CN102141555A - Method for establishing high-pressure liquid-phase fingerprinting of evodia and extractives thereof - Google Patents
Method for establishing high-pressure liquid-phase fingerprinting of evodia and extractives thereof Download PDFInfo
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Abstract
The invention provides a method for establishing the HPLC (High Performance Liquid Chromatography) fingerprinting quality of a GAP (Good Aquaculture Practices) evodia material and extractives thereof in Yuqing, Guizhou, and the method comprises the following steps: preparing a sample solution to be tested; preparing the extractives; determining chromatography conditions; utilizing an HPLC to measure; selecting two counterfeit drugs (pepper and coriaria sinica) of the evodia for the first time to finish the applicability inspection of the fingerprinting; obtaining the HPLC fingerprinting of the evodia material and the extractives thereof; expressing the integral chemical information of the evodia material and the extractives thereof more comprehensively; and determining the finger characteristics of the evodia material and the extractives thereof. The fingerprinting comprises a water solubility part and a lipid solubility part, has the characteristics of simple and convenient method, good repeatability, multiple characteristic peaks, accuracy and reliability. The established HPLC fingerprinting can be used for effectively controlling the quality of the evodia material and the extractives thereof and identifying truth or falsity.
Description
Technical field
The present invention relates to the method for building up of Yuqing, a kind of Guizhou GAP evodia rutaecarpa medicinal material and extractive HPLC (high performance liquid chromatography) finger-print thereof, and the evodia rutaecarpa medicinal material and the extractive HPLC standard finger-print thereof of gained thus, the Pharmaceutical Analysis technical field belonged to.
Background technology
Evodia rutaecarpa is rutaceae evodia rutaecarpa Evodia rutaecarpa (Juss.) Benth., Shi Hu Evodiarutaecarpa (Juss.) Benth.var.officinalis (Dode) Huang or the dry almost ripe fruit of dredging hair evodia rutaecarpa Evodiarutaecarpa (Juss.) Benth.var.bodinieri (Dode) Huang.Beginning is stated from Shennong's Herbal, main product in Guizhou, Hunan, Chongqing, Jiangxi, zhejiang and other places.Evodia rutaecarpa is famous genunie medicinal materials in Guizhou Province and seedling medicine commonly used, accounts for more than 30% of national total production, and the Yuqing, Guizhou has been carried out extensive artificial growth, and succeeded by GAP standardization requirement.
Traditional medicinal material and extract evaluation index thereof have significant limitation." only control the quality of evodia rutaecarpa under Chinese pharmacopoeia (version was an one in 2010) the evodia rutaecarpa item with total alkali in the evodia rutaecarpa medicinal material and limonin content, fail to reflect more all sidedly the situation of other compositions in evodia rutaecarpa and the extract thereof, traditional Chinese medicine fingerprint provides solution for this problem.
At present, existing evodia rutaecarpa liposoluble, water-soluble fingerprint technology (publication number: CN1932506A, CN1932507A) research, but fat-soluble, water-soluble portion research that this fingerprint pattern technology has only been done respectively, and the characteristic peak negligible amounts does not still have the investigative technique that comprehensively reflects full composition of GAP base, Yuqing, Guizhou evodia rutaecarpa and evodia extract finger-print in known technology.At the existing deficiency of present evodia rutaecarpa fingerprint pattern technology, the present invention studies evodia rutaecarpa medicinal material and extract finger-print thereof with the HPLC linear gradient elution method, select for use the more common two kinds of pseudo-product (Chinese prickly ash, Coriaria sinica) of evodia rutaecarpa to finish the check of finger-print applicability first, the finger-print of being set up has been integrated evodia rutaecarpa water-soluble composition and liposoluble constituent, can embody the overall chemical information of evodia rutaecarpa medicinal material and extract thereof more all sidedly; The degree of separation and the peak shape at the total peak of evodia rutaecarpa medicinal material of setting up and extractive HPLC fingerprint thereof are better; This finger-print has been included water-soluble portion and fat-soluble part in evodia rutaecarpa medicinal material and the extract thereof in addition, good reproducibility, workable, meet finger-print and detect requirement, for the quality control and the real and fake discrimination of evodia rutaecarpa medicinal material and extract thereof provides a kind of new method.
Summary of the invention
Purpose of the present invention provides a kind of construction method for evodia rutaecarpa medicinal material and extractive HPLC fingerprint thereof, and resulting evodia rutaecarpa medicinal material of method and extract finger-print thereof thus.
Evodia rutaecarpa medicinal material of the present invention and extractive HPLC fingerprint construction method thereof are as follows:
1, the construction method of Yuqing, Guizhou evodia rutaecarpa medicinal material HPLC finger-print:
1.1 the preparation of need testing solution
Precision takes by weighing sample powder (the crossing 60 mesh sieves) 0.1g～1g that is dried to constant weight, put in the tool plug conical flask, adding concentration is methanol solution 25mL～50mL of 45%～90%, weighs, sonicated 10 minutes～1.5 hours, put coldly, weigh, supply the weight that subtracts mistake, filter, it is an amount of to get subsequent filtrate, filters with 0.45 μ m miillpore filter, promptly.
1.2HPLC analyze:
Chromatographic condition is: chromatographic column: Diamonsil C
18Post (250mm * 4.6mm, 5 μ m); Column temperature: 20 ℃～35 ℃; Flow velocity: 0.8mLmin
-1～1.2mLmin
-1Chromatographic peak spectra collection scope: 190nm～400nm, moving phase is methyl alcohol-0.02% phosphoric acid (pH 2.95～3.05), adopt the linear gradient elution mode: 0 minute → 35 minutes → 40 minutes → 53 minutes → 56 minutes → 80 minutes, methyl alcohol: 15% → 31% → 50% → 53% → 72% → 95%, 0.02% phosphate aqueous solution 85% → 69% → 50% → 47% → 28% → 5%, detect wavelength 250nm ± 2nm, obtain evodia rutaecarpa medicinal material HPLC finger-print.
By the method for foregoing invention, by 21 batches of evodia rutaecarpa medicinal material samples are made up the HPLC finger-print and analyze comparison, find out its common characteristic peak (totally 22 peaks), obtain the finger-print of evodia rutaecarpa medicinal material, the retention time (t at 22 total peaks
R) be respectively: 10.0 minutes, 12.5 minutes, 14.0 minutes, 16.5 minutes, 17.4 minute, 18.7 minutes, 23.0 minutes, 24.6 minutes, 26.1 minute, 28.2 minutes, 30.1 minutes, 36.3 minutes, 47.7 minute, 50.0 minutes, 51.9 minutes, 52.6 minutes, 62.3 minute, 65.4 minutes, 69.4 minutes, 79.5 minute, 81.1 minutes, 82.6 minutes.
2, the construction method of Yuqing, Guizhou evodia extract HPLC finger-print:
2.1 the preparation of evodia extract:
2.1.1 the preparation of evodia rutaecarpa water extract: it is an amount of to take by weighing evodia rutaecarpa, and with 5～15 times of water gaging refluxing extraction 1～3 time, each 0.5～3 hour, merging filtrate placed evaporating dish, and it is 1.20～1.35 thick paste that water-bath is steamed to relative density.After thick paste is put in the drying under reduced pressure case in 0.02Mpa～0.15Mpa, 40 ℃～60 ℃ dry 24 hours～48 hours down, take out and grind promptly.
2.1.2 the preparation of evodol extract: it is an amount of to take by weighing evodia rutaecarpa, and with the alcohol reflux of 5～15 times of amounts 60%～80% 1～3 time, each 2 hours～4 hours, merging filtrate placed evaporating dish, and it is 1.20～1.35 thick paste that water-bath is steamed to relative density.After thick paste is put in the drying under reduced pressure case in 0.02Mpa～0.15Mpa, 40 ℃～60 ℃ dry 24 hours～48 hours down, take out and grind promptly.
2.2 the preparation of need testing solution
Take by weighing dry powder medicinal extract 0.1g～1g, the accurate title, decide, and puts in the tool plug conical flask of 50mL, add 45%～90% methyl alcohol 25mL～50mL, weigh, ultrasonic Extraction 10 minutes～90 minutes is put cold, weigh, supply the weight that subtracts mistake, filter, go subsequent filtrate an amount of, filter with 0.45 μ m miillpore filter, promptly.
2.3HPLC analyze:
Chromatographic condition is: chromatographic column ZORBAX Eclipse XDB-C
18(4.6 * 150mm, 5 μ m) analytical column, moving phase is acetonitrile-0.1% aqueous formic acid, adopt moving phase binary gradient elution system, 0 minute → 5 minutes → 38 minutes → 65 minutes, acetonitrile: 5% → 5% → 23% → 100%, 0.1% aqueous formic acid, 95% → 95% → 77% → 0% flow velocity is 1mLmin
-1The detection wavelength is 258nm ± 2nm, and 20 ℃～35 ℃ of column temperatures obtain evodia extract HPLC finger-print.
By the method for foregoing invention, by the evodia extract sample being made up the HPLC finger-print and analyzing, find out its characteristic peak (totally 20 peaks), obtain the finger-print of evodia extract, the retention time (t of 20 characteristic peaks
R) be respectively:
The retention time of evodol extract: 9.6 minutes, 12.2 minutes, 13.2 minutes, 15.9 minutes, 16.4 minute, 20.8 minutes, 21.3 minutes, 22.9 minutes, 24.4 minute, 25.7 minutes, 28.3 minutes, 35.7 minute, 39.2 minutes, 40.3 minutes, 41.3 minute, 53.3 minutes, 54.0 minutes, 55.6 minute, 56.6 minutes, 66.1 minutes.
The retention time of evodia rutaecarpa water extract: 9.6 minutes, 12.1 minutes, 13.2 minutes, 15.9 minutes, 16.4 minute, 20.8 minutes, 21.3 minutes, 22.9 minutes, 24.4 minute, 25.6 minutes, 28.2 minutes, 35.7 minute, 39.1 minutes, 40.2 minutes, 41.6 minute, 53.3 minutes, 54.0 minutes, 55.5 minute, 56.6 minutes, 63.8 minutes.
3. Yuqing, Guizhou evodia rutaecarpa medicinal material and extractive HPLC fingerprint method thereof have following significant advantage and purposes:
A. the finger-print of being set up has been integrated evodia rutaecarpa water-soluble composition and liposoluble constituent, can embody the overall chemical information of Yuqing, Guizhou evodia rutaecarpa medicinal material and extract thereof more all sidedly;
B. this method finger-print is than known method, and the chromatographic peak number is more, and degree of separation is better, and the quality control precision is higher;
C. compare with public technology, the need testing solution preparation process of this method is simpler and more direct, chromatographic condition is easier to realize that the experimental result reappearance is better;
D. the finger-print of being set up can be used for the real and fake discrimination and the quality control of evodia rutaecarpa medicinal material and extract thereof.
Description of drawings
Figure 112 criticizes the different places of production, Yuqing evodia rutaecarpa medicinal materials fingerprint common pattern;
The comparison collection of illustrative plates (S1 is that evodia rutaecarpa, S2 are that Chinese prickly ash, S3 are Coriaria sinica) of Fig. 2 Chinese prickly ash, Coriaria sinica and evodia rutaecarpa finger-print;
Fig. 3 evodol extract characteristic spectrum;
Fig. 4 evodia rutaecarpa water extract characteristic spectrum.
Embodiment
The method for building up of embodiment one, evodia rutaecarpa medicinal material HPLC finger-print
1 instrument, sample, reagent and reagent
1.1 instrument: Agilent 1100 high performance liquid chromatographs, DAD detecting device, Agilent Chemstation chromatographic work station, chromatographic column: Diamonsil C
18Post (250mm * 4.6mm, 5 μ m).
1.2 sample: 21 batches of evodia rutaecarpa medicinal material samples respectively from Guizhou, Hunan, Chongqing, Jiangxi, zhejiang and other places, are the fruit of rutaceae evodia rutaecarpa Evodia rutaecarpa (Juss.) Benth. through evaluation.
1.3 reagent: methyl alcohol is chromatographically pure, and water is pure water, and it is pure that all the other reagent are analysis.
2 methods and result
2.1 the preparation of need testing solution
Get the about 0.2g of sample powder (crossing 60 mesh sieves) that is dried to constant weight, the accurate title, decide, and puts in the 50mL tool plug conical flask, add 50% methyl alcohol 25mL, weigh, sonicated (power 250W, frequency 33kHz) 20 minute, put coldly, weigh, supply the weight that subtracts mistake, filter, it is an amount of to get subsequent filtrate, filters with 0.45 μ m miillpore filter, promptly.
2.2HPLC analyze:
Chromatographic column: Diamonsil C
18Post (250mm * 4.6mm, 5 μ m); Column temperature: 25 ℃; Flow velocity: 1.0mLmin
-1Chromatographic peak spectra collection scope: 190nm～400nm detects wavelength 250nm.Methyl alcohol-0.02% phosphoric acid (pH2.95～3.05) gradient elution, condition of gradient elution sees Table 1.
Table 1 condition of gradient elution
Method by foregoing invention, make up the HPLC finger-print and analyze comparison by being produced from Yuqing, 12 batches of Guizhou the different place of production of evodia rutaecarpa medicinal material evodia rutaecarpa medicinal material sample with 9 batches, find out its common characteristic peak (totally 22 peaks), obtain the finger-print of evodia rutaecarpa medicinal material, the retention time (t at 22 total peaks
R) be respectively: 10.0 minutes, 12.5 minutes, 14.0 minutes, 16.5 minutes, 17.4 minute, 18.7 minutes, 23.0 minutes, 24.6 minutes, 26.1 minute, 28.2 minutes, 30.1 minutes, 36.3 minutes, 47.7 minute, 50.0 minutes, 51.9 minutes, 52.6 minutes, 62.3 minute, 65.4 minutes, 69.4 minutes, 79.5 minute, 81.1 minutes, 82.6 minutes.
The pseudo-product of evodia rutaecarpa are analyzed: adopt in the literary composition " preparation of need testing solution " and " chromatographic condition " to carry out the check of finger-print specificity, two kinds of puppets of mensuration evodia rutaecarpa are tasted with discrimination Chinese prickly ash, Coriaria sinica.The result shows that 2 pseudo-product similarities are relatively poor, observes from graph direct and can distinguish two kinds of pseudo-product, illustrates that the HPLC fingerprint spectrum method of foundation can be promoted the true and false as the evodia rutaecarpa medicinal material, good and bad discriminating means.
The method for building up of embodiment two, evodia extract HPLC finger-print
1 instrument, sample, reagent and reagent
1.1 instrument: Agilent 1100 high performance liquid chromatographs, DAD detecting device, Agilent Chemstation chromatographic work station, chromatographic column: ZORBAX Eclipse XDB-C
18(4.6 * 250mm, 5 μ m).
1.2 sample: the crude drug of evodia extract sample produces the dry almost ripe fruit of dredging hair evodia rutaecarpa Evodiarutaecarpa (Juss.) Benth.var.bodinieri (Dode) Huang for the Yuqing, Guizhou.
1.3 reagent: acetonitrile is a chromatographically pure, and water is pure water, and it is pure that all the other reagent are analysis.
2 methods and result
2.1 the preparation of evodia extract:
2.1.1 the preparation of evodia rutaecarpa water extract: take by weighing evodia rutaecarpa 20g, with 10 times of water gaging refluxing extraction 3 times, each 2 hours, merging filtrate placed evaporating dish, and it is 1.30 thick paste that water-bath is steamed to relative density.After thick paste is put in the drying under reduced pressure case in 0.05Mpa, 60 ℃ dry 24 hours down, take out and grind promptly.
2.1.2 the preparation of evodol extract: take by weighing evodia rutaecarpa 20g, with 6 times of amount alcohol reflux of 60% 3 times, each 2 hours, merging filtrate placed evaporating dish, and it is 1.3 thick paste that water-bath is steamed to relative density.After thick paste is put in the drying under reduced pressure case in 0.05Mpa, 60 ℃ dry 24 hours down, take out and grind promptly.
2.2 the preparation of need testing solution
Take by weighing dry powder medicinal extract 0.1g, accurately claim surely, put in the tool plug conical flask of 50ml, add 50% methyl alcohol 25mL, weigh, ultrasonic Extraction 20 minutes is put coldly, weighs, and supplies the weight that subtracts mistake, filters, and goes subsequent filtrate an amount of, filters with 0.45 μ m miillpore filter, promptly.
2.3HPLC analyze:
Chromatographic column: ZORBAX Eclipse XDB-C
18(4.6 * 250mm, 5 μ m); Column temperature: 30 ℃; Flow velocity: 1.0mLmin
-1Chromatographic peak spectra collection scope: 190nm～400nm detects wavelength 258nm.Acetonitrile-0.1% aqueous formic acid (pH 2.55～2.65) gradient elution, condition of gradient elution sees Table 2.
Table 2 condition of gradient elution
By the method for foregoing invention, by the evodia extract sample being made up the HPLC finger-print and analyzing, find out its characteristic peak (totally 20 peaks), obtain the finger-print of evodia extract, the retention time (t of 20 characteristic peaks
R) be respectively:
The retention time of evodol extract: 9.6 minutes, 12.2 minutes, 13.2 minutes, 15.9 minutes, 16.4 minute, 20.8 minutes, 21.3 minutes, 22.9 minutes, 24.4 minute, 25.7 minutes, 28.3 minutes, 35.7 minute, 39.2 minutes, 40.3 minutes, 41.3 minute, 53.3 minutes, 54.0 minutes, 55.6 minute, 56.6 minutes, 66.1 minutes.
The retention time of evodia rutaecarpa water extract: 9.6 minutes, 12.1 minutes, 13.2 minutes, 15.9 minutes, 16.4 minute, 20.8 minutes, 21.3 minutes, 22.9 minutes, 24.4 minute, 25.6 minutes, 28.2 minutes, 35.7 minute, 39.1 minutes, 40.2 minutes, 41.6 minute, 53.3 minutes, 54.0 minutes, 55.5 minute, 56.6 minutes, 63.8 minutes.
Claims (3)
1. the method for building up of GAP base, Yuqing, Guizhou evodia rutaecarpa efficient liquid-phase chromatograph finger print atlas is characterized in that may further comprise the steps:
Step 1, the preparation of need testing solution:
Precision takes by weighing the sample powder 0.1g～1g that is dried to constant weight, crosses 60 mesh sieves, places tool plug conical flask, the adding volume ratio is methanol solution 25mL～50mL of 45%～90%, weigh, sonicated 10 minutes～90 minutes is put cold, weigh, supply the weight that subtracts mistake, filter, it is an amount of to get subsequent filtrate, filter with 0.45 μ m miillpore filter, promptly;
Step 2, efficient liquid phase chromatographic analysis:
Accurate need testing solution 2 μ L～20 μ L sample introductions of drawing step 1, chromatographic condition is as follows: chromatographic column is Diamonsil C
18Post, packing material size 2 μ m～8 μ m, column length 150mm～250mm, column temperature: 20 ℃～35 ℃; Flow velocity: 0.8mLmin
-1～1.2mLmin
-1Chromatographic peak spectra collection scope: 190nm～400nm, moving phase is mixed by methyl alcohol-0.01～0.02% phosphate aqueous solution (pH 2.95～3.05) by volume, adopt the linear gradient elution mode: from 0 minute → 35 minutes → 40 minutes → 53 minutes → 56 minutes → 80 minutes, methyl alcohol ratio: 15% → 31% → 50% → 53% → 72% → 95% (volume ratio), 0.02% phosphate aqueous solution ratio: 85% → 69% → 50% → 47% → 28% → 5% (volume ratio), detect wavelength 250nm ± 2nm; Obtain evodia rutaecarpa HPLC finger-print;
Step 3, analyze relatively:
Measure 12 batches of evodia rutaecarpa medicinal material sample efficient liquid-phase chromatograph finger print atlas and analyze comparison, obtain the evodia rutaecarpa medicinal materials fingerprint that constitutes by its common characteristic peak, the retention time t at 22 total peaks that this finger-print has
RBe respectively: 10.0 minutes, 12.5 minutes, 14.0 minutes, 16.5 minutes, 17.4 minutes, 18.7 minutes, 23.0 minutes, 24.6 minutes, 26.1 minutes, 28.2 minutes, 30.1 minutes, 36.3 minutes, 47.7 minutes, 50.0 minutes, 51.9 minutes, 52.6 minutes, 62.3 minutes, 65.4 minutes, 69.4 minutes, 79.5 minutes, 81.1 minutes, 82.6 minutes.
2. method according to claim 1 is characterized in that: retention time t
R=26.1 minutes No. 9 peak is chlorogenic acid, t
R=65.4 minutes No. 18 peak is rutaecarpin, t
R=69.4 minutes No. 19 peak is Rutaecarpine.
3. the method for building up of Yuqing, Guizhou evodia extract efficient liquid-phase chromatograph finger print atlas:
Step 1, the preparation of evodia extract:
The preparation of evodia rutaecarpa water extract: take by weighing an amount of evodia rutaecarpa, with 5～15 times of water gaging refluxing extraction 1～3 time, each 0.5 hour～3 hours, merging filtrate, place evaporating dish, it is 1.20～1.35 thick paste that water-bath is steamed to relative density, thick paste is put in the drying under reduced pressure case in 0.02Mpa～0.15Mpa after then, drying is 24 hours～48 hours under 40 ℃～60 ℃, takes out to grind promptly;
The preparation of evodol extract: take by weighing an amount of evodia rutaecarpa, alcohol reflux 1～3 time with 5～15 times of amounts 60%～80% (volume ratio), each 2～4 hours, merging filtrate, place evaporating dish, it is 1.20～1.35 thick paste that water-bath is steamed to relative density, after thick paste is put in the drying under reduced pressure case in 0.02Mpa～0.15Mpa, dry 24h～48h under 40 ℃～60 ℃ takes out grinding promptly;
Step 2, the preparation of need testing solution:
The preparation of need testing solution: take by weighing the powder medicinal extract of 0.1g～1g drying, the accurate title, decide, and places the tool plug conical flask of 50mL, add 45%～90% methyl alcohol (volume ratio) 25ml～50mL, weigh, ultrasonic Extraction 10 minutes～90 minutes is put cold, weigh, supply the weight that subtracts mistake, filter, go subsequent filtrate an amount of, filter with 0.45 μ m miillpore filter, promptly;
Step 3, efficient liquid phase chromatographic analysis:
Efficient liquid phase chromatographic analysis: the accurate need testing solution 2 μ L～20 μ L sample introductions of drawing, chromatographic condition is as follows: chromatographic column ZORBAX Eclipse XDB-C
18Analytical column, packing material size 5 μ m, column length 150mm, column internal diameter 4.6mm, 20 ℃～35 ℃ of column temperatures, moving phase is that acetonitrile-0.1% (volume ratio) aqueous formic acid (pH 2.55～2.65) mixes, adopt moving phase binary gradient elution system: 0 minute → 5 minutes → 38 minutes → 65 minutes, acetonitrile: 5% → 5% → 23% → 100%, 0.1% formic acid (volume ratio) aqueous solution 95% → 95% → 77% → 0%, flow velocity is 1mLmin
-1, the detection wavelength is 258nm ± 2nm; Obtain evodia extract HPLC finger-print;
Step 4, analyze relatively:
Measure evodia extract sample efficient liquid-phase chromatograph finger print atlas and also analyze, obtain the evodia extract finger-print that is made of its characteristic peak, the retention time tR of 20 characteristic peaks that this finger-print has is respectively:
The retention time of evodol extract: 9.6 minutes, 12.2 minutes, 13.2 minutes, 15.9 minutes, 16.4 minutes, 20.8 minutes, 21.3 minutes, 22.9 minutes, 24.4 minutes, 25.7 minutes, 28.3 minutes, 35.7 minutes, 39.2 minutes, 40.3 minutes, 41.3 minutes, 53.3 minutes, 54.0 minutes, 55.6 minutes, 56.6 minutes, 66.1 minutes.
The retention time of evodia rutaecarpa water extract: 9.6 minutes, 12.1 minutes, 13.2 minutes, 15.9 minutes, 16.4 minutes, 20.8 minutes, 21.3 minutes, 22.9 minutes, 24.4 minutes, 25.6 minutes, 28.2 minutes, 35.7 minutes, 39.1 minutes, 40.2 minutes, 41.6 minutes, 53.3 minutes, 54.0 minutes, 55.5 minutes, 56.6 minutes, 63.8 minutes.
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