CN102028883A - Standard fingerprint spectrum of Chinese medicinal composition, and measurement method and application thereof - Google Patents
Standard fingerprint spectrum of Chinese medicinal composition, and measurement method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of analysis of traditional Chinese medicines, and discloses a standard fingerprint spectrum of a Chinese medicinal composition, and a measurement method and application thereof. The standard fingerprint spectrum is a high performance liquid chromatography spectrum; six main chromatographic peaks are shown in the spectrum; the No. 3 peak is the chromatographic peak which has the same peak retention time as ferulic acid serving as a reference object; and compared with the No. 3 peak, the other five chromatographic peaks have the relative retention time of 0.23+/-10 percent, 0.27+/-10 percent, 1.20+/-8 percent, 1.65+/-10 percent and 1.80+/-10 percent respectively. The standard fingerprint spectrum can be used for quality control over the Chinese medicinal composition comprising szechuan lovage rhizome and tall gastrodia tuber serving as raw medicinal materials; and the similarity of the fingerprint spectrum of a qualified Chinese medicinal composition to the standard fingerprint spectrum is not less than 0.80. The standard fingerprint spectrum can completely and effectively control the product quality; a similarity evaluation system is adopted; and the invention has the advantages of convenience and high speed in operation and objective and accurate result.
Description
Technical field
The invention belongs to the Chinese medicine analysis field, relate to the standard finger-print of Chinese medicinal composition preparation, the invention still further relates to the assay method and the application of this standard finger-print in the control of this composition quality of this standard finger-print.
Background technology
The Chinese medicine composition that the present invention relates to is after being made up according to a certain percentage by Rhizoma Chuanxiong, Rhizoma Gastrodiae two flavor medicines, the Chinese medicine preparation that adopts water extraction and alcohol extraction process combined to be prepared into, effect with the suppressing the hyperactive liver of invigorating blood circulation, removing obstruction in the collateral to relieve pain, headache due to obstruction of collaterals by blood stasis or the excessive rising of liver-YANG with the passing of time, localized pain, or have that dizzy hypochondriac pain, insomnia are irritated concurrently, dark tongue quality or ecchymosis is arranged; Angioneurotic headache.In order more comprehensively, effectively to control the quality control level of this Chinese medicine composition, and international joint, allow clinical drug safety and curative effect guarantee more to some extent, need adopt more advanced quality control method to this Chinese medicine composition.
Because Chinese medicine and preparation thereof are the multi-component complex system, therefore estimating its quality should adopt and adapt with it, can provide the detection method of enriching authentication information, but methods such as existing microscopical identification, physicochemical identification and assay are not enough to all address this problem.Chinese medicine fingerprint is meant that some Chinese crude drug or Chinese medicine preparation after suitably handling, adopt certain analysis means, the chromatogram that can indicate its chemical feature or the spectrogram that obtain.Chinese medicine fingerprint is a kind of comprehensive, and quantifiable identification of means can reflect the kind and the quantity of contained chemical constituent in Chinese medicine and the preparation thereof comparatively all sidedly, and then drug quality be carried out integral body describe and estimate.So Chinese medicine fingerprint has become comparatively advanced in the world at present Chinese medicine quality control device.This Chinese medicine composition is not also openly reported as the finger printing of quality control standard.
All point out in FDA (Food and Drug Adminstration) (FDA) plant amedica product industrial directory, the WHO medical herbs evaluation guide, if the active component of herbal medicinal product can not differentiate, can pass through the unanimity that finger printing (fingerprint spectrum) proves product quality.The European Community also points out in medical herbs quality guideline note, medical herbs and preparation thereof be with integral body as active substance, therefore, the quality stability of medical herbs only depends on and measures known effective ingredient is not enough, should show the various compositions that it is contained by finger printing.India herbal medicine allusion quotation, British Herbal Pharmacopoeia, German medicinal plants association, Canada is medicinal and fragrant plant association etc., also accepts to guarantee with finger printing the concordance of the herbal products quality that effective ingredient is not bright.National Drug Administration has required to have relevant finger printing to Chinese medicine at present, the quality that improves Chinese medicine has been played pivotal role, but the Chinese medicine of other dosage forms is not still had Compulsory Feature.
Chinese medicine fingerprint comprises Chemistry for Chinese Traditional Medicine finger printing, protein fingerprint spectrum, dna fingerprinting and biological effect finger printing etc.Usually the finger printing of saying is meant chemical fingerprint, be Chinese crude drug, Chinese medicine extract or Chinese patent medicine after suitable processing, adopt certain analysis means, the chromatograph or the spectrum that can indicate this Chinese medicine main chemical compositions characteristic that obtain.
The Chemistry for Chinese Traditional Medicine finger printing can be divided into Chinese medicine spectral fingerprint collection of illustrative plates, as infrared spectrum (IR), ultraviolet spectra (UV), X ray diffracting spectrum etc.; Chromatographic fingerprinting is as thin layer chromatography (TLC), gas chromatogram (GC), high performance liquid chromatography (HPLC), capillary electrophoresis collection of illustrative plates (CE) etc.; The wave spectrum finger printing is as mass spectrum (MS), NMR (Nuclear Magnetic Resonance) spectrum (NMR) etc.; Dna fingerprinting; And the multidimensional that adopts the coupling of various modern analytical tool to obtain ceases characteristic spectrum (characteristic fingerprint of muhrdimension andmuhrdats) more, as HPLC/MS, HPLC/Ms/MS, GC/MS, CE/MS etc.
Though the Chinese medicine fingerprint research method is more, but the chromatography method should be main stream approach, especially TLC, HPLC and GC chromatographic technique, having become the analysis means of everybody confessed three kinds of routines, is to study Chinese medicine fingerprint at present to answer top-priority method.
Chinese medicine fingerprint has two effects: the one, by the characteristic of finger printing, can effectively differentiate the true and false or the place of production of Chinese crude drug: the 2nd, by the area at finger printing principal character peak or the formulation of ratio, can effectively control the quality of product, guarantee the consistent relatively of product quality.
The making and the application of Chinese medicine fingerprint generally include: (1) gathers representative Chinese medicine sample, takes suitable method to prepare need testing solution, and selects suitable standard standard substance (object of reference) for use, carries out the preferred of analytical method; (2) according to the analytical method of determining, certain batch Chinese medicine sample is carried out compartment analysis, the multiple batches of data of gained are handled, obtain standard finger-print; (3) with sample according to making after identical method carries out sample treatment, compartment analysis with standard finger-print, the finger printing collection of illustrative plates and the standard finger-print of gained carried out similarity relatively, generally to reach and promptly can be considered this sample more than 80% be qualified to similarity.Calculation of similarity degree and evaluation methodology are adopted correlation coefficient usually and are harmonious coefficient or included angle cosine method.Unit roots such as China Central South University, Zhejiang University go up method according to this, have worked out correspondent computer software and have been used to finish similarity evaluation, and wherein " the chromatographic fingerprints of Chinese materia medica similarity evaluation system " recommended with Chinese Pharmacopoeia Commission uses more.
Summary of the invention
The purpose of this invention is to provide standard finger-print as a kind of Chinese medicine composition of quality control standard.
Another object of the present invention provides the assay method of this Chinese medicine composition standard finger-print.
A further object of the invention provides the application of this Chinese medicine composition standard finger-print in the Chinese medicine preparation quality control.
The objective of the invention is to realize by following measures:
The Chinese medicine composition standard finger-print that the present invention relates to, this finger printing is the high-efficient liquid phase chromatogram spectrum, present 6 main chromatographic peaks in this collection of illustrative plates, wherein No. 3 peaks are chromatographic peaks identical with the peak retention time of object of reference ferulic acid, compare with No. 3 peak retention times (by 1), the relative retention time of other 5 chromatographic peaks is respectively: 1.65 ± 10%, No. 6 peaks 1.80 ± 10%, 1.20 ± 8%, No. 5 peaks, 0.27 ± 10%, No. 4 peaks, 0.23 ± 10%, No. 2 peaks, No. 1 peak.
Above-mentioned standard finger-print, it is characterized in that described Chinese medicine composition prepares by following method: get Rhizoma Chuanxiong 784g, Rhizoma Gastrodiae 196g, pulverize, mix, with 90% alcohol reflux secondary, each 2 hours, merge extractive liquid, filters, filtrate recycling ethanol and to be condensed into relative density be 1.27～1.28 clear paste I; Medicinal residues decoct with water secondary, and each 1 hour, collecting decoction filtered, and it is 1.27～1.28 clear paste II that filtrate is condensed into relative density, merges above-mentioned clear paste I and clear paste II, and the adding appropriate amount of auxiliary materials is made required Chinese medicine preparation.This Chinese medicine preparation includes but are not limited to the liquid preparation of the solid preparation of capsule, soft capsule, tablet, pill, drop pill, granule and oral liquid, injection.
The assay method of described Chinese medicine composition product standard finger printing, this method adopts high performance liquid chromatography, and its chromatographic condition is:
Chromatographic column adopting octadecylsilane chemically bonded silica chromatographic column;
Mobile phase is 0.1% phosphoric acid-methanol aqueous solution system,, wherein mobile phase A is 0.1% phosphoric acid solution, Mobile phase B is a methanol, adopts gradient elution;
Flow velocity is 1mL/min;
Column temperature is 30 ℃;
Detector adopts UV-detector, and the detection wavelength is 276nm;
Number of theoretical plate is pressed object of reference ferulic acid peak and is calculated, and should be not less than 6000.
It is that 25～100% methanol is made solvent that the assay method of described Chinese medicine composition standard finger-print, the solution that wherein is used for high-performance liquid chromatogram determination adopt concentration.
The assay method of described Chinese medicine composition standard finger-print, the need testing solution that wherein is used for high-performance liquid chromatogram determination adopts 50% methanol to make solvent, and object of reference solution adopts 50% methanol to make solvent.
The assay method of described Chinese medicine composition standard finger-print, wherein the preparation of object of reference solution is that to get ferulic acid an amount of, accurately claims surely, adds 50% methanol and makes the solution that every 1mL contains 20 μ g, promptly.
The assay method of described standard finger-print, the preparation process of need testing solution is as follows:
This composition capsule, tablet, pill, drop pill, granule: get this Chinese medicine composition content, mixing, porphyrize is got about 1g, puts in the conical flask, the accurate 50% methanol 25mL that adds, ultrasonic 30min filters, and gets subsequent filtrate as need testing solution, promptly;
This composition soft: get this Chinese medicine composition content, mixing is got about 1g, puts in the conical flask, the accurate 75% methanol 30mL that adds, and ultrasonic 30min filters, and gets subsequent filtrate as need testing solution, promptly;
This composition oral liquid: get this Chinese medicine composition, mixing is got about 10mL, to flask, and the accurate 95% methanol 50mL that adds, reflux, extract, 30min filters, and gets subsequent filtrate as need testing solution, promptly.
This composite injection: get the about 10mL of injection, to flask, add 95% methanol 50mL, fully stir, filter, get subsequent filtrate as need testing solution, promptly.
The assay method of described standard finger-print, wherein gradient elution is in proper order:
The assay method of described standard finger-print, wherein sample size is 2 μ L～50 μ L.
The application of described standard finger-print in this Chinese medicine composition quality control.
Adopt above-mentioned finger printing to sample detection, the standard of qualified products is: the finger printing of qualified Chinese medicine composition and the similarity of standard finger-print are not less than 0.80.The method of comparative sample finger printing and standard finger-print similarity is to adopt included angle cosine method or correlation coefficient process, and it adopts correspondent computer software is the chromatographic fingerprints of Chinese materia medica similarity evaluation system of Chinese Pharmacopoeia Commission's regulation.
If no special instructions, capsule of the present invention is meant the hard capsule in an appendix IL of Pharmacopoeia of People's Republic of China version in 2005 capsule.
Beneficial effect of the present invention:
1, the present invention has set up the standard finger-print under the 276nm wavelength, the quality information that can comprehensively reflect this compositions need not more more complicated collection of illustrative plates or more complicated quality control index and just can reach the purpose of controlling this composite preparation product quality fully and effectively.
2, to the identification of survey finger printing, the chromatographic fingerprints of Chinese materia medica similarity evaluation system that adopts Chinese Pharmacopoeia Commission to provide, easy to operate, quick; And, with this similarity result that draws preparation finger to be estimated, conclusion is comparatively objective, accurate.
The present invention is with reference to the requirement of Chinese medicine finger printing, the Chinese medicine composition finger printing that the present invention relates to is studied, process is to the investigation of test sample preparation method and the instrument of mensuration finger printing, chromatographic column, mobile phase, conditions such as detection wavelength are carried out the preferred of system, set up the determining fingerprint pattern condition and carried out methodological study, on basis to many batches of this Chinese medicine composition finger printing testing results, accumulation data gradually, standard finger-print has been proposed, as this product finger printing standard, thereby be able to more comprehensively, control the purpose of the quality of the pharmaceutical preparations effectively.
Identification to measured finger printing, the present invention adopts Chinese Pharmacopoeia Commission to provide chromatographic fingerprints of Chinese materia medica similarity evaluation system as this Chinese medicine composition finger printing similarity software for calculation, through test of many times research, and by comparing with the method for calculating relative retention time and relative peak area, the evaluation conclusion basically identical that is drawn, use the similarity of chromatographic fingerprints of Chinese materia medica similarity evaluation system evaluation finger printing, easy to operate, fast, with its similarity result that draws, preparation finger is estimated, and conclusion is comparatively objective, accurately.
Research and explanation to finger print measuring method of the present invention:
Capsule with Chinese medicine composition of the present invention is an example, and the detection method of finger printing of the present invention is carried out methodological study:
1. the selection of object of reference solution
Select ferulic acid as object of reference.
2. the preparation of need testing solution
Through the experiment screening comparative analysis, determine that this Chinese medicine composition determining fingerprint pattern test sample preparation method is:
This composition capsule: get this Chinese medicine composition content under the content uniformity item, mixing, porphyrize is got about 1g, puts in the conical flask, the accurate 50% methanol 25mL that adds, ultrasonic 30min filters, and gets subsequent filtrate as need testing solution, promptly;
3. detection method
Instrument and reagent:
Instrument: Agilent 1100 liquid chromatograph; MWD multi-wavelength ultraviolet-visible detector, the full-automatic injector of G1313A, Agilent LC chromatographic work station.
Chromatographic column: C
18, 4.6 * 250mm, 5 μ m; Mobile phase A is 0.1% phosphoric acid solution, and Mobile phase B is a methanol, carries out gradient elution;
Eluting order is:
Flow velocity is 1mL/min; The detection wavelength is 276nm, and number of theoretical plate is pressed object of reference (ferulic acid) peak and calculated, and should be not less than 6000.
Reagent: methanol is chromatographically pure (Tedia company), and water is ultra-pure water, and all the other reagent are analytical pure.
Measure wavelength: in order more fully to reflect the composition in the preparation, compare analysis through adopting a plurality of wavelength to measure finger printing, determine that 276nm is the detection wavelength of preparation finger, in the preparation finger under this wavelength, other composition fingerprint peaks also can be embodied preferably, and each peak separating degree is good, and baseline is steady, good reproducibility.See Fig. 1, Fig. 2.
4. stability test
Get this Chinese medicinal composition capsules finished product, prepare need testing solution, measure once its finger printing at set intervals, the results are shown in Table 1, show the need testing solution stable components by the preparation method of need testing solution among the embodiment 1.
Table 1 lot number is 060712 Chinese medicinal composition capsules finished product stability similarity (wavelength 276nm)
| Time | Similarity (reference) |
| 0h | 1.000 |
| 3h | 0.998 |
| 6h | 0.997 |
| 9h | 0.998 |
| 12h | 0.998 |
| 15h | 0.997 |
5. precision test
Get this Chinese medicinal composition capsules finished product, prepare need testing solution by the preparation method of need testing solution, continuous sample introduction is measured.Measurement result sees Table 2.Calculate the similarity of back 5 sample introduction gained finger printing with the 1st sample introduction gained finger printing as contrast again, measurement result sees Table 3, shows that this method precision is good.
Table 2 lot number is 060712 Chinese medicinal composition capsules finished product finger printing precision investigation result (wavelength 276nm)
(accounting for the retention time of total peak area 5% above main peaks)
Table 3 lot number is 060712 Chinese medicinal composition capsules finished product precision similarity (wavelength 276nm)
| The sample introduction number of times | Similarity (reference) |
| 1 | 1.000 |
| 2 | 0.998 |
| 3 | 0.999 |
| 4 | 0.997 |
| 5 | 0.998 |
| 6 | 0.998 |
6. replica test
Get this Chinese medicine composition of lot number, prepare need testing solution by the preparation method of need testing solution among the embodiment 1, be equipped with need testing solution with legal system, measure in accordance with the law, measurement result sees Table 4, and the result calculates similarity, meets the specification requirement of finger printing.
Table 4 lot number is 060712 Chinese medicinal composition capsules finished product repeatability similarity (wavelength 276nm)
| Sample number into spectrum | Similarity (reference) |
| 1 | 1.000 |
| 2 | 0.997 |
| 3 | 0.998 |
| 4 | 0.998 |
| 5 | 0.997 |
| 6 | 0.999 |
According to above methodological study result, show that this method measures the finger printing of this Chinese medicine composition, precision, repeatability, stability are all better, can accurately measure the finger printing of this compositions.
7. the mensuration of finger printing manufactures a finished product greatly
Get this Chinese medicinal composition capsules finished product respectively, measure according to the fingerprint atlas detection method that the invention described above provides, measurement result sees Table 5, gained finished product finger printing calculates with similarity software with standard finger-print respectively, and similarity meets the regulation of this Chinese medicine composition finished product finger printing as a result.Analysis result shows that concordance is preferably arranged between different batches.
10 batches of present composition capsule finished products of table 5 similarity (wavelength 276nm)
| Lot number | Similarity (standard) |
| 060712 | 0.977 |
| 060806 | 0.978 |
| 060819 | 0.975 |
| 060902 | 0.977 |
| 060916 | 0.979 |
| 060930 | 0.982 |
| 061012 | 0.975 |
| 061025 | 0.978 |
| 061116 | 0.978 |
| 061209 | 0.982 |
Description of drawings
Fig. 1: the Chinese medicine composition liquid-phase fingerprint is measured the selection of wavelength.
Fig. 2: the finger printing HPLC-UV 3D figure of Chinese medicine composition.
Fig. 3: Chinese medicine composition standard finger-print (the detection wavelength is 276nm).
The specific embodiment
The invention will be further elaborated by the following examples.
Embodiment 1: determining fingerprint pattern
The preparation method of capsule is as follows:
Prescription: Rhizoma Chuanxiong 784g Rhizoma Gastrodiae 196g
Method for making: above two flavors, pulverize, mix, with 90% alcohol reflux secondary, each 2 hours, merge extractive liquid,, filtration, filtrate recycling ethanol and to be condensed into relative density be 1.27～1.28 clear paste I; Medicinal residues decoct with water secondary, and each 1 hour, collecting decoction filtered, and it is 1.27～1.28 clear paste II that filtrate is condensed into relative density, merge above-mentioned clear paste I and clear paste II, add an amount of silicon dioxide, vacuum drying is pulverized, sieve, incapsulate, make 1000, promptly.Specification: every dress 0.34g
Finger printing detects:
Get this product content, mixing, porphyrize, get about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate 50% methanol 25ml that adds claims to decide weight, supersound process (power 250W, frequency 40kHz) 30 minutes, put coldly, claim to decide weight again, supply the weight that subtracts mistake with 50% methanol, shake up, filter, get subsequent filtrate, as need testing solution.It is an amount of that other gets the ferulic acid reference substance, and accurate the title decides, and adds 50% methanol and makes the solution that every 1ml contains 20 μ g, in contrast product solution.
Measure instrument: Agilent 1100 liquid chromatograph according to high performance liquid chromatography (2005 editions appendix VID of Chinese Pharmacopoeia); MWD multi-wavelength ultraviolet-visible detector; Reagent: methanol is chromatographically pure (Tedia company), and water is ultra-pure water, and all the other reagent are analytical pure.With the octadecylsilane chemically bonded silica is filler, phenomenex Luna C
18Chromatographic column (column length is 250mm, and column internal diameter is 4.6mm, granularity 5 μ m); As mobile phase A, methanol is Mobile phase B with 0.1% phosphoric acid solution, and according to the form below carries out gradient elution; Flow velocity is per minute 1ml; The detection wavelength is 276nm; Column temperature is 30 ℃.Number of theoretical plate calculates by the ferulic acid peak should be not less than 6000.
Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, write down the chromatogram in 55 minutes.
Should present 6 main chromatographic peaks in the test sample chromatograph, the chromatographic peak identical with reference substance peak retention time is No. 3 peaks, compare with No. 3 peak retention times, the relative retention time of other 5 chromatographic peaks is respectively: 1.65, No. 6 peaks 1.80,1.20, No. 5 peaks, 0.27, No. 4 peaks, 0.23, No. 2 peaks, No. 1 peak.
The similarity software for calculation is the chromatographic fingerprints of Chinese materia medica similarity evaluation system of Chinese Pharmacopoeia Commission regulation, after measured, with the similarity of standard finger-print be 0.95.
Embodiment 2: the acquisition of standard finger-print.
10 batches of this Chinese medicinal composition capsules finished products, preparation method by need testing solution prepares need testing solution, measure (the detection wavelength is 276nm) according to embodiment 1 method, the result calculates similarity, the results are shown in Table 6, with serving as that the basis obtains " common pattern " as standard finger-print with these 10 batches of test sample finger printing in the similarity software, the results are shown in Figure 3.
Ten batches of similarities of this composition capsule of table 6 finished product (wavelength 276nm)
| Lot number | Similarity (standard) |
| 060712 | 0.977 |
| 060806 | 0.978 |
| 060819 | 0.975 |
| 060902 | 0.977 |
| 060916 | 0.979 |
| 060930 | 0.982 |
| 061012 | 0.975 |
| 061025 | 0.978 |
| 061116 | 0.978 |
| 061209 | 0.982 |
Embodiment 3: the determining of control of product quality standard
Adopt the chromatographic fingerprints of Chinese materia medica similarity evaluation system of Chinese Pharmacopoeia Commission's regulation, version is 2004 editions.
The principal character of the finger printing of control of product quality standard:
Present 6 main chromatographic peaks in this collection of illustrative plates, wherein No. 3 peaks are chromatographic peaks identical with the peak retention time of object of reference ferulic acid, compare with No. 3 peak retention times (by 1), the relative retention time of other 5 chromatographic peaks is respectively: 1.65 ± 10%, No. 6 peaks 1.80 ± 10%, 1.20 ± 8%, No. 5 peaks, 0.27 ± 10%, No. 4 peaks, 0.23 ± 10%, No. 2 peaks, No. 1 peak.
Embodiment 4: different auxiliary material and different dosage form are to the influence of product fingerprint collection of illustrative plates.
1, chewable tablet:
Prescription: Rhizoma Chuanxiong 784g Rhizoma Gastrodiae 196g
Method for making: above two flavors, pulverize, mix, with 90% alcohol reflux secondary, each 2 hours, merge extractive liquid,, filtration, filtrate recycling ethanol and to be condensed into relative density be 1.27～1.28 clear paste I; Medicinal residues decoct with water secondary, each 1 hour, collecting decoction, filter, it is 1.27～1.28 clear paste II that filtrate is condensed into relative density, merge above-mentioned clear paste I and clear paste II, add appropriate amount of auxiliary materials (as silicon dioxide, dextrin, starch, phosphate, carbonate, mannitol, sorbitol, sorbic acid or potassium salt, xylitol, maltose, glucose, fructose, dextran, glycine, starch, sucrose, in dilution such as lactose or the mannitol adjuvant one or more) mix, dry, pulverize, obtain fine powder and an amount of binding agent (solid binder such as PEG200, PEG300, PEG400, PEG600, PEG800, PEG1000, PEG1500, the macromolecular material polyvinylpyrrolidone, sodium carboxymethyl cellulose, methylcellulose, low-substituted hydroxypropyl cellulose, hydroxypropyl emthylcellulose, sodium alginate or the like or liquid adhesive such as ethanol, starch slurry, the dextrin slurry waits one or more) mixed granule, add an amount of correctives (as mannitol, sucrose, xylitol, stevioside, maltose alcohol, Mentholum, erythrol, orange peel oil, Oleum Cinnamomi, various essence etc. one or more), lubricant is (as magnesium stearate, Pulvis Talci, sodium stearyl fumarate, magnesium laurylsulfate etc. one or more), disintegrating agent is (as carboxymethyl starch sodium, cross-linking sodium carboxymethyl cellulose, crospolyvinylpyrrolidone, low-substituted hydroxypropyl cellulose, pregelatinized Starch, microcrystalline Cellulose, soybean polysaccharide, alginic acid, handle agar etc. one or more) granulate, total mixing, be pressed into 1000, promptly.
By the detection method of need testing solution preparation method provided by the invention and embodiment 1 above-mentioned preparation is carried out finger printing and detect, and carry out similarity with standard finger-print and calculate, the result is as follows:
No. 3 peaks are chromatographic peaks identical with the peak retention time of object of reference ferulic acid, compare with No. 3 peak retention times (by 1), the relative retention time of other each chromatographic peaks is respectively: 1.75, No. 6 peaks 1.87,1.22, No. 5 peaks, 0.28, No. 4 peaks, 0.24, No. 2 peaks, No. 1 peak.With the similarity of standard finger-print be 0.90.
2, buccal tablet:
Prescription: Rhizoma Chuanxiong 784g Rhizoma Gastrodiae 196g
Method for making: above two flavors, pulverize, mix, with 90% alcohol reflux secondary, each 2 hours, merge extractive liquid,, filtration, filtrate recycling ethanol and to be condensed into relative density be 1.27～1.28 clear paste I; Medicinal residues decoct with water secondary, each 1 hour, collecting decoction, filter, it is 1.27～1.28 clear paste II that filtrate is condensed into relative density, merge above-mentioned clear paste I and clear paste II, add appropriate amount of auxiliary materials (as silicon dioxide, dextrin, starch, phosphate, carbonate, mannitol, sorbitol, sorbic acid or potassium salt, xylitol, maltose, glucose, fructose, dextran, glycine, starch, sucrose, lactose, the dilution adjuvant that mannitol and other pharmaceuticss are commonly used etc. one or more) mix, dry, pulverize, obtain fine powder and an amount of correctives (as mannitol, sucrose, xylitol, stevioside, maltose alcohol, Mentholum, erythrol, orange peel oil, Oleum Cinnamomi, various essence etc. one or more) mix, add an amount of binding agent (solid binder such as PEG200, PEG300, PEG400, PEG600, PEG800, PEG1000, PEG1500, the macromolecular material polyvinylpyrrolidone, sodium carboxymethyl cellulose, methylcellulose, low-substituted hydroxypropyl cellulose, hydroxypropyl emthylcellulose, sodium alginate or the like or liquid adhesive such as ethanol, gelatine size, starch slurry etc. one or more) system granule, add lubricant (as magnesium stearate, Pulvis Talci, sodium stearyl fumarate etc. one or more) granulate, total mixing, be pressed into 1000, promptly.
By the detection method of need testing solution preparation method provided by the invention and embodiment 1 above-mentioned preparation is carried out finger printing and detect, and carry out similarity with standard finger-print and calculate, the result is as follows:
No. 3 peaks are chromatographic peaks identical with the peak retention time of object of reference ferulic acid, compare with No. 3 peak retention times (by 1), the relative retention time of other each chromatographic peaks is respectively: 1.54, No. 6 peaks 1.65,1.28, No. 5 peaks, 0.28, No. 4 peaks, 0.23, No. 2 peaks, No. 1 peak.With the similarity of standard finger-print be 0.90.
3, oral cavity disintegration tablet:
Prescription: Rhizoma Chuanxiong 784g Rhizoma Gastrodiae 196g
Method for making: above two flavors, pulverize, mix, with 90% alcohol reflux secondary, each 2 hours, merge extractive liquid,, filtration, filtrate recycling ethanol and to be condensed into relative density be 1.27～1.28 clear paste I; Medicinal residues decoct with water secondary, each 1 hour, collecting decoction, filter, it is 1.27～1.28 clear paste II that filtrate is condensed into relative density, merge above-mentioned clear paste I and clear paste II, add appropriate amount of auxiliary materials (as silicon dioxide, dextrin, starch, phosphate, carbonate, mannitol, sorbitol, sorbic acid or potassium salt, xylitol, maltose, glucose, fructose, dextran, glycine, starch, sucrose, lactose, the dilution adjuvant that mannitol and other pharmaceuticss are commonly used etc. one or more) mix, dry, pulverize, obtain fine powder and add an amount of correctives (as mannitol, sucrose, xylitol, stevioside, maltose alcohol, Mentholum, erythrol, orange peel oil, Oleum Cinnamomi, various essence etc. one or more), lubricant is (as magnesium stearate, Pulvis Talci, sodium stearyl fumarate, magnesium laurylsulfate etc. one or more), disintegrating agent is (as carboxymethyl starch sodium, cross-linking sodium carboxymethyl cellulose, crospolyvinylpyrrolidone, low-substituted hydroxypropyl cellulose, microcrystalline Cellulose, handle agar etc. one or more) directly be pressed into 1000, promptly.
By the detection method of need testing solution preparation method provided by the invention and embodiment 1 above-mentioned preparation is carried out finger printing and detect, and carry out similarity with standard finger-print and calculate, the result is as follows:
No. 3 peaks are chromatographic peaks identical with the peak retention time of object of reference ferulic acid, compare with No. 3 peak retention times (by 1), the relative retention time of other each chromatographic peaks is respectively: 1.45, No. 6 peaks 1.69,1.16, No. 5 peaks, 0.28, No. 4 peaks, 0.25, No. 2 peaks, No. 1 peak.With the similarity of standard finger-print be 0.90.
4, oral liquid:
Prescription: Rhizoma Chuanxiong 784g Rhizoma Gastrodiae 196g
Method for making: above two flavors, mix, with 90% alcohol reflux secondary, each 2 hours, merge extractive liquid, filtered, and filtrate recycling ethanol also is condensed into the clear paste that relative density is 1.27 (55～60 ℃); Medicinal residues decoct with water secondary, each 1 hour, collecting decoction filters, and filtrate shortens the clear paste that relative density is 1.27 (55～60 ℃) deeply into, merge with above-mentioned clear paste, join in the boiling water heat treatment appropriate time, cold preservation, filter, add the agent of the tender flavor of adjuvant as sucrose, Mel, xylitol, stevioside, maltose alcohol etc. one or more; Antiseptic such as sorbic acid or potassium salt, benzoic acid and propanoic acid etc. one or more; Solubilizing agent such as tween series etc., antioxidant such as sodium sulfite, sodium thiosulfate or the like one or more), filter, 1000mL is made in embedding, sterilization, promptly.
By the detection method of need testing solution preparation method provided by the invention and embodiment 1 above-mentioned preparation is carried out finger printing and detect, and carry out similarity with standard finger-print and calculate, the result is as follows:
No. 3 peaks are chromatographic peaks identical with the peak retention time of object of reference ferulic acid, compare with No. 3 peak retention times (by 1), the relative retention time of other each chromatographic peaks is respectively: 1.55, No. 6 peaks 1.76,1.19, No. 5 peaks, 0.26, No. 4 peaks, 0.22, No. 2 peaks, No. 1 peak.With the similarity of standard finger-print be 0.90.
5, granule:
Prescription: Rhizoma Chuanxiong 784g Rhizoma Gastrodiae 196g
Method for making: above two flavors, pulverize, mix, with 90% alcohol reflux secondary, each 2 hours, merge extractive liquid,, filtration, filtrate recycling ethanol and to be condensed into relative density be 1.27～1.28 clear paste I; Medicinal residues decoct with water secondary, each 1 hour, collecting decoction, filter, it is 1.27～1.28 clear paste II that filtrate is condensed into relative density, merge above-mentioned clear paste I and clear paste II, add appropriate amount of auxiliary materials (as silicon dioxide, dextrin, starch, phosphate, carbonate, mannitol, sorbitol, sorbic acid or potassium salt, xylitol, maltose, glucose, fructose, dextran, glycine, starch, sucrose, lactose, in dilution such as the mannitol adjuvant one or more), dry, pulverize, add suitable bonding (solid binder such as PEG200, PEG300, PEG400, PEG600, PEG800, PEG1000, PEG1500, microcrystalline Cellulose etc. or liquid adhesive such as ethanol, gelatine size, starch slurry, syrup etc. one or more), granulate, granulate is made 1000g, promptly.
By the detection method of need testing solution preparation method provided by the invention and embodiment 1 above-mentioned preparation is carried out finger printing and detect, and carry out similarity with standard finger-print and calculate, the result is as follows:
No. 3 peaks are chromatographic peaks identical with the peak retention time of object of reference ferulic acid, compare with No. 3 peak retention times (by 1), the relative retention time of other each chromatographic peaks is respectively: 1.72, No. 6 peaks 1.86,1.22, No. 5 peaks, 0.26, No. 4 peaks, 0.21, No. 2 peaks, No. 1 peak.With the similarity of standard finger-print be 0.90.
6, soft capsule:
Prescription: Rhizoma Chuanxiong 784g Rhizoma Gastrodiae 196g
Method for making: above two flavors, pulverize, mix, with 90% alcohol reflux secondary, each 2 hours, merge extractive liquid,, filtration, filtrate recycling ethanol and to be condensed into relative density be 1.27～1.28 clear paste I; Medicinal residues decoct with water secondary, each 1 hour, collecting decoction, filter, it is 1.27～1.28 clear paste II that filtrate is condensed into relative density, merge above-mentioned clear paste I and clear paste II, add appropriate amount of auxiliary materials (as silicon dioxide, dextrin, starch, phosphate, carbonate, mannitol, sorbitol, sorbic acid or potassium salt, xylitol, maltose, glucose, fructose, dextran, glycine, starch, sucrose, lactose, in dilution such as the mannitol adjuvant one or more), dry, pulverize, with proper supplementary material (as PEG200, PEG300, PEG400, PEG600, PEG800, PEG1000, PEG1500, and vegetable oil series etc.; Antiseptic such as sorbic acid or potassium salt, benzoic acid and propanoic acid etc.; Solubilizing agent such as tween series wait one or more, antioxidant such as sodium sulfite, sodium thiosulfate etc. one or more) by any way behind the mixing, in incapsulating, make 1000 soft capsules, promptly.
By the detection method of need testing solution preparation method provided by the invention and embodiment 1 above-mentioned preparation is carried out finger printing and detect, and carry out similarity with standard finger-print and calculate, the result is as follows:
No. 3 peaks are chromatographic peaks identical with the peak retention time of object of reference ferulic acid, compare with No. 3 peak retention times (by 1), the relative retention time of other each chromatographic peaks is respectively: 1.55, No. 6 peaks 1.70,1.28, No. 5 peaks, 0.27, No. 4 peaks, 0.22, No. 2 peaks, No. 1 peak.With the similarity of standard finger-print be 0.90.
7, injection:
Prescription: Rhizoma Chuanxiong 784g Rhizoma Gastrodiae 196g
Method for making: above two flavors, pulverize, mix, with 90% alcohol reflux secondary, each 2 hours, merge extractive liquid,, filtration, filtrate recycling ethanol and to be condensed into relative density be 1.27～1.28 clear paste I; Medicinal residues decoct with water secondary, and each 1 hour, collecting decoction filtered, and it is 1.27～1.28 clear paste II that filtrate is condensed into relative density, merges clear paste, mixing, and drying obtains intermediate.Get water for injection 1000ml, boil, add intermediate, cold preservation 48 hours, filter, get filtrate, boiled cold preservation 48 hours 45 minutes, filter, get filtrate, add 0.5% active carbon, boiled 3 minutes, filter, filtrate is got in cold preservation, filtrate is got in ultrafiltration (molecular weight 30000), adds the injection water and supplies 1000ml, embedding, sterilization, promptly.
By the detection method of need testing solution preparation method provided by the invention and embodiment 1 above-mentioned preparation is carried out finger printing and detect, and carry out similarity with standard finger-print and calculate, the result is as follows:
No. 3 peaks are chromatographic peaks identical with the peak retention time of object of reference ferulic acid, compare with No. 3 peak retention times (by 1), the relative retention time of other each chromatographic peaks is respectively: 1.72, No. 6 peaks 1.85,1.18, No. 5 peaks, 0.26, No. 4 peaks, 0.23, No. 2 peaks, No. 1 peak.With the similarity of standard finger-print be 0.90.
8, drop pill:
Prescription: Rhizoma Chuanxiong 784g Rhizoma Gastrodiae 196g
Method for making: above two flavors, pulverize, mix, with 60% alcohol reflux secondary, 1.5 hours for the first time, 6 times of amount ethanol, 1 hour for the second time, 4 times of amount ethanol, merge extractive liquid,, drying under reduced pressure are concentrated into does not have the alcohol flavor, uses the water saturation n-butanol extraction, the extract reclaim under reduced pressure is to relative density 1.30～1.35, drying under reduced pressure with 20 times of water gaging suspendibles, is used absorption with macroporous adsorbent resin to there not being the n-butyl alcohol flavor, wash the deresination post then with water, again with 30% ethanol to the adsorbent resin eluting, collect eluent, concentrate, drying under reduced pressure gets extract powder.With Polyethylene Glycol-4000 and extract powder with 3～6: 1～4 ratio melting mixing, methyl-silicone oil is made coolant, drips to make drop pill, promptly.
By the detection method of need testing solution preparation method provided by the invention and embodiment 1 above-mentioned preparation is carried out finger printing and detect, and carry out similarity with standard finger-print and calculate, the result is as follows:
No. 3 peaks are chromatographic peaks identical with the peak retention time of object of reference ferulic acid, compare with No. 3 peak retention times (by 1), the relative retention time of other each chromatographic peaks is respectively: 1.56, No. 6 peaks 1.78,1.23, No. 5 peaks, 0.28, No. 4 peaks, 0.23, No. 2 peaks, No. 1 peak.With the similarity of standard finger-print be 0.90.
Get this Chinese medicine composition of above employing different dosage form and different auxiliary material, method (the detection wavelength is 276nm) with reference to embodiment 1 detects, its determining fingerprint pattern result all meets the requirement of the finger printing (the detection wavelength is 276nm) of the present invention's regulation, the not influence of finger printing to this Chinese medicine composition of different dosage form and different auxiliary material is described, the finger printing quality control standard of the present invention's regulation (is that described this collection of illustrative plates is the high-efficient liquid phase chromatogram spectrum, present 6 main chromatographic peaks in the collection of illustrative plates, wherein No. 3 peaks are chromatographic peaks identical with the peak retention time of object of reference ferulic acid, compare with No. 3 peak retention times (by 1), the relative retention time of other 5 chromatographic peaks is respectively: No. 1 peak 0.23 ± 10%, No. 2 peaks 0.27 ± 10%, No. 4 peaks 1.20 ± 8%, No. 5 peaks 1.65 ± 10%, No. 6 peaks 1.80 ± 10%) can be used as the standard finger-print quality control standard of this Chinese medicine composition.Adopt finger printing and this Chinese medicine composition standard finger-print calculating similarity of the chromatographic fingerprints of Chinese materia medica similarity evaluation system of Chinese Pharmacopoeia Commission's regulation to this Chinese medicine composition product of above-mentioned different auxiliary material different dosage form, its result is all greater than 0.80.
Claims (12)
1. the standard finger-print of a Chinese medicine composition, it is characterized in that this finger printing is the high-efficient liquid phase chromatogram spectrum, present 6 main chromatographic peaks in this collection of illustrative plates, wherein No. 3 peaks are chromatographic peaks identical with the peak retention time of object of reference ferulic acid, compare with No. 3 peak retention times, the relative retention time of other 5 chromatographic peaks is respectively: 1.65 ± 10%, No. 6 peaks 1.80 ± 10%, 1.20 ± 8%, No. 5 peaks, 0.27 ± 10%, No. 4 peaks, 0.23 ± 10%, No. 2 peaks, No. 1 peak.
2. standard finger-print according to claim 1, it is characterized in that described Chinese medicine composition prepares by following method: get Rhizoma Chuanxiong 784g, Rhizoma Gastrodiae 196g, pulverize, mix, with 90% alcohol reflux secondary, each 2 hours, merge extractive liquid, filters, filtrate recycling ethanol and to be condensed into relative density be 1.27～1.28 clear paste I; Medicinal residues decoct with water secondary, and each 1 hour, collecting decoction filtered, and it is 1.27～1.28 clear paste II that filtrate is condensed into relative density, merges above-mentioned clear paste I and clear paste II, and the adding appropriate amount of auxiliary materials is made required Chinese medicine preparation.
3. Chinese medicine preparation according to claim 2 comprises capsule, soft capsule, tablet, pill, granule, drop pill, oral liquid, injection.
4. the assay method of standard finger-print according to claim 1 is characterized in that this method adopts high performance liquid chromatography, and chromatographic condition is:
Chromatographic column adopting octadecylsilane chemically bonded silica chromatographic column;
Mobile phase adopts 0.1% phosphoric acid-methanol aqueous solution system, and wherein mobile phase A is 0.1% phosphoric acid solution, and Mobile phase B is a methanol, adopts gradient elution;
Flow velocity is 1mL/min;
Column temperature is 30 ℃;
Detector adopts UV-detector, and the detection wavelength is 276nm;
Number of theoretical plate is pressed object of reference ferulic acid peak and is calculated, and should be not less than 6000.
5. it is that 25～100% methanol is made solvent that the assay method of standard finger-print according to claim 4, the solution that it is characterized in that being used for high-performance liquid chromatogram determination adopt concentration; Preferred need testing solution adopts 50% methanol to make solvent, and object of reference solution adopts 50% methanol to make solvent.
6. the assay method of standard finger-print according to claim 5, the preparation that it is characterized in that object of reference solution are that to get ferulic acid an amount of, accurately claim surely, add 50% methanol and make the solution that every 1mL contains ferulic acid 20 μ g, promptly.
7. the assay method of standard finger-print according to claim 5 is characterized in that the preparation process of need testing solution is as follows:
This composition capsule, tablet, pill, drop pill, granule: get this Chinese medicine composition content, mixing, porphyrize is got about 1g, puts in the conical flask, the accurate 50% methanol 25mL that adds, ultrasonic 30min filters, and gets subsequent filtrate as need testing solution, promptly;
This composition soft: get this Chinese medicine composition content, mixing is got about 1g, puts in the conical flask, adds 75% methanol 30mL, and ultrasonic 30min filters, and gets subsequent filtrate as need testing solution, promptly;
This composition oral liquid: get this Chinese medicine composition, mixing is got about 10mL, to flask, adds 95% methanol 50mL, fully stirs, and filters, and gets subsequent filtrate as need testing solution, promptly.
This composite injection: get the about 10mL of injection, to flask, add 95% methanol 50mL, fully stir, filter, get subsequent filtrate as need testing solution, promptly.
8. the assay method of according to claim 4 Chinese medicine composition standard finger-print is characterized in that gradient elution is in proper order:
9. the assay method of standard finger-print according to claim 4 is characterized in that sample size is 2 μ L～50 μ L.
10. the application of standard finger-print according to claim 1 in the Chinese medicine composition quality control of forming by Rhizoma Chuanxiong and Rhizoma Gastrodiae.
11. application according to claim 10 is characterized in that the finger printing of qualified Chinese medicine composition and the similarity of standard finger-print are not less than 0.80.
12. application according to claim 11, the method that it is characterized in that being used for comparison Chinese medicine composition finger printing and standard finger-print similarity are to adopt included angle cosine method or correlation coefficient process; The preferred chromatographic fingerprints of Chinese materia medica similarity evaluation system that adopts Chinese Pharmacopoeia Commission's regulation.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108478715A (en) * | 2018-06-25 | 2018-09-04 | 江苏康缘药业股份有限公司 | A kind of Chinese medicine composition is preparing the application in treating children's hyperkinetic syndrome drug |
| CN108653586A (en) * | 2018-06-28 | 2018-10-16 | 江苏康缘药业股份有限公司 | A kind of Chinese medicine composition is preparing the application in treating anti-parkinson drug |
| CN109991356A (en) * | 2019-04-15 | 2019-07-09 | 吉林益民堂制药有限公司 | A kind of detection method of Zhipiantong Capsules medicinal material |
| CN113030291A (en) * | 2021-01-28 | 2021-06-25 | 成都第一制药有限公司 | HPLC-ELSD characteristic spectrum of motherwort injection and establishing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100518798C (en) * | 2006-04-17 | 2009-07-29 | 浙江大德药业集团有限公司 | Dispersible tablet with gastrodia tuber for treating headache, and its testing method |
| CN101639470B (en) * | 2008-07-29 | 2013-03-20 | 江苏康缘药业股份有限公司 | Checking method of Chinese medicinal composition standard fingerprint, and use thereof |
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2009
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108478715A (en) * | 2018-06-25 | 2018-09-04 | 江苏康缘药业股份有限公司 | A kind of Chinese medicine composition is preparing the application in treating children's hyperkinetic syndrome drug |
| CN108653586A (en) * | 2018-06-28 | 2018-10-16 | 江苏康缘药业股份有限公司 | A kind of Chinese medicine composition is preparing the application in treating anti-parkinson drug |
| CN109991356A (en) * | 2019-04-15 | 2019-07-09 | 吉林益民堂制药有限公司 | A kind of detection method of Zhipiantong Capsules medicinal material |
| CN109991356B (en) * | 2019-04-15 | 2021-05-07 | 吉林益民堂制药有限公司 | Detection method of medicinal materials of migraine treating capsule |
| CN113030291A (en) * | 2021-01-28 | 2021-06-25 | 成都第一制药有限公司 | HPLC-ELSD characteristic spectrum of motherwort injection and establishing method thereof |
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Inventor after: Zhou Xiaofeng Inventor after: Xiao Wei Inventor after: Bi Yuan Inventor after: Hu Junhua Inventor after: Qin Jianping Inventor after: Wang Zhenzhong Inventor after: Zhang Chenfeng Inventor before: Xiao Wei Inventor before: Bi Yuan Inventor before: Hu Junhua Inventor before: Qin Jianping Inventor before: Wang Zhenzhong Inventor before: Zhang Chenfeng |
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Free format text: CORRECT: INVENTOR; FROM: XIAO WEI BI YUAN HU JUNHUA QIN JIANPING WANG ZHENZHONG ZHANG CHENFENG TO: ZHOU XIAOFENG XIAO WEI BI YUAN HU JUNHUA QIN JIANPING WANG ZHENZHONG ZHANG CHENFENG |
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