CN105738546A - Establishment method of curcuma aromatica medicine fingerprint map and the fingerprint map thereof - Google Patents
Establishment method of curcuma aromatica medicine fingerprint map and the fingerprint map thereof Download PDFInfo
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Abstract
The invention discloses an establishment method of a curcuma aromatica medicine fingerprint map and the fingerprint map thereof, and particularly, provides establishment of a HPLC fingerprint map for controlling the quality of curcuma aromatica medicine. The method includes the steps of: 1) preparation of a reference substance solution: preparing the reference substance solutions of curdione, curcumadiol, procurcumenol; 2) preparation of a sample solution: extracting the curcuma aromatica medicine and filtering an extract liquid; 3) HPLC detection to obtain the fingerprint map: performing HPLC detection with octadecylsilane chemically bonded silica as a filler and an acetonitrile-tetrahydrofuran-0.1% phosphoric acid water system as a mobile phase in a chromatographic column in a gradient elution manner, wherein column temperature is 30 DEG C, ultraviolet detection wavelength is 230-250 nm and time is 60-65 min; and 4) similarity evaluation: introducing the obtained fingerprint map into "fingerprint similarity evaluation system of traditional Chinese medicine chromatography" (2004A version) similarity software for performing similarity evaluation. The method is simple, quick and accurate, has good repeatability, and provides powerful guarantee for comprehensive and effective control on quality of the curcuma aromatica medicine.
Description
Technical field
The invention belongs to pharmaceutical analysis technical field, relate to the method for quality control of Chinese medicinal material, particularly relate to method for building up and the finger printing thereof of Radix Curcumae HPLC-FPS.
Background technology
Chinese medicine fingerprint refer to some Chinese crude drug or Chinese medicine preparation appropriately processed after, adopt certain analysis means, the chromatogram that can indicate its chemical feature obtained or spectrogram.The features such as it can more fully reflect kind and the quantity of chemical composition contained by medical material, effectively embodies globality and the comprehensive function of Chinese medicine ingredients, quick with it, accurate have been widely used to be identified and the aspect such as quality control in Analysis of Chinese Traditional Medicine.
Radix Curcumae is the dry rhizome of zingiberaceous plant Radix Curcumae CurcumaaromaticaSalisb., it it is one of important Ethnic crude drugs of China, it is distributed mainly on the ground such as Hengxian County, the Lingshan, Nanning, there is removing blood stasis circulation of qi promoting, inducing menstruation to relieve menalgia effect, cure mainly costa sternales twinge, amenorrhea, rheumatism shoulder arm pain, tumbling and swelling etc., wait [1].Modern pharmacology is it is demonstrated experimentally that Radix Curcumae also has the effect such as antiinflammatory [2], immunosuppressant [3], pain easing and hemostasis [4], antioxidation [5].Radix Curcumae rhizome chemical composition is complex, rhizome is containing volatile oil, α in oil-, nopinene, Austria, zingiberene, 1-α γ-curcumene, 1-β-curcumene, Camphora, terpineol, cuminyl alcohol (Cumiylaleohol), d-Borneolum Syntheticum, zingiberol (zingiberol) and a small amount of curcumin.Volatile ingredient mainly contains cineole (Eucalypto1), elemene (Elemene), curzerene (Curzerene), B-olive ketenes (p-Elemenone), 3,7-Cyclodecadien-1-one, 3,7-dimethyl-10-(1-methylethylidene)-, (E,E)-(Germacrone), curdione (Curdione), (-)-Neocurdione (Neocurdione), additionally includes the compositions such as resinae, sterols, many peptides, triterpenes.Due to the impact of the factor such as climate, the place of production, different Radix Curcumae medical material ingredients there is also different.The GC-MS of volatile oil component in the research of Radix Curcumae pharmacological action and Radix Curcumae is analyzed by existing scholar, but yet there are no the research of other quality aspects.This patent carries out HPLC finger printing by different Radix Curcumae of originating to ten batches and studies, and establishes the finger printing of Radix Curcumae medical material, and the quality control for this medical material provides powerful guarantee.
Summary of the invention
It is an object of the invention to provide the method for building up of a kind of Radix Curcumae medicinal materials fingerprint and the Radix Curcumae medical material standard finger-print that thus method obtains.The present invention, by the research to Radix Curcumae medical material efficient liquid-phase chromatograph finger print atlas, obtains a kind of Radix Curcumae quality of medicinal material control method preferably.
The method of the Radix Curcumae medical material efficient liquid-phase chromatograph finger print atlas of the present invention comprises the following steps:
(1) preparation of reference substance solution: precision weighs curdione, curcumadiol, procurcumenol reference substance, respectively with methanol be configured to every 1mL containing curdione 0.1～0.2mg, curcumadiol 0.01～0.02mg, procurcumenol 0.02～0.04mg solution, as reference substance solution；
(2) preparation of need testing solution: precision weighs Radix Curcumae medicinal material coarse powder, adds methanol supersound extraction 30～60min, filters, takes subsequent filtrate as need testing solution；
(3) chromatographic condition: chromatographic column, with octadecylsilane chemically bonded silica for filler, adopts gradient elution, mobile phase is the gradient eluent of acetonitrile-oxolane-0.1% phosphoric acid water system composition, ultraviolet detection: wavelength is 230～250nm；
(4) measure: accurate need testing solution 10～20 μ L of absorption injects high performance liquid chromatograph, according to high effective liquid chromatography for measuring, obtains finger printing.
Preferably, in step (1), the concentration of curdione reference substance solution is 0.1990mg mL-1, the concentration of curcumadiol reference substance solution is 0.0152mg mL-1, the concentration of procurcumenol reference substance solution is 0.0295mg mL-1。
Preferably, in step (2), Radix Curcumae medicinal material coarse powder crosses 40 mesh sieves, and Radix Curcumae medical material weighs as about 0.5g.
Preferably, in step (2), extraction step is for adopting methanol supersound extraction, and extraction time is 30min.
Preferably, the gradient eluent that mobile phase is acetonitrile-oxolane-0.1% phosphoric acid water system of gradient elution in step (3)；Elution time is 65min；Flow velocity 1.0mL min-1；Column temperature: 30 DEG C.
Gradient elution described in described step (3) chromatographic condition, gradient elution program carries out with the configuration of following volumetric concentration: when 0 minute, 0.1% phosphate aqueous solution that acetonitrile-oxolane (10:1) that mobile phase A is 15%, Mobile phase B are 85%；When 50 minutes, 0.1% phosphate aqueous solution that acetonitrile-oxolane (10:1) that mobile phase A is 85%, Mobile phase B are 15%；50.1 minute time, 0.1% phosphate aqueous solution that acetonitrile-oxolane (10:1) that mobile phase A is 15%, Mobile phase B are 85%；When 65 minutes, 0.1% phosphate aqueous solution that acetonitrile-oxolane (10:1) that mobile phase A is 15%, Mobile phase B are 85%.
Preferably, during step (4) measures, HPLC automatic sampler sample introduction 20 μ L.
Preferably, having 12 features to have peak in stricture of vagina collection of illustrative plates, wherein No. 1 peak is curcumadiol reference peak, and No. 5 peaks are procurcumenol, and No. 11 peaks are curdione, specific as follows:
No. 1 peak, Average residence time is 9.73min, and peak area is 875.686；
No. 2 peaks, Average residence time is 13.71min, and peak area is 403.140；
No. 3 peaks, Average residence time is 14.54min, and peak area is 336.420；
No. 4 peaks, Average residence time is 15.52min, and peak area is 118.226；
No. 5 peaks, Average residence time is 24.54min, and peak area is 264.982；
No. 6 peaks, Average residence time is 30.12min, and peak area is 104.990；
No. 7 peaks, Average residence time is 31.62min, and peak area is 2344.064；
No. 8 peaks, Average residence time is 32.45min, and peak area is 926.635；
No. 9 peaks, Average residence time is 33.65min, and peak area is 166.430；
No. 10 peaks, Average residence time is 34.76min, and peak area is 172.176；
No. 11 peaks, Average residence time is 37.48min, and peak area is 415.697；
No. 12 peaks, Average residence time is 47.25min, and peak area is 288.828.
Another object of the present invention is to the application providing the aforementioned finger printing obtained in Radix Curcumae medical material and Radix Curcumae medicinal substances extract and preparation detection.
As the preferred embodiment of the present invention, 10 batches of Radix Curcumae medicinal materials fingerprint data are studied, the method establishing Radix Curcumae medical material efficient liquid-phase chromatograph finger print atlas, comprise the following steps:
(1) preparation of reference substance solution: precision weighs curdione, curcumadiol, procurcumenol in right amount, adds methanol respectively and makes 0.1990g L-1Curdione reference substance solution, 0.0152g L-1Curcumadiol reference substance solution 0.0295g L-1The reference substance solution of procurcumenol reference substance solution.
(2) preparation of need testing solution: take Radix Curcumae medicinal powder and be about 0.5g, accurately weighed, put in tool plug conical flask, accurate addition methanol 25mL, close plug, weighed quality, supersound extraction 30min, let cool, weighed weight again, supplies the weight of less loss, shakes up with methanol, filter, take subsequent filtrate and filter with 0.45 μm of microporous filter membrane and get final product.
(3) efficient liquid phase chromatographic analysis: AgelaPromosilC18Chromatographic column；Acetonitrile-oxolane (10:1) (A)-0.1% phosphoric acid water (B) gradient elution；Flow velocity 1.0mL min-1；Detection wavelength 250nm；Column temperature 30 DEG C；Sample size 20 μ L, carries out gradient elution by table 1:
Table 1 mobile phase elution program
Carry out HPLC analysis with this understanding, obtain the finger printing of Radix Curcumae medical material.
null(4) determination of standard finger-print: according to method provided by the invention，10 batches of Radix Curcumae medical materials of separate sources are established HPLC finger printing，Pass through com-parison and analysis，Determine 12 common characteristic peaks，With No. 1 peak of object of reference and curcumadiol peak for S peak，Calculate the relative retention time at each common characteristic peak and S peak，Its relative retention time should setting ± 5% in，Setting is: 1.000 (peaks 1)、1.410 (peaks 2)、1.495 (peaks 3)、1.596 (peaks 4)、2.523 (peaks 5)、3.097 (peaks 6)、3.251 (peaks 7)、3.336 (peaks 8)、3.460 (peaks 9)、3.575 (peaks 10)、3.854 (peaks 11)、4.858 (peaks 12)，These common characteristic peaks constitute the fingerprint characteristic of Radix Curcumae medical material，Can as the standard finger-print of Radix Curcumae medical material.
(5) similarity evaluation: 10 batches of medical material sample finger printing adopt " similarity evaluation " 2004A version similarity software to be evaluated, and result shows that test sample fingerprint similarity is all higher than 0.90.
(6) hierarchial-cluster analysis: by 12 total peak-to-peak area standardization composition 10 × 12 rank raw data matrixs in the Radix Curcumae HPLC collection of illustrative plates of separate sources, use SPSS19.0 software, attached method between employing group, utilize Euclidean distance for estimating, carry out hierarchial-cluster analysis, 10 batches of medical materials from different sources are divided into 3 classes.
Advantages of the present invention and having the beneficial effect that
1. the test sample preparation that preparation method of the present invention adopts is simple, and chromatographic condition is easily achieved；Quickly, accurately, precision, repeatability and having good stability, chromatographic peak abundant information and separating degree are good, and the finger printing set up can characterize the quality of Radix Curcumae medical material effectively for the method.
2. Radix Curcumae medical material is made as a whole treating by the present invention, can find out the nuance between different medical material by comparing its total peak, it is adaptable to discriminating and the control to the Radix Curcumae medical material true and false, the place of production and quality.
Accompanying drawing explanation
Fig. 1,10 batches of Radix Curcumae HPLC-FPSs
Fig. 2, Radix Curcumae medical material standard finger-print
Fig. 3,10 batches of Radix Curcumae medicinal materials fingerprint cluster analyses
Detailed description of the invention
Embodiment 1: the method for Radix Curcumae HPLC-FPS is set up and checking
1. instrument and material
1.1 instruments: wear peace P680 type high performance liquid chromatograph, including P680 type infusion pump, ASI-100 automatic sampler, column oven and UV-detector, chromeleon chromatographic work station.BK-240A type ultrasonic washing unit (Bark ultrasound wave science and technology Group Co., Ltd), BP211 type electronic analytical balance (Germany Sai Duolisi).
1.2 reference substances and reagent: curdione reference substance (Chengdu Puffy moral Bioisystech Co., Ltd, lot number 130713), curcumadiol reference substance, procurcumenol reference substance are self-control, and all reference substance purity are all higher than 98%.Acetonitrile (Fisher chemical reagents corporation of the U.S., chromatographically pure), phosphoric acid (Tianjin Concord Technology Co., Ltd.'s analytical pure), methanol (Tianjin Concord Technology Co., Ltd., analytical pure), water is pure water (limit company of Hangzhou WAHAHA group).
1.3 medical materials: Radix Curcumae medical material totally 10 batches, are designated as S1-S10 respectively, and wherein S1, S6 are from Hengxian County, and S2, S4, S7 are from Guilin, and S3, S8, S9, S10 are from Huanggang, and S5 is new field from Hunan.
2. high performance liquid chromatography
2.1 chromatographic conditions: AgelaPromosilC18Chromatographic column；Acetonitrile-oxolane (10:1) (A)-0.1% phosphoric acid water (B) gradient elution；Flow velocity 1.0mL min-1；Detection wavelength 250nm；Column temperature 30 DEG C；Sample size 20 μ L.
Mobile phase elution program such as table 1:
Table 1 mobile phase elution program
The preparation of 2.2 reference substance solution: precision weighs curdione, curcumadiol, procurcumenol in right amount, adds methanol respectively and makes 0.1990mg mL-1Curdione reference substance solution, 0.0152mg mL-1Curcumadiol reference substance solution 0.0295mg mL-1The reference substance solution of procurcumenol reference substance solution.
The preparation of 2.3 need testing solutions: take Radix Curcumae medicinal powder and be about 0.5g, accurately weighed, put in tool plug conical flask, accurate addition methanol 25mL, close plug, weighed quality, supersound extraction 30min, let cool, weighed weight again, supplies the weight of less loss, shakes up with methanol, filter, take subsequent filtrate and filter with 0.45 μm of microporous filter membrane and get final product.
3. Method validation
3.1 precision tests: taking Radix Curcumae (S1) need testing solution, continuous sample introduction 6 times, relative retention time and relative peak area to total peak are investigated respectively.It is shown that the equal < 1.5% of the RSD of the relative retention time at each total peak, the equal < 3.4% of RSD of relative peak area.Show that the method precision is good.
3.2 replica tests: take 6 parts of Radix Curcumae (S1) medical material sample, need testing solution is prepared by 2.3 lower method operations, sample introduction is analyzed, record the equal < 1.8% of RSD of the relative retention time at each total peak, the equal < 3.8% of RSD of relative peak area.Show that the method repeatability is good.
3.3 stability tests: take Radix Curcumae (S1) need testing solution, be analyzed respectively at 0,2,4,6,12,24h, investigate relative retention time and the relative peak area at its total peak.It is shown that the equal < 1.6% of the RSD of the relative retention time at each total peak, the equal < 3.5% of RSD of relative peak area, it was shown that need testing solution is basicly stable in 24h.
4. measure: the accurate need testing solution 20 μ Ls each with reference substance solution that draw inject high performance liquid chromatograph, according to high effective liquid chromatography for measuring, obtain finger printing.
Embodiment 2:10 criticizes detection and the data analysis of Radix Curcumae medicinal materials fingerprint
1.1 Radix Curcumae medicinal materials fingerprints measure: take 10 batches of Radix Curcumae medical materials, are measured by embodiment 1 condition, obtain the HPLC collection of illustrative plates of 10 batch samples.Using No. 1 peak (curcumadiol) as reference, it is determined that 12 total peaks, such as Fig. 1.Relative retention time and relative peak area to each total peak are calculated, the wherein equal < 0.15% of RSD of each total peak relative retention time, but the RSD of each relative peak area is all relatively big, illustrating that the medicinal ingredient content difference of different sources is relatively big, result is in Table 2～3.
The relative retention time of 210 batches of HPLC-FPSs of table
The relative peak area of 310 batches of HPLC-FPSs of table
1.2 similarity evaluations: 10 batches of Radix Curcumae medical material chromatograms are imported " similarity evaluation " 2004A version similarity software, adopt averaging method Auto-matching to generate comparison collection of illustrative plates R, such as Fig. 2.L0 batch sample and reference fingerprint similarity are between 0.943～0.995, and prompting quality of medicinal material is relatively stable, and result is in Table 4.
410 batches of Radix Curcumae medicinal materials fingerprint similarity evaluations of table
1.3 cluster analyses: by 12 total peak-to-peak area standardization composition 10 × 12 rank raw data matrixs in the Radix Curcumae HPLC collection of illustrative plates of separate sources, use SPSS19.0 software, attached method between employing group, utilize Euclidean distance for estimating, carry out hierarchial-cluster analysis, see Fig. 3.According to cluster analysis result, can being divided three classes by 10 batches of Radix Curcumae medical materials, wherein S2, S3, S4, S6, S8, S9, S10 gather for I class, and S5, S7 gather for II class, and S1 is Group III.
Similarity evaluation is it is shown that 10 batches of medical material similarities are all higher than 0.9, it was shown that the Radix Curcumae quality of medicinal material of different sources is more stable, but from relative peak area ratio, medicinal ingredient content difference is bigger.Adopt cluster analysis that the Radix Curcumae medical material of separate sources is divided into 3 classes, find that classification results does not fit like a glove with place of production distribution, there is some difference in conjunction with similarity evaluation result, the quality of the different Radix Curcumae medical material in source to be described, be likely to also with the plantation of medical material, gather relevant with the factor such as storage, need to investigate further.
Claims (9)
1. the method for building up of a Radix Curcumae medicinal materials fingerprint, it is characterised in that adopt HPLC method, comprise the steps:
(1) preparation of reference substance solution: precision weighs curdione, curcumadiol, procurcumenol reference substance, respectively with methanol be configured to every 1mL containing curdione 0.1～0.2mg, curcumadiol 0.01～0.02mg, procurcumenol 0.02～0.04mg solution, as reference substance solution；
(2) preparation of need testing solution: precision weighs Radix Curcumae medicinal material coarse powder, adds methanol supersound extraction 30～60min, filters, takes subsequent filtrate as need testing solution；
(3) chromatographic condition: chromatographic column, with octadecylsilane chemically bonded silica for filler, adopts gradient elution, mobile phase is the gradient eluent of acetonitrile-oxolane-0.1% phosphoric acid water system composition, ultraviolet detection: wavelength is 230～250nm；
(4) measure: accurate need testing solution 10～20 μ L of absorption injects high performance liquid chromatograph, according to high effective liquid chromatography for measuring, obtains finger printing.
2. the method for building up of Radix Curcumae HPLC-FPS according to claim 1, it is characterised in that: described in step (1), the concentration of curdione reference substance solution is 0.1990mg mL-1, curcumadiol reference substance solution concentration be 0.0152mg mL-1, procurcumenol reference substance solution concentration be 0.0295mg mL-1。
3. the method for building up of Radix Curcumae HPLC-FPS according to claim 1, it is characterised in that: Radix Curcumae medicinal material coarse powder described in step (2) crosses 40 mesh sieves, and Radix Curcumae medical material weighs as about 0.5g.
4. the method for building up of Radix Curcumae HPLC-FPS according to claim 1, it is characterised in that: extraction step described in step (2) is for adopting methanol supersound extraction, and extraction time is 30min.
5. the method for building up of Radix Curcumae HPLC-FPS according to claim 1, it is characterised in that: the gradient eluent that mobile phase is acetonitrile-oxolane-0.1% phosphoric acid water system of gradient elution described in step (3)；Elution time is 65min；Flow velocity 1.0mL min-1；Column temperature: 30 DEG C.
6. the method for building up of Radix Curcumae medicinal materials fingerprint according to claim 1, it is characterised in that:
Gradient elution described in described step (3) chromatographic condition, gradient elution program carries out with the configuration of following volumetric concentration: when 0 minute, 0.1% phosphate aqueous solution that acetonitrile-oxolane (10:1) that mobile phase A is 15%, Mobile phase B are 85%；When 50 minutes, 0.1% phosphate aqueous solution that acetonitrile-oxolane (10:1) that mobile phase A is 85%, Mobile phase B are 15%；50.1 minute time, 0.1% phosphate aqueous solution that acetonitrile-oxolane (10:1) that mobile phase A is 15%, Mobile phase B are 85%；When 65 minutes, 0.1% phosphate aqueous solution that acetonitrile-oxolane (10:1) that mobile phase A is 15%, Mobile phase B are 85%.
7. the method for building up of Radix Curcumae HPLC-FPS according to claim 1, it is characterised in that: in measuring described in step (4), HPLC automatic sampler sample introduction 20 μ L.
8. the method for building up of the Radix Curcumae HPLC-FPS according to claim 1-7, it is characterized in that: have 12 features to have peak in described finger printing, wherein No. 1 peak is curcumadiol reference peak, and No. 5 peaks are procurcumenol, No. 11 peaks are curdione, specific as follows:
No. 1 peak, Average residence time is 9.73min, and peak area is 875.686；
No. 2 peaks, Average residence time is 13.71min, and peak area is 403.140；
No. 3 peaks, Average residence time is 14.54min, and peak area is 336.420；
No. 4 peaks, Average residence time is 15.52min, and peak area is 118.226；
No. 5 peaks, Average residence time is 24.54min, and peak area is 264.982；
No. 6 peaks, Average residence time is 30.12min, and peak area is 104.990；
No. 7 peaks, Average residence time is 31.62min, and peak area is 2344.064；
No. 8 peaks, Average residence time is 32.45min, and peak area is 926.635；
No. 9 peaks, Average residence time is 33.65min, and peak area is 166.430；
No. 10 peaks, Average residence time is 34.76min, and peak area is 172.176；
No. 11 peaks, Average residence time is 37.48min, and peak area is 415.697；
No. 12 peaks, Average residence time is 47.25min, and peak area is 288.828.
9. the finger printing that the method according to any one of claim 1 to 7 prepares application in Radix Curcumae medical material and Radix Curcumae medicinal substances extract and preparation detection.
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| CN108459089A (en) * | 2017-02-17 | 2018-08-28 | 中国中医科学院中药研究所 | A method of Radix Curcumae secondary metabolite is measured using HPLC-DAD-MS |
| CN108562662A (en) * | 2017-02-17 | 2018-09-21 | 中国中医科学院中药研究所 | A method of Radix Curcumae Contained Serum is measured using Thermo UPLC-ITQ-Orbitrap high resolution mass spectrums |
| CN108562661A (en) * | 2017-02-17 | 2018-09-21 | 中国中医科学院中药研究所 | A method of turmeric Contained Serum is measured using Thermo UPLC-ITQ-Orbitrap high resolution mass spectrums |
| CN107091893B (en) * | 2017-05-26 | 2019-06-11 | 浙江中医药大学 | The measuring method of multi-target ingredient content in a kind of XINGNAOJING ZHUSHEYE or in which mesosome |
| CN107091893A (en) * | 2017-05-26 | 2017-08-25 | 浙江中医药大学 | The assay method of multi-target ingredient content in a kind of XINGNAOJING ZHUSHEYE or its intermediate |
| CN108717088B (en) * | 2018-05-25 | 2021-10-26 | 无锡济煜山禾药业股份有限公司 | Method for evaluating volatile components of radix curcumae medicinal material by one test and multiple tests |
| CN108717088A (en) * | 2018-05-25 | 2018-10-30 | 无锡济民可信山禾药业股份有限公司 | A kind of Radix Curcumae medicinal material volatile ingredient one is surveyed comments assay method more |
| CN110082446A (en) * | 2019-05-08 | 2019-08-02 | 陕西中医药大学 | A kind of turmeric quality determining method |
| CN113759007A (en) * | 2020-08-25 | 2021-12-07 | 北京康仁堂药业有限公司 | Quality control method of curcuma kwangsiensis |
| CN113759006A (en) * | 2020-08-25 | 2021-12-07 | 北京康仁堂药业有限公司 | Quality control method of radix curcumae longae formula granules |
| CN113759006B (en) * | 2020-08-25 | 2023-03-21 | 北京康仁堂药业有限公司 | Quality control method of radix curcumae longae formula granules |
| CN113759007B (en) * | 2020-08-25 | 2023-03-21 | 北京康仁堂药业有限公司 | Quality control method of curcuma kwangsiensis |
| CN114689745A (en) * | 2022-03-22 | 2022-07-01 | 广东一方制药有限公司 | Fingerprint construction method and identification method of curcuma aromatica or curcuma zedoaria |
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