CN1763514A - Method for rapid qualitative and quantitative analysis of active components in gingkgo product - Google Patents
Method for rapid qualitative and quantitative analysis of active components in gingkgo product Download PDFInfo
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- CN1763514A CN1763514A CN 200410086046 CN200410086046A CN1763514A CN 1763514 A CN1763514 A CN 1763514A CN 200410086046 CN200410086046 CN 200410086046 CN 200410086046 A CN200410086046 A CN 200410086046A CN 1763514 A CN1763514 A CN 1763514A
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Abstract
The invention provides a rapid qualitative and quantitative analysis method of active ingredient in the ginkgo product, which is characterized by the following: hydrolyzing the ginkgo extractant and product through simple disposal; adapting nuclear magnetic resonance spectrometer to do qualitative and quantitative analysis of Ginkgo terpene trilactones and flavonols through different deuteride solvent systems.
Description
Technical field
The present invention relates to a kind of with NMR (Nuclear Magnetic Resonance) spectrum (
1H NMR) carries out the quantitative ginkgolides of method, particularly while of the active component in the ginkgo of the qualitative and quantitative analysis rapidly and accurately goods and the analytical approach of flavonols compound.
Background technology
Ginkgo (Ginkgo biloba L.) is the Chinese medicine that a tradition is used, studies show that of past, contained ginkgolides (Ginkgo terpene trilactones) and the flavonols (flavonols) of ginkgo leaf is main active (consulting list of references 1~3).More general identification is that contained ginkgolides total amount should be more than 5.4~6.6% in the ginkgo leaf extract produced of bulk drug supplier, and the flavonols total amount should be more than 21.6~26.4%.
Analytical approach at ginkgolides mainly cooperates UV-detector (UV) or RI-detector (RI) as main analytical tools (consulting list of references 4~6) with high performance liquid chromatograph (HPLC), but analytic sample must be earlier through pre-treatment, remove possible interfering material, particularly the flavonols compound.Also having in addition with gas chromatograph (GC) cooperates flame ionization detector (FID) or mass spectrometer (MS) as analysis tool (consulting list of references 7~11), equally must be earlier through sample pre-treatments, remove possible interfering material, and the higher structure of the compound-modified one-tenth volatility of ginkgolides that desire is analyzed, to carry out gas chromatography.Also the someone proposes to utilize the analytical approach of nuclear magnetic resonance spectrometer in addition.
Analysis at flavonols is main analytical tools (consulting list of references 12) with high performance liquid chromatography cooperation UV-detector mainly then.
The method of analyzing simultaneously ginkgolides and flavonols two compounds is not effectively arranged at present as yet.
Summary of the invention
Because ginkgolides and flavonols compound are the main active (consulting list of references 3) of commercially available ginkgo leaf extract, and this two classes reactive compound ginkgolides especially, its content in ginkgo leaf can be along with tender, old, verdant, the withered and yellow situation of the place of production, kind, the age of tree and the ginkgo leaf of ginkgo, and the factors such as season of gathering have very big variation, and the paced work of contained ginkgolides and Flavonol compound is very important in the biloba extract thing that manufactures.
Because ginkgolides chemical constitution (shown in Figure 6) does not have tangible chromophore (Cllromophore), its content in ginkgo leaf is extremely low, and separation and purification is difficult for, had the strong existing interference of UV Absorption material by contained other in the ginkgo leaf easily, analyze very difficulty of this compounds in the past, must remove possible interference earlier, the flavonols compound that particularly has strong UV Absorption, and this flavonols compound also is the another kind of reactive compound that needs quantitative test.Therefore method in the past is to sacrifice flavone compound, a quantitative test ginkgolides.The method of sample pre-treatments is normally removed most of possible interfering material through tubing string chromatography or solid phase adsorption or supercritical extraction earlier, carries out the high performance liquid chromatography quantitative test again, and cooperates and change detecting device to improve sensitivity.If then must be when analyzing through structural modification to improve volatility (consulting list of references 7~11) with gas chromatograph.These methods have all that sensitivity is low, baseline (Baseline) is unstable, need not good or the like the shortcoming of preposition purifying of sample or derivatization step and the recovery.For improving these shortcomings, also be suggested (consulting list of references 13,14) with nuclear magnetic resonance spectrometer as the analytical approach of analysis tool, but equally also can't be simultaneously quantitative flavonols compound.
As for the flavonols compound,, therefore can cooperate the UV-detector quantitative test by high performance liquid chromatography easily because it has good chromophore (as shown in Figure 6).But equally also do not have tangible chromophore, so can't simultaneously quantitative ginkgolides compound owing on the ginkgolides chemical constitution.
So far occur effectively as yet, fast and accurately analytical approach can be simultaneously quantitative contained ginkgolides and flavonols compound in the biloba extract thing.
Because the special benefits of nuclear magnetic resonance spectrometry, comprise fast, easily, repeatability is good, do not need derivatization and can not need high-purity to analyze subject matter as standard items, therefore the present invention also utilizes nuclear magnetic resonance spectrometer as analysis tool, through simple hydrolysing step, as test solvent, qualitative and quantitative is analyzed ginkgolides and flavonols compound simultaneously with different deuterate solvent combinations.
The chemical constitution of the ginkgolides compound of institute's desire analysis has common feature proton H-12, because the contiguous substituting group of H-12 is configured with different slightly, cause that different chemical shifts is arranged in NMR (Nuclear Magnetic Resonance) spectrum, therefore can distinguish different ginkgolides by the chemical potential in-migration of H-12 in NMR (Nuclear Magnetic Resonance) spectrum, and because the singularity of structure, the chemical shift of H-12 is distributed between 5.8~6.4ppm, the zone that this section generally cannot not be crowded in NMR (Nuclear Magnetic Resonance) spectrum, the proton signal that therefore is subjected to other compound disturbs less.And Flavonol compound has distinctive proton H-2 ' equally, and same owing to contiguous substituent difference, the H-2' proton of different flavonols also can present different chemical shifts, can distinguish different Flavonol compounds by this.But the Flavonol compound kind that is contained in the ginkgo leaf extract is very many, H-2 ' the proton of all flavonols compounds to be made a distinction very difficulty, and signal also can interfere with each other, one by one quantitative these compounds also too big meaning not in practical application.The chemical constitution that anatomizes these flavone compounds is found, these compounds mostly are to be skeleton with kaempferol (kaempferol), Quercetin (quercetin) and Isorhamnetin (isorhamnetin), have different candy bases to replace on the C-3 position and form.Therefore if these candy substituting groups are handled with hydrolysis method, then should obtain corresponding kaempferol, Quercetin and Isorhamnetin.So originally, very complicated and diversified flavonols compound can be reduced to 3 kinds of main flavonols by hydrolysis.Therefore the zone of H-2 ' the feature signal between 7.8~8.8ppm can present comparatively clean part because the proton of rare other compound disturbs, and can be used to as the characteristic area of distinguishing 3 kinds of different flavonols.So can make through simple hydrolysing step utilizes simultaneously quantitative ginkgolides of nuclear magnetic resonance spectrometer and flavonols two compounds to become possibility.
Owing to still contain other very many compositions in the hydrolysate of biloba extract thing, these compositions may interfere with the target signal that desire is analyzed, and the target signal that institute's desire is analyzed each other also may be interfering with each other, therefore must think in the selection of test solvent.For compositions all in the hydrolysate is all dissolved, in order to avoid the inaccuracy on causing quantitatively, be necessary as the selection of deuterate methyl alcohol, deuterate dioxy sulfoxide, the contour polar solvent of deuterate pyridine.Be separated from each other for target signal in addition or separate with other chaff interference proton signal with institute's desire analysis, must be by the solvent effect that is showed as aromatic solvents (aromatic solvents) such as deuterate benzene, deuterate toluene or deuterate pyridines, the difference that influences to the compound of structure similar, select in varing proportions and high polarity deuterate solvent, use the preferable test solvent condition (referring to Fig. 2 and Fig. 3) that obtains.
In addition, for qualitative and quantitative is analyzed ginkgolides and flavonols compound, must select suitable internal standard product.These internal standard product must have high-purity and stable, have the conditions such as composition interference in characteristic absorption signal and the not analyzed sample.The various different standard items of measuring the compound of desires analysis are added quantitative internal standard product, carry out NMR (Nuclear Magnetic Resonance) spectrum scanning with the appropriate solvent condition of selecting, integration ratio with target signal and internal standard product feature signal is mapped to concentration, tries to achieve the inspection amount line (see figure 4) of respectively desiring analyte.
Be to reduce the interference signal of other compound in the nmr spectrum chart, analyze the different solubility of composition different solvents by desire, again with different solvent extractions to remove more interfering material, the interference of NMR (Nuclear Magnetic Resonance) spectrum is reduced.The biloba extract thing is after hydrolysis, and with different solvents extraction, the active component of gained partly adds quantitative internal standard product,, carries out NMR (Nuclear Magnetic Resonance) spectrum and scans, and try to achieve the content of each active component with inspection amount line as test solvent with the deuterate solvent system selected.
The method (as Fig. 1) of carrying out of reality of the present invention is that commercially available biloba extract thing or ginkgo product are hydrolyzed with different temperature, normally utilize the strong acid hydrolysis, the hydrolysate of gained utilizes active component such as ginkgolides and flavonols compound to the different solubility of organic solvent, distributes separation.Elder generation distributes extraction to remove other composition of low polarity with low polar organic solvent and water, distributes extraction with medium polar solvent and water again, obtains containing the extract layer part of active component.The active component of gained partly adds quantitative suitable internal standard product, as 1,3,5-trimethoxy-benzene (as shown in Figure 6) etc., and with the deuterate solvent system selected as test solvent, carry out NMR (Nuclear Magnetic Resonance) spectrum scanning, and try to achieve the content of each active component with inspection amount line.
The object of the present invention is to provide the method for active ingredient contained in a kind of fast qualitative and the quantitative test ginkgo goods, to reach simultaneously the quantitatively purpose of the analysis of ginkgolides and flavonols compound.
The invention provides the method for active ingredient contained in a kind of fast qualitative and the quantitative test ginkgo goods, mainly is that it comprises at the qualitative and quantitative analytical approach of institute's bilobalide-containing in the ginkgo and flavonols compound:
(a) measure the target signal of ginkgo goods active component as nuclear magnetic resonance spectrometry with the H-2 ' of the H-12 of ginkgolides and flavonols;
(b) have the deuterate solvent of obvious solvent effect and deuterate solvent system that various high polar solvent mixes are measured the ginkgo goods as nuclear magnetic resonance spectrometry dissolving and test solvent with aromatic solvent;
(c) with the internal standard product of benzene substituted compound as nuclear magnetic resonance spectrometry measurement ginkgo goods;
(d) after the strong acid hydrolysis with the combination of various concentration and temperature, with nuclear magnetic resonance spectrometry qualitative and quantitative analysis simultaneously to measure the ginkgolides and the flavonols compound of ginkgo goods.
Method provided by the present invention by utilize NMR (Nuclear Magnetic Resonance) spectrum (
1H NMR), the active component in the ginkgo of the qualitative and quantitative analysis rapidly and accurately goods.
The method of contained active ingredient in above-mentioned fast qualitative and the quantitative test ginkgo goods, wherein, this aromatic solvent is deuterate benzene, deuterate toluene and deuterate pyridine; This high polar solvent is deuterate methyl alcohol, deuterate acetone, deuterate dioxy sulfoxide and deuterate pyridine; This benzene substituted compound is 1,3, the 5-trimethoxy-benzene.
This method greatest benefit is that simultaneously quantitatively contained active component comprises ginkgolides (Bilobalide (bilobalide) in the biloba extract thing, ginkalide A (ginkgolide A), ginkolide B (ginkgolide B), ginkalide C (ginkgolide C), bilobalide J (ginkgolideJ)) and flavonols (kaempferol (kaempferol), Quercetin (quencetin), Isorhamnetin (isorhamnetin)) compound, and only need just can reach through simple hydrolysing step, do not need to sacrifice the flavonols compound and analyze ginkgolides, or can't detect ginkgolides in order to analyze the flavonols compound.And need not analyse or the like the prepurification method through column chromatography or Solid-Phase Extraction or shooting flow, and can reduce the loss that in preposition purge process desire is analyzed composition, avoid the shortcoming that repeatability is not good and the recovery is low.Do not need to cause productive rate fixedly not cause the inaccurate of analysis result through derivative reaction yet.And the advantage of nuclear magnetic resonance spectrometry itself comprises fast, repeatability is good, and if apparatus status is good, standard items and the inspection amount line of desiring analyte can not need.
Description of drawings
Figure l is the quick-reading flow sheets synoptic diagram of the inventive method;
Fig. 2 is a nmr spectrum chart of measuring the biloba extract thing after the acid hydrolysis with the combination of different deuterate solvents as test solvent, wherein: (A) deuterate pyridine, (B) deuterate dioxy sulfoxide-deuterate toluene, (C) deuterate dioxy sulfoxide-deuterate benzene, (D) deuterate methyl alcohol-deuterate toluene, (E) deuterate methyl alcohol-deuterate benzene, (F) deuterate methyl alcohol;
Fig. 3 be in varing proportions deuterate methyl alcohol and the nmr spectrum chart of the biloba extract thing of deuterate benzene after as the acid hydrolysis of test solvent, wherein: (A) deuterate methyl alcohol-deuterate benzene (25: 75), (B) deuterate methyl alcohol-deuterate benzene (50: 50), (C) deuterate methyl alcohol-deuterate benzene (65: 35), (D) deuterate methyl alcohol-deuterate benzene (75: 25), (E) deuterate methyl alcohol;
Fig. 4 analyzes composition for each desire standard items are at deuterate methyl alcohol and 65: 35 ratio of the deuterate benzene nmr spectrum chart as the test solvent gained, wherein: (A) Bilobalide, (B) ginkalide A, (C) ginkolide B, (D) ginkalide C, (E) bilobalide J, (F) kaempferol, (G) Quercetin, (H) Isorhamnetin, IS: internal standard product (1,3, the 5-trimethoxy-benzene);
Fig. 5 is various commercially available biloba extract things through hydrolysis and the part of distributing the extraction gained with deuterate methyl alcohol and 65: 35 ratio of the deuterate benzene nmr spectrum chart as the test solvent gained, and wherein: (A) sample one, and (B) sample two, (C) sample three, (D) sample four, and (E) sample five, and (F) sample six, (G) sample seven, (H) sample eight, and (I) sample nine, IS: internal standard product (1,3, the 5-trimethoxy-benzene);
Fig. 6 is ginkgolides, flavonols compound and 1,3, the chemical constitution of 5-trimethoxy-benzene.Peak number explanation among the figure:
1 Bilobalide (bilobalide)
2 ginkalide As (ginkgolide A)
3 ginkolide Bs (ginkgolide B)
4 ginkalide Cs (ginkgolide C)
5 bilobalide Js (ginkgolide J)
6 kaempferols (kaempferol)
7 Quercetins (quencetin)
8 Isorhamnetins (isorhamnetin)
IS internal standard product, 1,3, the 5-trimethoxy-benzene
BB Bilobalide (bilobalide)
GA ginkalide A (ginkgolide A)
GB ginkolide B (ginkgolide B)
GC ginkalide C (ginkgolide C)
GJ bilobalide J (ginkgolide J)
K kaempferol (kaempferol)
Q Quercetin (quencetin)
I Isorhamnetin (isorhamnetin)
Embodiment
The present invention illustrates as example with the quantitative test of commercially available biloba extract thing.
1, make inspection amount line: the analyte standard items of respectively desiring with variable concentrations add a certain amount of internal standard product (1,3, the 5-trimethoxy-benzene), add 390 μ L deuterate methyl alcohol and 210 μ L deuterate benzene carry out nuclear magnetic resonance spectroscopy (Fig. 4) as test solvent.The feature proton of careful each reference material of integration absorbs the characteristic absorption signal of signal and internal standard product.With the integrated value comparison concentration mapping of the target signal of the target signal of each reference material and internal standard product, respectively desired the inspection amount line of analyte.
Table 1: the inspection amount line (Calibration curve) of Bilobalide (bilobalide), ginkalide A (ginkgolide A), ginkolide B (ginkgolide B), ginkalide C (ginkgolide C), bilobalide J (ginkgolideJ), kaempferol (kaempferol), Quercetin (quencetin), Isorhamnetin (isorhamnetin).
Composition (Compound) | Inspection amount line (Calibration curve) | Linear (R square value) (Linearity (R-squared)) |
Bilobalide (Bilobalide) | Y=1.8500X+0.2313 | 0.9992 |
Ginkalide A (GinkgolideA) | Y=1.3882X+0.1352 | 0.9998 |
Ginkolide B (Ginkgolide B) | Y=1.9500X-0.1246 | 0.9993 |
Ginkalide C (Ginkgolide C) | Y=1.6516X+0.0875 | 0.9998 |
Bilobalide J (Ginkgolide J) | Y=1.1469X+0.1999 | 0.9991 |
Kaempferol (Keampferol) | Y=1.2853X+0.1280 | 0.9996 |
Quercetin (Quercetin) | Y=0.8612X-0.0059 | 0.9995 |
Isorhamnetin (Isorhamnetin) | Y=0.9384X-0.0327 | 0.9993 |
2, accurately take by weighing the commercially available biloba extract thing A of 50mg, with 30mL 5% HCl aqueous solution reflux 30 minutes, 120 ℃ of temperature.
3, reaction is got back to room temperature and is added the 30mL thiacyclohexane and distribute extraction, keeps water layer.Repeat 3 times.
4, add 30mL MEK and water and distribute extraction, collect the MEK layer.Repeat 3 times.
5, collected MEK layer is evaporated to dried, adds 390 μ L deuterate methyl alcohol and 210 μ L deuterate benzene, and a certain amount of internal standard product, carry out nuclear magnetic resonance spectroscopy (Fig. 5).The feature proton of careful each reference material of integration absorbs the characteristic absorption signal of signal and internal standard product, tries to achieve the integrated value of the target signal of the target signal of each reference material and internal standard product.Just can obtain the content that each desire is analyzed composition by inspection amount line.
Table 2: the Bilobalide of measuring by nuclear magnetic resonance spectrometry (Bilobalide (BB)), ginkalide A (ginkgolide A (gA)), ginkolide B (ginkgolide B (gB)), ginkalide C (ginkgolide C (gC)), bilobalide J (ginkgolide J (gJ)), kaempferol (kaempferol (K)), Quercetin (quercetin (Q)) and Isorhamnetin (isorhamnetin (the I)) content (measure and average for 3 times) in the commercially available biloba extract thing of various differences
Sample (Sample) | BB | gA | gB | gC | gJ | K | Q | I |
Sample 1 (Sample 1) sample 2 (Sample 2) sample 3 (Sample 3) sample 4 (Sample 4) sample 5 (Sample 5) sample 6 (Sample 6) sample 7 (Sample 7) sample 8 (Sample 8) sample 9 (Sample 9) | 1.42 2.51 1.53 1.55 1.66 1.04 1.31 1.08 1.68 | 2.85 1.80 0.89 0.67 1.35 1.26 3.12 3.01 1.44 | 1.11 0.67 0.40 0.21 0.47 0.58 1.33 1.28 0.38 | 0.57 0.66 0.51 0.61 0.71 0.72 1.09 1.47 0.73 | 0.28 0.42 0.34 0.30 0.44 0.34 0.58 0.65 0.38 | 2.94 3.05 1.70 1.89 1.71 1.56 2.19 3.19 1.84 | 3.20 2.94 1.67 2.38 1.89 2.68 1.90 2.18 2.09 | 0.72 0.76 0.48 0.57 0.48 0.58 0.45 0.58 0.47 |
6, recovery test: accurately take by weighing each standard items of 3mg, with 30mL 5%HCl aqueous solution reflux 30 minutes, 120 ℃ of temperature.Try to achieve the content that each desire is analyzed composition according to step 3.4.5., and calculate the recovery.
Table 3: Bilobalide (Bilobalide) (BB), ginkalide A (ginkgolide A) (gA), ginkolide B (ginkgolide B) (gB), ginkalide C (ginkgolide C) (gC), bilobalide J (ginkgolide J) (gJ), kaempferol (kaempferol) (K), Quercetin (quercetin) (Q) and Isorhamnetin (isorhamnetin) (I) distribute the recovery (recovery) of extraction gained after 30 minutes with cyclohexane and MEK through the aqueous hydrochloric acid solution reflux
Sample (sample) | BB | gA | gB | gC | gJ | K | Q | I |
The recovery (recovery) | 103.0±3.0 | 98.2±2.1 | 102.3±1.5 | 97.2±2.1 | 98.1±1.1 | 97.3±2.1 | 98.6±2.9 | 96.8±2.0 |
Contained active component comprises ginkgolides (Bilobalide (bilobalide), ginkalide A (ginkgolide A), ginkolide B (ginkgolide B), ginkalide C (ginkgolide C), bilobalide J (ginkgolide J)) and flavonols (kaempferol (kaempferol), Quercetin (quercetin) and Isorhamnetin (isorhamnetin)) compound in the simultaneously quantitative biloba extract thing of this method, and only need just can reach through simple hydrolysing step.Inspection amount line linear splendid, the linearly dependent coefficient value is more than 0.999.The analysis result repeatability that obtains is splendid, and the variation value all is controlled in 3.2%.Recovery experiment shows that desire analysis composition does not change because of hydrolysis and extraction process.Avoid tubing string chromatography or Solid-Phase Extraction or shooting flow to analyse or the like the prepurification method, be created in the preposition purge process desire and analyze the loss of composition, the shortcoming that repeatability is not good and the recovery is low.Need not cause productive rate fixedly not cause the inaccurate of analysis result through derivative reaction yet.And the simultaneously quantitative contained active component of biloba extract thing comprises ginkgolides (Bilobalide (bilobalide), ginkalide A (ginkgolide A), ginkolide B (ginkgolide B), ginkalide C (ginkgolide C), bilobalide J (ginkgolide J)) and flavonols (kaempferol (kaempferol), Quercetin (quercetin) and Isorhamnetin (isorhamnetin)) compound.
List of references:
1.DeFeudis,F.V.Ginkgo biloba Extract(EGb 761):From Chemistry to Clinic;Ullstein Medical:Weisbaden,1998.
2.Joyeux,M,;Lobstein,A.;Anton,R,;Mortier,F.Planta Med.1995,61,126-129.
3.Sticher,O.Planta Med.1993,59,2-11.
4.Xing,S.Y.;Wu,D.J.;Xing,L.F.;You,X.L.;Zhang,Y.P.;Sun,X.;Liu,Y.Q.Yi ChuanXue Bao 2002,29,928-935.
5.Pietta,P.G.;Maud,P.L.;Rava,A.,/..Pharm.Biomed.Anal.1992,10,1077-1079.
6.Chen,P.;Su,N.L.;Nie,L.H.;Yao,S.Z.;Zeng,J.G.J.Chromatogr.Sci.1998,36,197-200.
7.Van Beek,T.A.J.Chromatogr.A.2002,967,21-55.
8.Huh,H.;Staba,E.J.Planta Med.1993,59,232-239.
9.Yang,C.;Xu,Y.R,;Yao,W.X.J.Agric.Food Chem.2002,50,846-849.
10.Deng,F.;Zito,S.W.J.Chromatogr.A.2003,986,323-327.
11.Chauret,N.;Carder,J.;Mancini,M.;Neufeld,R.;Weber,M.;Archambault,J.J.Chromatogr.1991,588,281-287.
12.Hasler,A,;Sficher,O.;Meier,B.J.Chromatogr.1992,605,43-48.
13.Van Beek,T.A.;Van Veldhuizen,A.;Lelyveld,G.Pt;Piron,I.;Lankhorst,P.P.Phytochem.Anal.1993,4,263-268.
14.Choi,Y.H.;Choi,H.K.;Hazekamp,A.;Bermejo,P.;Schilder,Y.;Erkelens,C.;Verpoorte,R.Chem.Pharm.Bull.2003,51,358-161.
Claims (4)
1, the method for contained active ingredient in a kind of fast qualitative and the quantitative test ginkgo goods is the qualitative and quantitative analytical approach at institute's bilobalide-containing in the ginkgo and flavonols compound, and it comprises:
(a) measure the target signal of ginkgo goods active component as nuclear magnetic resonance spectrometry with the H-2 ' of the H-12 of ginkgolides and flavonols;
(b) have the deuterate solvent of obvious solvent effect and deuterate solvent system that various high polar solvent mixes are measured the ginkgo goods as nuclear magnetic resonance spectrometry dissolving and test solvent with aromatic solvent;
(c) with the internal standard product of benzene substituted compound as nuclear magnetic resonance spectrometry measurement ginkgo goods;
(d) after the strong acid hydrolysis with the combination of various concentration and temperature, with nuclear magnetic resonance spectrometry qualitative and quantitative analysis simultaneously to measure the ginkgolides and the flavonols compound of ginkgo goods.
2, the method for contained active ingredient in fast qualitative as claimed in claim 1 and the quantitative test ginkgo goods, wherein, this aromatic solvent is deuterate benzene, deuterate toluene and deuterate pyridine.
3, the method for contained active ingredient in fast qualitative as claimed in claim 1 and the quantitative test ginkgo goods, wherein, this high polar solvent is deuterate methyl alcohol, deuterate acetone, deuterate dioxy sulfoxide and deuterate pyridine.
4, the method for contained active ingredient in fast qualitative as claimed in claim 1 and the quantitative test ginkgo goods, wherein, this benzene substituted compound is 1,3, the 5-trimethoxy-benzene.
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