing, be specially the discrimination method that whether has adulterated other source procyanidin in gingko leaf preparation.
Background technology
Ginkgo is one of the most ancient seeds that survive in the world at present, and its preparation, health food have become one of plant product the most popular on market, the world today.The medical value of ginkgo biloba p.e is very high, has antagonism platelet activating factor, removes free radical, anti-inflammatory, antiallergy, hemangiectasis, protection cardiovascular and cerebrovascular, improves peripheral blood circulation, reduces serum cholesterol and assists the multiple pharmacological activities such as anticancer.Ginkgolides and flavones are the principal ingredients that produces above-mentioned pharmacological activity, are also main effective constituent and the quality control index of ginkgo biloba p.e.
Research in recent years has been found to contain procyanidin in ginkgo, and it has pharmacological activity widely equally, is the another principal ingredient that gingko leaf preparation produces curative effect.
Procyanidin is that a class is polymerized by several catechin compounds, has the plant polyphenol compounds of flavan-3-alcohol structure.Procyanidin has multiple hypotype at occurring in nature, comprises that Propelargonidin(monomer is afzelechin and epiafzelechin), Procyanidin(monomer is catechin and epicatechin), Prodelphinidin(monomer is nutgall catechin and epigallocatechin), Profisetinidin(monomer is fisetinidol and table fisetinidol), Prorobinetinidin(monomer is robinetinidol and table robinetinidol).Procyanidin in different plants, monomer whose forms and ratio is all different.Majority of plant procyanidin be take Procyanidin that catechin and epicatechin form as main.Ginkgo procyanidin is mainly comprised of nutgall catechin and epigallocatechin, i.e. Prodelphinidin, and its ratio is up to 85%.Up to the present, Prodelphinidin only finds to be present in the medulla and ginkgo leaf of pecan tree (Carya illionensis).
For analyzing the method for procyanidin, have a lot, once had scholar to apply positive-high performance liquid chromatography the procyanidin of cocoa, strawberry is carried out to separation by degree of polymerization size, this is the means that a kind of effective analysis procyanidin forms.But at present, the research of ginkgo procyanidin is still in the starting stage, and the analysis to procyanidin in gingko leaf preparation, comprises qualitative and quantitative analysis, all there is no bibliographical information.
Because the examination criteria of present national gingko leaf preparation product is lower, caused illegal businessman with other at a low price product mix in ginkgo in formulation products, prepare and detect qualified gingko leaf preparation fake products, jeopardize the people's drug safety, greatly dangerous.At present to the existing specific method of the detection of GINKGO BILOBA EXTRACT, but it has relatively high expectations, and applies limited.And the true and false discriminating of procyanidin has no relevant report in gingko leaf preparation, in context of detection, be therefore a blank.
Summary of the invention
The object of the present invention is to provide a kind of for analyzing the method for gingko leaf preparation procyanidin, the method can be removed the interference of most impurity, fast ginkgo leaf procyanidin is carried out to separation by the size of the degree of polymerization, and according to the difference of separate sources procyanidin collection of illustrative plates, for differentiate ginkgo agent have do not have adulterated.
The inventor finds during procyanidin research in to gingko leaf preparation, although all contain procyanidin in various plants, because plant origin is different, procyanidin content is wherein different, and kind is also different, also shows different effects.Although at present more to the correlative study of procyanidin, the procyanidin that all concentrates on single source detects, the procyanidin of separate sources is not effectively compared, particularly the procyanidin for two or more separate sources detects not research.Procyanidin is detected and mainly concentrates on content, therefore as there being the procyanidin product of low price as adulterated in grape pip procyanidin in ginkgo leaf procyanidin on market, do not have at present method to detect.And because heterogeneity effect is different, this adulterated behavior is very harmful to product.Therefore a kind of simple, be quick on the draw, significant to underwriter people's drug safety to the adulterated detection method of procyanidin fast.
The inventor is in the middle discovery that studies for a long period of time, procyanidin in ginkgo leaf is different with the procyanidin of other plant origin, as each degree of polymerization of grape pip procyanidin at a low price in the market all only goes out a peak, and ginkgo procyanidin is from dimer, all has 2～3 characteristic peaks.As being effectively used, can become and whether differentiate in ginkgo leaf the key point of adulterated other procyanidin.
For achieving the above object, the invention provides following a kind of solution, mainly comprise following content:
1. gingko leaf preparation sample pre-treatments
Because impurity component in gingko leaf preparation can affect the mensuration of procyanidin, so need to carry out pre-treatment to gingko leaf preparation.
Pre-treatment mainly contains three steps: I, gingko leaf preparation is made to aqueous solution and be splined on 30-60 object polyamide; II, remove 20% acetone soln wash-out position; III, collect 80% acetone soln wash-out position and dry after with appropriate methyl alcohol, it is dissolved completely.
Different according to gingko leaf preparation source, the above-mentioned pre-treating method of solid pharmaceutical preparation and liquid preparation is described below:
(1) solid pharmaceutical preparation: after gingko leaf preparation is pulverized, by the ultrasonic assist in dissolving of 20% acetone soln, filter, remove insoluble auxiliary material; Filtrate is splined on to 30～60 object polyamides, after completion of the sample, with 20% acetone soln wash-out of 3～4 times of volumes, discards the eluent at this position; Use again 80% acetone soln wash-out of 3～4 times of volumes, obtain the eluent at 80% acetone position; 80% acetone position eluent is recycled to without acetone taste, uses equal-volume n-butyl acetate extraction 2 times, discard organic phase, reclaim water to dry; Residue dissolves it with appropriate methyl alcohol completely, obtains methyl alcohol lysate.
(2) liquid preparation: gingko leaf preparation is directly splined on to 30～60 object polyamides, with 20 % acetone soln wash-outs of 3～4 times of volumes, discards the eluent at this position after completion of the sample; Use again 80% acetone soln wash-out of 3～4 times of volumes, the eluent at 80% acetone position; 80% acetone position eluent is recycled to without acetone taste, uses equal-volume n-butyl acetate extraction 2 times, discard organic phase, reclaim water to dry; Residue dissolves it with appropriate methyl alcohol completely, obtains methyl alcohol lysate.
2. positive-high performance liquid chromatography removes (NP-HPLC) separated above-mentioned methyl alcohol lysate, and detects with HPLC, and wherein NP-HPLC chromatographic condition is as follows:
(1) fixing is phenomenex dibasic alcohol post (250 * 4.6 mm, 5 μ m) mutually;
(2) mobile phase is (A) acetonitrile, (B) methanol/water/acetic acid (95/3/2, V/V/V); Eluent gradient is 0～10 min:0～12%B; 10～10.01 min:12～15%B; 10.01～30 min:15～45%B; 30～35 min:45%B; 35～40 min:45～0%B;
(3) flow velocity is 1.0 ml/min;
(4) detect wavelength: fluorescence exciting wavelength 276 nm; Emission wavelength 316 nm;
(5) sample size is 20 μ L.
3. chromatogram contrast
By the chromatogram of said method gained, contrast with pure ginkgo biloba p.e chromatogram, if any adulterated situation, chromatogram has obviously different from pure ginkgo biloba p.e chromatogram.
Whether by said method, can be used for detecting procyanidin in gingko leaf preparation has adulterated, and react very sensitive, the procyanidin of minute quantity is adulterated is that available the inventive method detects, can detect other source procyanidin of mixing in ginkgo biloba p.e more than 0.5%, namely the adulterated in addition detection and identification of the inventive method that just can pass through of more than 0.5% procyanidin.
Whether the present invention not only can be used in ginkgo leaf extract preparation procyanidin has adulteratedly, also can be used for food, health products, pharmaceuticals and/or the cosmetics of composition containing ginkgo leaf extract, as Folium Ginkgo, YINXINGYE ZHUSHEYE, capsule of ginkgo leaves health products etc.; The source of the adulterated procyanidin relating to comprise grape pip pine tree sheet, apple, hawthorn, peanut, manaca, wild strawberry, cowberry, european cranberry, lotus pod etc.
By the method in the present invention, detect the procyanidin in gingko leaf preparation, be subject to external interference few.In the present invention, analysis is used the pre-treating method of sample, the interference that can remove most impurity.Adopt method of the present invention to detect pure ginkgo biloba p.e, Folium Ginkgo, capsule of ginkgo leaves, ginkgo leaf injection, found that figure spectral shape is consistent, all two obvious characteristic peaks, tripolymer and the tetramer characteristic peak of visible procyanidin dimers in all collection of illustrative plates.And other detection side's rule is because there being a large amount of impurity, can not effectively distinguish Partial Feature peak wherein.Illustrate that method specificity of the present invention is high, other composition in preparation does not affect the mensuration of the inventive method.
First the inventor detects fine silver apricot phyllogen anthocyanidin, and concrete outcome is shown in embodiment 1.
In the present invention, high-efficient liquid phase chromatogram process measuring method is referring to 1 appendix VI D high performance liquid chromatography of < < Chinese Pharmacopoeia > > version in 2010, and concrete instrument condition etc. are referring to concrete testing process and embodiment.
The present invention is applicable to analysis and the discriminating of procyanidin in the gingko leaf preparation of various formulations, and pre-treating method is simple, operation steps is few; Analytical approach fast, accurately; The method of discerning the false from the genuine is easy, judge index clear and definite.Therefore, express-analysis and the discriminating of method of the present invention to procyanidin in food, health products, pharmaceuticals and/or the cosmetics of the preparation of the various formulations of ginkgo leaf, composition containing ginkgo leaf extract, is suitable method.
Use for reference and improve above-mentioned analytical approach, it is suitable for and is applied to the analysis of procyanidin in gingko leaf preparation, significant for further developing of the raising of gingko leaf preparation standard and industrialization.
accompanying drawing explanation:
Fig. 1 is embodiment 1: the NP-HPLC chromatogram of ginkgo leaf procyanidin (A) and grape pip procyanidin (B)
Fig. 2 is embodiment 2: the NP-HPLC chromatogram of procyanidin in tablets of Ginkgo biloba L: (A) sample 1: without the sample of any pre-treatment; (B) sample 2: through polyamide purifying, without the sample of n-butyl acetate extraction; (C) sample 3: through the sample of the complete pre-treatment of the inventive method
Fig. 3 is embodiment 3: the NP-HPLC chromatogram of procyanidin in capsule of ginkgo leaves agent
Fig. 4 is embodiment 4: the NP-HPLC chromatogram of procyanidin in ginkgo leaf injection
Fig. 5 is embodiment 5: the NP-HPLC chromatogram of procyanidin in adulterated gingko leaf preparation: (A) mix 0.5% grape pip procyanidin; (B) mix 1.0% grape pip procyanidin; (C) mix 2.0% grape pip procyanidin; (D) mix 4.0% grape pip procyanidin; (E) not adulterated.
embodiment:
The present invention further illustrates as follows in conjunction with specific embodiments:
Embodiment 1 ginkgo leaf procyanidin detect and with the contrast of grape pip procyanidin
Get homemade ginkgo procyanidin extract (procyanidin content is 95%) and grape pip procyanidin extract (procyanidin content is 96%), be dissolved in respectively methyl alcohol, after filtration, carry out HPLC detection:
Equipment: Aglient 1200 type high performance liquid chromatographs; Diamonsil C18 chromatographic column 5 μ m 4.6 * 150mm
Chromatographic condition:
(1) fixing is phenomenex dibasic alcohol post (250 * 4.6 mm, 5 μ m) mutually;
(2) mobile phase is (A) acetonitrile, (B) methanol/water/acetic acid (95/3/2, V/V/V); Eluent gradient is 0～10 min:0～12 %B; 10～10.01 min:12～15 %B; 10.01～30 min:15～45 %B; 30～35 min:45 %B; 35～40 min:45～0 %B;
(3) flow velocity is 1.0 ml/min;
(4) detect wavelength: fluorescence exciting wavelength 276 nm; Emission wavelength 316 nm;
(5) sample size is 20 μ L.
The results are shown in Figure 1, from HPLC chromatogram, can find, each degree of polymerization of grape pip procyanidin all only goes out a peak, and ginkgo procyanidin is from dimer, all have 2～3 characteristic peaks, its reason is that the procyanidin that forms ginkgo forms different from the procyanidin composition of grape pip.
The analysis of procyanidin in embodiment 2 tablets of Ginkgo biloba Ls
Sample source: Folium Ginkgo (Kang Enbei Zhejiang Pharmaceutical Co of producer, lot number 20100709)
Sample 1: get 2, tablet, be ground to fine powder, dissolve with methyl alcohol, filter, obtain.
Sample 2: get 2, tablet, be ground to fine powder, by 16ml 20% acetone soln, ultrasonic assist in dissolving, filter, remove insoluble auxiliary material; Filtrate is splined on to 30～60 object polyamides, after completion of the sample, with 20% acetone soln wash-out of 3～4 times of volumes, discards this position; The 80% acetone soln wash-out of using again 3～4 times of volumes, obtains 80% acetone position; 80% acetone position is recycled to dry; Residue dissolves with methyl alcohol, obtains methyl alcohol lysate.
Sample 3: get 2, tablet, be ground to fine powder, by 16ml 20% acetone soln, ultrasonic assist in dissolving, filter, remove insoluble auxiliary material; Filtrate is splined on to 30～60 object polyamides, after completion of the sample, with 20% acetone soln wash-out of 3～4 times of volumes, discards this position; The 80% acetone soln wash-out of using again 3～4 times of volumes, obtains 80% acetone position; 80% acetone position is recycled to without acetone taste, uses equal-volume n-butyl acetate extraction 2 times, discard organic phase, reclaim water to dry; Residue dissolves with methyl alcohol, obtains methyl alcohol lysate.
Above-mentioned 3 samples, carry out respectively the separation of procyanidin with the chromatographic condition in embodiment 1, the results are shown in Figure 2.
From HPLC chromatogram, can find, through in the tablets of Ginkgo biloba L (sample 3) of pre-treatment, procyanidin dimers has two obvious characteristic peaks in 14min left and right and 15min left and right, and tripolymer and tetrameric characteristic peak are also out distinguishable simultaneously; Without the sample 1 of any pre-treatment, owing to there being a large amount of impurity, therefore almost there is not the characteristic peak of procyanidin; Through polyamide purifying, without the sample 2 of organic solvent extraction, after having removed a large amount of impurity, can tell two characteristic peaks of procyanidin dimers, but owing to still there is more impurity, therefore, tripolymer is more difficult to be distinguished.
The analysis of procyanidin in embodiment 3 capsule of ginkgo leaves agent
Sample source: Tianbaoning capsule (health products, Hangzhou Kang'Enbei Pharmaceutical Co., Ltd produces, lot number 20110516)
Get 2 of capsules, open capsule, pour out content, be ground to fine powder, by 16ml 20% acetone soln, ultrasonic assist in dissolving, filter, remove insoluble auxiliary material.Filtrate is splined on to 30～60 object polyamides, after completion of the sample, with 20% acetone soln wash-out of 3～4 times of volumes, discards this position; The 80% acetone soln wash-out of using again 3～4 times of volumes, obtains 80% acetone position; 80% acetone position is recycled to without acetone taste, uses equal-volume n-butyl acetate extraction 2 times, discard organic phase, reclaim water to dry; Residue dissolves with methyl alcohol, obtains methyl alcohol lysate.
With the chromatographic condition in embodiment 1, carry out the separation of procyanidin, the results are shown in Figure 3.
Dimeric two the obvious characteristic peaks of procyanidin from HPLC chromatogram can clearly be differentiated, and tripolymer and tetrameric characteristic peak.
The analysis of procyanidin in embodiment 4 ginkgo leaf injections
Sample source: ginkgo leaf injection (Dr Willmar Schwabe produces, lot number 20110423)
Get one of ginkgo leaf injection, be directly splined on 30～60 object polyamides, after completion of the sample, with 20% acetone soln wash-out of 3～4 times of volumes, discard this position; The 80% acetone soln wash-out of using again 3～4 times of volumes, obtains 80% acetone position; 80% acetone position is recycled to without acetone taste, uses equal-volume n-butyl acetate extraction 2 times, discard organic phase, reclaim water to dry; Residue dissolves with methyl alcohol, obtains methyl alcohol lysate.
With the chromatographic condition in embodiment 1, carry out the separation of procyanidin, the results are shown in Figure 4.
Dimeric two the obvious characteristic peaks of procyanidin in HPLC chromatogram can clearly be differentiated equally, and tripolymer and tetrameric characteristic peak.
The analysis of procyanidin in the adulterated gingko leaf preparation of embodiment 5
In ginkgo biloba p.e, simulate adulterated grape seed extract, and carried out coherent detection.Take 4 parts of ginkgo biloba extracts of self-control, be respectively 1.99g, 1.98g, 1.96g, 1.92g; Add successively grape seed extract 0.01g, 0.02g, 0.04g, 0.08g, adulterated amount is respectively 0.5%, 1.0%, 2.0%, 4.0%.Above-mentioned four parts of adulterated preparations are used respectively to 200ml 20% acetone soln, ultrasonic assist in dissolving, filter, remove insoluble auxiliary material; Filtrate is splined on to 30～60 object polyamides, after completion of the sample, with 20% acetone soln wash-out of 3～4 times of volumes, discards this position; The 80% acetone soln wash-out of using again 3～4 times of volumes, obtains 80% acetone position; 80% acetone position is recycled to without acetone taste, uses equal-volume n-butyl acetate extraction 2 times, discard organic phase, reclaim water to dry; Residue dissolves with methyl alcohol, obtains methyl alcohol lysate.
With the chromatographic condition in embodiment 1, carry out the separation of procyanidin, the results are shown in Figure 5.
By HPLC chromatogram, can be obtained, there is obvious change in the ginkgo biloba extract HPLC characteristic peak that mixes grape pip procyanidin: 1. the feature at two peaks of dimer changes: the dimer peak that the peak of 14min left and right is Procyanidin, the peak of 15min left and right is the distinctive dimer of Prodelphinidin peak, therefore add after grape pip procyanidin, leading peak compared with postpeak go out peak intensity more obviously, peak height is higher, peak area is larger; 2. the Procyanidin tripolymer peak of about 17min, in not adulterated preparation, going out peak is not clearly, but adds after grape pip procyanidin, this peak goes out peak intensity obviously to be increased; 3. the trend of above-mentioned two kinds of changes is directly proportional to grape pip procyanidin addition.
Utilize variation and the trend of characteristic peak, can discern the false from the genuine, can very easily identify in gingko leaf preparation, whether have adulterated.
The source of above-mentioned adulterated procyanidin also can comprise pine tree sheet, apple, hawthorn, peanut, manaca, wild strawberry, cowberry, european cranberry, lotus pod etc.Adulterated rear all obvious changes of visible last gained chromatogram.
Claims (5)
1. a method of differentiating procyanidin in gingko leaf preparation, whether differentiate in gingko leaf preparation and to comprise the following steps adulterated procyanidin: 1) pre-treatment of gingko leaf preparation: I, gingko leaf preparation is made to aqueous solution and is splined on 30-60 object polyamide; II, remove 20% acetone soln wash-out position; III, collect 80% acetone soln wash-out position and be recycled to without acetone taste, with equal-volume n-butyl acetate extraction 2 times, reclaim water to dry; Residue dissolves it with methyl alcohol completely, obtains methyl alcohol lysate; 2) the separated above-mentioned methyl alcohol lysate of positive-high performance liquid chromatography, wherein positive-high-efficient liquid phase chromatogram condition is as follows: fixing is phenomenex dibasic alcohol post mutually, 250 * 4.6 mm, 5 μ m; Mobile phase is acetonitrile-methanol/water/acetic acid, and wherein acetonitrile is A, and methanol/water/acetic acid is B, A+B=100%, and the volume ratio V/V/V of methanol/water/acetic acid is 95/3/2; Eluent gradient is 0～10 min:0～12 %B; 10～10.01 min:12～15%B; 10.01～30 min:15～45 %B; 30～35 min:45 %B; 35～40 min:45～0 %B; Flow velocity is 1.0 ml/min; Detect wavelength: fluorescence exciting wavelength 276 nm; Emission wavelength 316 nm; Sample size is 20 μ L; 3) chromatogram contrast: by the chromatogram of said method gained, contrast with pure ginkgo biloba p.e chromatogram, if any adulterated situation, chromatogram has obviously different from pure ginkgo biloba p.e chromatogram.
2. method according to claim 1, is characterized in that described gingko leaf preparation is solid pharmaceutical preparation, after ginkgo leaf solid pharmaceutical preparation is pulverized, by the ultrasonic assist in dissolving of 20% acetone soln, filters, and removes insoluble auxiliary material; Filtrate is splined on to 30～60 object polyamides, after completion of the sample, with 20 % acetone soln wash-outs of 3～4 times of volumes, discards this position; The 80% acetone soln wash-out of using again 3～4 times of volumes, obtains 80% acetone position; 80% acetone position is recycled to without acetone taste, uses equal-volume n-butyl acetate extraction 2 times, discard organic phase, reclaim water to dry; Residue dissolves with methyl alcohol, obtains gingko leaf preparation methyl alcohol lysate.
3. method according to claim 1, it is characterized in that described gingko leaf preparation is liquid preparation, gingko leaf preparation is directly splined on to 30～60 object polyamides, after completion of the sample, with 20% acetone soln wash-out of 3～4 times of volumes, discards the eluent at this position; Use again 80% acetone soln wash-out of 3～4 times of volumes, the eluent at 80% acetone position; 80% acetone position eluent is recycled to without acetone taste, uses equal-volume n-butyl acetate extraction 2 times, discard organic phase, reclaim water to dry; Residue dissolves it with appropriate methyl alcohol completely, obtains methyl alcohol lysate.
4. according to the method described in claim 1 or 2 or 3, it can be used for the detection of adulterated procyanidin in food, health products, pharmaceuticals and the cosmetics of composition containing ginkgo leaf extract.
5. according to the method described in claim 1 or 2 or 3, the source that it is characterized in that adulterated procyanidin comprise grape pip pine tree sheet, apple, hawthorn, peanut, manaca, wild strawberry, cowberry, european cranberry, lotus pod.
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| CN103954700A (en) * | 2014-04-12 | 2014-07-30 | 陕西衡道检测技术有限公司 | Method used for procyanidin content detection and identification |
| CN105424947B (en) * | 2015-12-28 | 2016-08-24 | 青岛古高生物科技有限公司 | The application of procyanidin and the thrombin time test reagent containing procyanidin |
| CN108287202A (en) * | 2017-12-07 | 2018-07-17 | 佛山科学技术学院 | A method of detection honey vinegar black soya bean procyanidins |
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