CN105424850A - Quality evaluation method for dendrobe medicinal material - Google Patents
Quality evaluation method for dendrobe medicinal material Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000013441 quality evaluation Methods 0.000 title abstract 3
- 238000012360 testing method Methods 0.000 claims abstract description 23
- MMDUKUSNQNWVET-WMRYYKKOSA-N 5,7-dihydroxy-2-(4-hydroxyphenyl)-6-[(2r,3r,4r,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]-8-[(2s,3r,4s,5s)-3,4,5-trihydroxyoxan-2-yl]chromen-4-one Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1C1=C(O)C([C@H]2[C@@H]([C@@H](O)[C@@H](O)CO2)O)=C(OC(=CC2=O)C=3C=CC(O)=CC=3)C2=C1O MMDUKUSNQNWVET-WMRYYKKOSA-N 0.000 claims abstract description 22
- NIABBGMPPWXWOJ-UHFFFAOYSA-N schaftoside Natural products OC1C(O)C(O)C(CO)OC1OC1=C(O)C(OC2C(C(O)C(O)CO2)O)=C(OC(=CC2=O)C=3C=CC(O)=CC=3)C2=C1O NIABBGMPPWXWOJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- MMDUKUSNQNWVET-UHFFFAOYSA-N schaftozide Natural products OC1C(O)C(O)C(CO)OC1C1=C(O)C(C2C(C(O)C(O)CO2)O)=C(OC(=CC2=O)C=3C=CC(O)=CC=3)C2=C1O MMDUKUSNQNWVET-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 21
- 239000013558 reference substance Substances 0.000 claims abstract description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 165
- 240000004638 Dendrobium nobile Species 0.000 claims description 90
- 239000000523 sample Substances 0.000 claims description 46
- 239000000243 solution Substances 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 241001523681 Dendrobium Species 0.000 claims description 25
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 20
- 230000005477 standard model Effects 0.000 claims description 18
- 238000011156 evaluation Methods 0.000 claims description 17
- 241000026010 Dendrobium candidum Species 0.000 claims description 16
- 230000014759 maintenance of location Effects 0.000 claims description 16
- UXDFUVFNIAJEGM-UHFFFAOYSA-N 2-methoxy-5-[2-(3,4,5-trimethoxyphenyl)ethyl]phenol Chemical compound C1=C(O)C(OC)=CC=C1CCC1=CC(OC)=C(OC)C(OC)=C1 UXDFUVFNIAJEGM-UHFFFAOYSA-N 0.000 claims description 14
- 244000283926 Dendrobium chrysotoxum Species 0.000 claims description 14
- 239000000706 filtrate Substances 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 14
- 239000012982 microporous membrane Substances 0.000 claims description 14
- 239000012488 sample solution Substances 0.000 claims description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- 244000131844 Dendrobium aphyllum Species 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000002390 rotary evaporation Methods 0.000 claims description 10
- 239000012453 solvate Substances 0.000 claims description 10
- 239000005695 Ammonium acetate Substances 0.000 claims description 6
- 229940043376 ammonium acetate Drugs 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 6
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 3
- 244000030990 Dendrobium fimbriatum Species 0.000 claims description 3
- 235000019257 ammonium acetate Nutrition 0.000 claims description 3
- 239000013068 control sample Substances 0.000 claims description 3
- 241001264165 Dendrobium devonianum Species 0.000 claims description 2
- 241000229499 Dendrobium loddigesii Species 0.000 claims description 2
- 239000012567 medical material Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
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- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
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- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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Abstract
The invention relates to a quality evaluation method for a dendrobe medicinal material. The method includes the steps that a schaftoside chromatographic peak is adopted as a reference substance, and a standard fingerprint spectrum is formulated through HPLC (high performance liquid chromatography); through comparison of fingerprint spectrums of samples for test and the standard fingerprint spectrum, the quality of the samples for test is determined. According to the method, the pretreatment method for all the samples for test is simple, characteristic components are reserved, and the solution stability of the samples for test is good. The high performance liquid chromatography is high in precision, good in reproducibility and short in analysis time, and has certain specificity, the separation effect of all fingerprint peaks in the obtained fingerprint spectrum is good, the quality of the dendrobe medicinal material can be accurately and comprehensively reflected, the quality standard of the dendrobe medicinal material is further perfected, and therefore the quality evaluation method can be applied to quality grading and authenticity of dendrobe tissue culture seedlings, fresh dendrobe and air-dried dendrobe of medicinal dendrobe.
Description
Technical field
The present invention relates to the quality of medicinal material analysis of the field of Chinese medicines, be specifically related to the quality evaluating method of a kind of HPLC (high performance liquid chromatography) finger print method to all kinds of stem of noble dendrobium medicinal material.
Background technology
The stem of noble dendrobium is a kind of conventional tonic Chinese medicine, is mainly Dendrobium Sw.Dendrobium Sw is a genus maximum in orchid, comprises multiple kinds such as dendrobium candidum, HERBA DENDROBII, dendrobium, Dendrobium Chrysotoxum Lindl.In the world, about have more than the 1100 kind of stem of noble dendrobium, what wherein find in China has 76 kinds.The medical value of the stem of noble dendrobium is with a long history.Early in ancient times, it is top grade that the stem of noble dendrobium is just listed in nourishing in Shennong's Herbal, and for a long time, along with the development in epoch, the stem of noble dendrobium is considered as precious Chinese herbal medicine by people always, has very important nourishing effects.Clinically, the stem of noble dendrobium is used to treat various diseases, has develop immunitypty, anti-oxidant, hypoglycemic and suppress the pharmacological effect such as cancer.Excavate and the irrational utilization stem of noble dendrobium due to artificial uncontrolled for a long time, its wild resource reduces increasingly, market has occurred some are mixed the spurious with the genuine, shoddy phenomenon.In addition, because stem of noble dendrobium product is numerous, quality is also uneven, and its interracial hybridization makes the kind of its nearly edge there is proterties crossover phenomenon, and classification difference is more difficult.At present the evaluation to indivedual or a few constituents is confined to the quality assessment of stem of noble dendrobium medicinal material, evaluation result is more unilateral, evaluation second can not be carried out on the whole, can not repeat, be difficult to apply, therefore, be necessary to find one easy to operate, the quality of medicinal material of efficient assay method to dendrobe fresh product, dry product is evaluated.
Summary of the invention
The object of this invention is to provide a kind of quality evaluating method of stem of noble dendrobium medicinal material, solution is mainly limited to the quality assessment to indivedual or a few constituents to the quality assessment of stem of noble dendrobium medicinal material, its evaluation method is more unilateral, can not repeat, be not enough to system, the complete technical matters showing stem of noble dendrobium medicinal material total quality.
The object of the invention is to be achieved through the following technical solutions, specifically comprise the steps:
1. the preparation of reference substance solution: precision takes schaftoside, methyl alcohol dissolved dilution.
2. the preparation of standard model solution: the standard stem of noble dendrobium medicinal material drying sample getting a certain class different batches, pulverizes, sieves, precision takes Dendrobium, add water or monohydroxy alcohol dissolving, ultrasonic under room temperature, filter, filtrate is concentrated into dry, dissolve with methyl alcohol, constant volume in volumetric flask, shakes up again, filtering with microporous membrane, obtains the standard model solution of such stem of noble dendrobium medicinal material;
3. the foundation of stem of noble dendrobium HPLC-FPS: AlltimaC
18chromatographic column; Diode array detector; Mobile phase is acetonitrile/acetic acid-ammonium acetate solution, gradient elution; Determined wavelength is 280 ± 10nm; Column temperature 25-35 DEG C; Flow velocity 0.8-1.2ml/min; Analyze such standard model solution with this understanding, obtain the finger-print of such stem of noble dendrobium medicinal material;
4. the foundation of standard finger-print: the reference peak using control sample schaftoside chromatographic peak as finger-print, calculates the relative retention time of each characteristic peak of this class standard stem of noble dendrobium sample and retain peak area, formulating the standard finger-print obtaining such stem of noble dendrobium;
5. the preparation of test sample solution: get for examination stem of noble dendrobium medicinal material drying sample, pulverize, sieve, precision takes Dendrobium, add water or monohydroxy alcohol dissolving, ultrasonic under room temperature, filter, filtrate is concentrated into dry, dissolve with methyl alcohol, constant volume in volumetric flask, shakes up again, filtering with microporous membrane, obtains test sample solution;
6. stem of noble dendrobium evaluation of medical materials' quality: the finger-print 3. measuring test sample according to step, contrast with the relative retention time of the characteristic peak in test sample finger-print and reservation peak area and such standard finger-print, similarity >'s 0.85 is the measured stem of noble dendrobium medicinal material of such matter, and similarity <'s 0.6 is the inferior goods of such stem of noble dendrobium medicinal material or the stem of noble dendrobium medicinal material of other kinds.
Further, step 1. described in control sample solution preparation process be: precision takes schaftoside product in contrast, with 75% methyl alcohol (V water: V methyl alcohol=25:75) dissolved dilution, being prepared into concentration is that 16.4 μ g/ml schaftoside solution are reference substance solution;
Further, step 1. described in the preparation process of standard model solution be: the standard stem of noble dendrobium dry sample getting such different batches respectively, pulverize with comminutor, sieve, obtain Dendrobium, precision takes Dendrobium 1.000g, be placed in 100ml conical flask, add 50mL75% methyl alcohol (V water: V methyl alcohol=25:75), take out after ultrasonic 30min under room temperature, filter, filtrate concentrated by rotary evaporation is to dry, dissolve with 75% methanol solvate (V water: V methyl alcohol=25:75), then constant volume in 5ml volumetric flask is transferred to, shake up, with 0.45 μm of filtering with microporous membrane, obtain the standard stem of noble dendrobium sample solution of such different batches,
Further, step 1. described in the preparation process of test sample solution be: get for examination dry sample, pulverize with comminutor, sieve, obtain Dendrobium, precision takes Dendrobium 1.000g, is placed in 100ml conical flask, adds 50mL75% methyl alcohol (V water: V methyl alcohol=25:75), take out after ultrasonic 30min under room temperature, filter, filtrate concentrated by rotary evaporation, to dry, is dissolved with 75% methanol solvate (V water: V methyl alcohol=25:75), then constant volume in 5ml volumetric flask is transferred to, shake up, with 0.45 μm of filtering with microporous membrane, obtain test sample solution;
Further, precision takes weighing error≤0.2% of Dendrobium;
Further, the sieve sieved as crossing aperture 0.335mm;
Further, dissolving the monohydroxy alcohol added is methyl alcohol or ethanol;
Further, room temperature ultrasonic time is 10-40min;
Further, step 3. in adopt high performance liquid chromatograph to carry out the chromatographic condition that measures and system suitability to test and be: chromatographic column: AlltimaC18 chromatographic column (250mm × 4.6mm, 5um); Flow velocity: 1.0ml/min; Column temperature: 30 DEG C; Sample size: 20ul; Determined wavelength: 280nm, reference wavelength 500nm; Mobile phase: comprise mobile phase A and Mobile phase B, mobile phase A is 0.4% acetic acid+20mmol/L ammonium acetate solution, and Mobile phase B is acetonitrile, and carries out wash-out by certain gradient, and number of theoretical plate is pressed schaftoside and calculated, and should be not less than 10000.
Further, step 2. described in the standard stem of noble dendrobium be any one in dendrobium candidum, Dendrobidium huoshanness, Dendrobium aphyllum (Roxb.) C. E. Fisch., dendrobium devonianum, HERBA DENDROBII, Herba Dendrobii, Dendrobium Chrysotoxum Lindl, dendrobium loddigesii Rolfe and Dendrobium fimbriatum Hook.
Further, containing 11 characteristic peaks in the standard finger-print of the described stem of noble dendrobium, one of them is the characteristic peak of schaftoside reference substance.The retention time of 11 characteristic peaks in the standard finger-print of this stem of noble dendrobium is respectively: 10.83min, 13.01min, 21.22min, 24.15min, 27.84min, 28.80min, 43.32min, 44.64min, 52.67min, 56.37min and 66.15min, wherein, the characteristic peak of retention time to be the peak of 24.15min be schaftoside reference substance; The error of this retention time is generally in ± 0.3min, i.e. the retention time of 11 characteristic peaks in the standard finger-print of this stem of noble dendrobium may be 10.83 ± 0.3min, 13.01 ± 0.3min, 21.22 ± 0.3min, 24.15 ± 0.3min, 27.84 ± 0.3min, 28.80 ± 0.3min, 43.32 ± 0.3min, 44.64 ± 0.3min, 52.67 ± 0.3min, 56.37 ± 0.3min and 66.15 ± 0.3min respectively.
Further, described gradient is as follows:
The invention provides a kind of method for building up of stem of noble dendrobium characteristic fingerprint pattern, its beneficial effect mainly had is: compared with the finger-print in past, the inventive method has following significant advantage and purposes: the present invention selects schaftoside to be contrast peak, retention time and peak area normalized are carried out to other characteristic peaks in the stem of noble dendrobium, the impact such as shift of retention time, operate miss between deduction different batches; Fingerprint characteristic peak that the present invention is greater than 5% to relative peak area in the method building finger-print carries out qualitative, breach the too ambiguity of finger-print in the past, clear and definite further to the principal ingredient of finger-print, the globality of stem of noble dendrobium finger-print and composition specificity are united, thus the dendrobe tissue culture seedling of medicinal dendrobium, dendrobe fresh product, the quality grading of air-dried Dendrobium and True-false distinguish can be applied to.Particularly:
1. the reappearance of the method for the invention is good, and the RSD of each total peak relative peak area is less than 5%, and relative retention time is less than 1%; In Precision Experiment, the RSD of each total peak relative peak area is less than 5%, and relative retention time is less than 1%, and sample had good stability within 24 hours.Illustrate that each total chromatographic peak can reflect the interior quality of the stem of noble dendrobium objectively, can as the quality control index of the stem of noble dendrobium.
2. the characteristic fingerprint pattern detection method of the present invention's foundation is simple to the pre-treating method of each test sample, and characteristic chemical constituent retains complete, and test sample stability of solution is good;
3. the precision of this efficient liquid-phase chromatography method is higher, reappearance good, and analysis time is shorter, has certain specificity, and in gained finger-print, each fingerprint peaks separating effect is better;
4. the present invention select peak area larger total peak as characteristic fingerprint peak, by the comparison of characteristic fingerprint peak relative retention time and relative peak area, effectively can characterize the quality of medicinal dendrobium;
5. the characteristic fingerprint pattern set up of the present invention is with schaftoside reference substance for reference to peak, guarantees the relative stability of each speciality fingerprint peaks.
The quality assessment of current China to the stem of noble dendrobium is mainly limited to the quality assessment to indivedual or a few constituents, and its evaluation method is more unilateral, is not enough to system, the complete total quality showing stem of noble dendrobium medicinal material, is badly in need of exploring more advanced, more effective quality evaluating method.And high-efficient liquid phase character finger-print to differentiate stem of noble dendrobium medicinal material and the quality of compound preparation containing stem of noble dendrobium medicinal material significant, and set up a kind of energy more comprehensive quality evaluating method and quality control is carried out to the chemical composition that the stem of noble dendrobium detects have great importance.
Accompanying drawing explanation
With reference to the accompanying drawings the present invention is described in further detail below.
Fig. 1 is the HPLC figure of the reference substance schaftoside chromatographic peak described in the embodiment of the present invention;
Fig. 2 is the finger-print to 10 batches of dendrobium candidum medicinal materials described in the embodiment of the present invention one;
Fig. 3 is the HPLC standard finger-print of the dendrobium candidum described in the embodiment of the present invention one;
Fig. 4 is the finger-print beautifying the stem of noble dendrobium;
Fig. 5 is the finger-print of Dendrobium fimbriatum Hook;
Fig. 6 is the finger-print of HERBA DENDROBII.
Fig. 7 is the HPLC finger-print of 10 batches of Dendrobium Chrysotoxum Lindls described in the embodiment of the present invention two;
Fig. 8 is the HPLC standard finger-print of the Dendrobium Chrysotoxum Lindl described in the embodiment of the present invention two;
Fig. 9 is the HPLC finger-print of 10 batches of Dendrobium aphyllum (Roxb.) C. E. Fisch.s described in the embodiment of the present invention three;
Figure 10 is the HPLC standard finger-print of the Dendrobium aphyllum (Roxb.) C. E. Fisch. described in the embodiment of the present invention three;
Figure 11 is the HPLC finger-print of 10 batches of Herba Dendrobiis described in the embodiment of the present invention four;
Figure 12 is the HPLC standard finger-print of the Herba Dendrobii described in the embodiment of the present invention four;
Figure 13 is the HPLC finger-print of 10 batches of Herba Dendrobiis described in the embodiment of the present invention four;
Figure 14 is the HPLC standard finger-print of the Herba Dendrobii described in the embodiment of the present invention four;
Embodiment
The specific embodiment of the invention is as follows:
Embodiment 1: dendrobium candidum quality evaluating method
Instrument and reagent: instrument: Agilent1200series high performance liquid chromatograph (comprises low pressure binary gradient pump G1312A, column oven G1316A, diode array detector G1315B, Chemstation chem workstation, Agilent Science and Technology Ltd. of the U.S.), the portable comminutor of 100g (Guangzhou Xu Lang plant equipment company limited) Milli-QSynthesis ultrapure water purification system (Millipore company), RQ-250B type ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.), PB303-N electronic balance (MEETTLERTOLEDO, 0.001g), 0.45 μm of micropore filter (Jin Teng company).Reagent: acetonitrile, methyl alcohol (chromatographically pure, Fisherscientific company of the U.S.); Other reagent is pure for analyzing; Ultrapure water (MilliQ ultrapure water crosses 0.45 μm of miillpore filter); Acetic acid (Beijing Orient fine chemical product company limited).
The chromatographic condition that in the present invention, stem of noble dendrobium HPLC-FPS is set up is AlltimaC18 chromatographic column; Diode array detector; Mobile phase is acetonitrile/acetic acid-ammonium acetate solution, gradient elution; Determined wavelength is 280 ± 10nm; Column temperature 25-35 DEG C; Flow velocity 0.8-1.2ml/min; Preferably when flow velocity is 1ml/min, determined wavelength is 280nm, and when column temperature is 30 DEG C, evaluation method is as follows:
(1) preparation of reference substance solution: precision takes schaftoside reference substance 0.164mg, with 75% methyl alcohol (V water: V methyl alcohol=25:75) dissolved dilution, being prepared into concentration is 16.4 μ g/ml schaftoside reference substance solution.
(2) preparation of standard model solution: the dendrobium candidum dry sample getting different batches respectively, pulverize with comminutor, cross pharmacopeia sieve (aperture 0.335mm), precision takes dendrobium candidum powder 1.000g, be placed in 100ml conical flask, add 50mL75% methyl alcohol (V water: V methyl alcohol=25:75), take out after ultrasonic 30min under room temperature, filter, filtrate concentrated by rotary evaporation is to dry, dissolve with 75% methanol solvate (V water: V methyl alcohol=25:75), finally be transferred to constant volume in 5ml volumetric flask, shake up, with 0.45 μm of filtering with microporous membrane, obtain the standard solution of different batches dendrobium candidum sample.
(3) chromatographic condition adopting high performance liquid chromatograph to carry out measuring and system suitability are tested and are: chromatographic resolution column packing AlltimaC18 chromatographic column (250mm × 4.6mm, 5um), mobile phase: comprise mobile phase A and Mobile phase B, mobile phase A is 0.4% acetic acid+20mmol/L ammonium acetate solution, Mobile phase B is acetonitrile; Flow velocity 1ml/min, determined wavelength 280nm, column temperature 30 DEG C; Adopt gradient elution mode: 0min → 12min → 35min → 45min → 60min → 80min, acetonitrile 2% → 15% → 24% → 36% → 75% → 95% (namely employing gradient elution side is as shown in table 1), rear operation 10min; Analyze the standard model solution of different batches with this understanding, obtain the finger-print of dendrobium candidum.
The gradient elution change list of table 1 mobile phase
(4) mensuration of standard finger-print: accurate absorption different batches standard model solution and reference substance solution respectively, inject high performance liquid chromatograph respectively to measure, reference peak using reference substance schaftoside chromatographic peak as finger-print, schaftoside chromatographic peak as shown in Figure 1, calculate the relative retention time of each characteristic peak of standard model and retain peak area, formulating and obtain standard finger-print;
(5) preparation process of test sample solution is: get for examination dry sample, pulverize with comminutor, sieve, obtain Dendrobium, precision takes Dendrobium 1.000g, be placed in 100ml conical flask, add 50mL75% methyl alcohol (V water: V methyl alcohol=25:75), take out after ultrasonic 30min under room temperature, filter, filtrate concentrated by rotary evaporation is to dry, dissolve with 75% methanol solvate (V water: V methyl alcohol=25:75), be then transferred to constant volume in 5ml volumetric flask, shake up, with 0.45 μm of filtering with microporous membrane, obtain test sample solution;
(6) test sample quality assessment: get test sample (comprising the stem of noble dendrobium of dendrobium candidum inferior and other types) according to above-mentioned (3) described method and step, determine finger-print, contrast with standard finger-print, calculate similarity.
According to the method described above, establish HPLC finger-print (as shown in Figure 2) to 10 batches of dendrobium candidum medicinal materials, table 2 is 10 batches of stem of noble dendrobium similarity result, according to the finger-print of 10 batch sample, formulates the standard finger-print of dendrobium candidum.Similarity shows each batch of collection of illustrative plates and the similarity degree contrasting collection of illustrative plates, and its value more illustrates with to contrast collection of illustrative plates more similar close to 1.000.As shown in Table 2, each sample Similarity value is greater than 0.85, and similarity is higher, and the chemical substance difference between sample is less.Each sample collection of illustrative plates similarity concentrates between 0.85-0.96, illustrates that these 10 batches of dendrobium candidum qualities are relatively stable; And the similarity of the stem of noble dendrobium medicinal material of dendrobium candidum medicinal material inferior and other types all below 0.6 (Fig. 4-6 is the stem of noble dendrobium of other types), therefore, evaluation can be made to the quality of all kinds of stem of noble dendrobium according to these characteristic sum similarities of finger-print.
Table 210 batch dendrobium candidum similarity result
Embodiment two: the quality evaluating method of Dendrobium Chrysotoxum Lindl
With embodiment one unlike:
The preparation of standard model solution: the Dendrobium Chrysotoxum Lindl dry sample getting different batches, pulverize with comminutor, cross pharmacopeia sieve (aperture 0.335mm), precision takes Dendrobium 1.000g, be placed in 100ml conical flask, add 50mL75% methyl alcohol (V water: V methyl alcohol=25:75), take out after ultrasonic 30min under room temperature, filter, filtrate concentrated by rotary evaporation, to dry, is dissolved with 75% methanol solvate (V water: V methyl alcohol=25:75), finally be transferred to constant volume in 5ml volumetric flask, shake up, with 0.45 μm of filtering with microporous membrane, obtain the standard model solution of different batches.
Table 310 batch Dendrobium Chrysotoxum Lindl fingerprint similarity evaluation result
According to the method described above, HPLC finger-print (as Fig. 7) is established to 10 batches of Dendrobium Chrysotoxum Lindl medicinal materials, table 3 is 10 batches of Dendrobium Chrysotoxum Lindl similarity result, according to the finger-print of 10 batch sample, formulates the standard finger-print (as Fig. 8) of Dendrobium Chrysotoxum Lindl.
As shown in Table 3, each sample Similarity value is greater than 0.85, and similarity is higher, and the chemical substance difference between sample is less.Illustrate that these 10 batches of Dendrobium Chrysotoxum Lindl qualities are relatively stable; And the similarity of the stem of noble dendrobium medicinal material of Dendrobium Chrysotoxum Lindl medicinal material inferior and other types all below 0.6 (Fig. 4-6 is the stem of noble dendrobium of other types), therefore, evaluation can be made to the quality of all kinds of stem of noble dendrobium according to these characteristic sum similarities of finger-print.
Embodiment three: the quality evaluating method of Dendrobium aphyllum (Roxb.) C. E. Fisch.
With embodiment one unlike:
The preparation of standard model solution: the Dendrobium aphyllum (Roxb.) C. E. Fisch. dry sample getting different batches, pulverize with comminutor, cross pharmacopeia sieve (aperture 0.335mm), precision takes Dendrobium 1.000g, be placed in 100ml conical flask, add 50mL75% methyl alcohol (V water: V methyl alcohol=25:75), take out after ultrasonic 30min under room temperature, filter, filtrate concentrated by rotary evaporation, to dry, is dissolved with 75% methanol solvate (V water: V methyl alcohol=25:75), finally be transferred to constant volume in 5ml volumetric flask, shake up, with 0.45 μm of filtering with microporous membrane, obtain the standard model solution of different batches.
Table 410 batch Dendrobium aphyllum (Roxb.) C. E. Fisch. fingerprint similarity evaluation result
According to the method described above, HPLC finger-print (as Fig. 9) is established to 10 batches of Dendrobium aphyllum (Roxb.) C. E. Fisch. medicinal materials, table 3 is 10 batches of Dendrobium aphyllum (Roxb.) C. E. Fisch. similarity result, according to the finger-print of 10 batch sample, formulates the standard finger-print (as Figure 10) of Dendrobium aphyllum (Roxb.) C. E. Fisch..
As shown in Table 4, each sample Similarity value is greater than 0.85, and similarity is higher, and the chemical substance difference between sample is less.Illustrate that these 10 batches of Dendrobium Chrysotoxum Lindl qualities are relatively stable; And the similarity of the stem of noble dendrobium medicinal material of Dendrobium aphyllum (Roxb.) C. E. Fisch. medicinal material inferior and other types all below 0.6 (Fig. 4-6 is the stem of noble dendrobium of other types), therefore, evaluation can be made to the quality of all kinds of stem of noble dendrobium according to these characteristic sum similarities of finger-print.
Embodiment four: the quality evaluating method of Herba Dendrobii
With embodiment one unlike:
The preparation of standard model solution: the accurate Herba Dendrobii dry sample of label taking, pulverize with comminutor, cross pharmacopeia sieve (aperture 0.335mm), precision takes Dendrobium 1.000g, be placed in 100ml conical flask, add 50mL75% methyl alcohol (V water: V methyl alcohol=25:75), take out after ultrasonic 30min under room temperature, filter, filtrate concentrated by rotary evaporation, to dry, is dissolved with 75% methanol solvate (V water: V methyl alcohol=25:75), finally be transferred to constant volume in 5ml volumetric flask, shake up, with 0.45 μm of filtering with microporous membrane, obtain the standard model solution of different batches.
Table 510 batch Herba Dendrobii fingerprint similarity evaluation result
According to the method described above, HPLC finger-print (as Figure 11) is established to 10 batches of Herba Dendrobii medicinal materials, table 3 is 10 batches of Herba Dendrobii similarity result, according to the finger-print of 10 batch sample, formulates the standard finger-print (as Figure 12) of Herba Dendrobii.
As shown in Table 5, each sample Similarity value is greater than 0.85, and similarity is higher, and the chemical substance difference between sample is less.Illustrate that these 10 batches of Herba Dendrobii qualities are relatively stable; And the similarity of the stem of noble dendrobium medicinal material of Herba Dendrobii medicinal material inferior and other types all below 0.6 (Fig. 4-6 is the stem of noble dendrobium of other types), therefore, evaluation can be made to the quality of all kinds of stem of noble dendrobium according to these characteristic sum similarities of finger-print.
Embodiment five: the quality evaluating method of Dendrobidium huoshanness
With embodiment one unlike:
The preparation of standard model solution: the accurate Dendrobidium huoshanness dry sample of label taking, pulverize with comminutor, cross pharmacopeia sieve (aperture 0.335mm), precision takes Dendrobium 1.000g, be placed in 100ml conical flask, add 50mL75% methyl alcohol (V water: V methyl alcohol=25:75), take out after ultrasonic 30min under room temperature, filter, filtrate concentrated by rotary evaporation, to dry, is dissolved with 75% methanol solvate (V water: V methyl alcohol=25:75), finally be transferred to constant volume in 5ml volumetric flask, shake up, with 0.45 μm of filtering with microporous membrane, obtain the standard model solution of different batches.
Table 610 batch Dendrobidium huoshanness fingerprint similarity evaluation result
According to the method described above, HPLC finger-print (as Figure 13) is established to 10 batches of Dendrobidium huoshanness medicinal materials, table 3 is 10 batches of Dendrobidium huoshanness similarity result, according to the finger-print of 10 batch sample, formulates the standard finger-print (as Figure 14) of Dendrobidium huoshanness.
As shown in Table 5, each sample Similarity value is greater than 0.85, and similarity is higher, and the chemical substance difference between sample is less.Illustrate that these 10 batches of Dendrobidium huoshanness qualities are relatively stable; And the similarity of the stem of noble dendrobium medicinal material of Dendrobidium huoshanness medicinal material inferior and other types all below 0.6 (Fig. 4-6 is the stem of noble dendrobium of other types), therefore, evaluation can be made to the quality of all kinds of stem of noble dendrobium according to these characteristic sum similarities of finger-print.
The present invention is not limited to above-mentioned preferred forms, anyone for the present invention any modification done under enlightenment of the present invention or change, and every have identical with the application or akin technical scheme, all drops within protection scope of the present invention.
Claims (9)
1. a quality evaluating method for stem of noble dendrobium medicinal material, is characterized in that, take schaftoside as reference substance, high performance liquid chromatography is adopted to formulate standard finger-print, the finger-print measured for examination stem of noble dendrobium sample compares with standard finger-print, calculates similarity, determines the quality of sample.
2. the quality evaluating method of stem of noble dendrobium medicinal material according to claim 1, it is characterized in that, standard finger-print is made up by normalization method of the finger-print of the standard stem of noble dendrobium medicinal material of the some different batches of certain class, and similarity >'s 0.85 is the measured stem of noble dendrobium medicinal material of matter; Similarity <'s 0.6 is poor quality or the stem of noble dendrobium medicinal material not belonging to such.
3. the quality evaluating method of the stem of noble dendrobium medicinal material stated according to claim 1 or 2, it is characterized in that, concrete detecting step is as follows:
1. the preparation of reference substance solution: precision takes schaftoside, methanol dilution dissolves.
2. the preparation of standard model solution: the standard stem of noble dendrobium medicinal material drying sample getting certain class different batches respectively, pulverizes, sieves, precision takes powder, add water or monohydroxy alcohol dissolving, ultrasonic under room temperature, filter, filtrate is concentrated into dry, dissolve with methyl alcohol, constant volume in volumetric flask, shakes up again, filtering with microporous membrane, obtains the standard stem of noble dendrobium sample solution of such each batch;
3. the foundation of stem of noble dendrobium HPLC-FPS: AlltimaC
18chromatographic column; Diode array detector; Mobile phase is acetonitrile/acetic acid-ammonium acetate solution, gradient elution; Determined wavelength is 280 ± 10nm; Column temperature 25-35 DEG C; Flow velocity 0.8-1.2ml/min; Analyze the standard stem of noble dendrobium sample solution of such each batch with this understanding, obtain the finger-print of such each batch of standard stem of noble dendrobium sample;
4. the foundation of standard finger-print: the reference peak using control sample schaftoside chromatographic peak as finger-print, calculate the relative retention time of such each batch of each characteristic peak of standard stem of noble dendrobium sample and retain peak area, formulating the standard finger-print obtaining such stem of noble dendrobium medicinal material;
5. the preparation of test sample solution: get for examination stem of noble dendrobium medicinal material drying sample, pulverize, sieve, precision takes Dendrobium, add water or monohydroxy alcohol dissolving, ultrasonic under room temperature, filter, filtrate is concentrated into dry, dissolve with methyl alcohol, constant volume in volumetric flask, shakes up again, filtering with microporous membrane, obtains test sample solution;
6. stem of noble dendrobium evaluation of medical materials' quality: the finger-print 3. measuring test sample according to step, contrast with the relative retention time of the characteristic peak in test sample finger-print and reservation peak area and standard finger-print, similarity >'s 0.85 is matter such stem of noble dendrobium medicinal material measured, and similarity <'s 0.6 is the stem of noble dendrobium medicinal material of such stem of noble dendrobium medicinal material inferior or other kinds.
4. the quality evaluating method of stem of noble dendrobium medicinal material according to claim 1 and 2, it is characterized in that: the preparation process of the reference substance solution that step is 1. described is: precision takes schaftoside, with 75% methyl alcohol (V water: V methyl alcohol=25:75) dissolved dilution, being prepared into concentration is that the schaftoside solution of 16.4 μ g/ml is reference substance solution, the preparation process of the standard model solution that step is 1. described is: the standard stem of noble dendrobium dry sample getting certain class different batches, pulverize with comminutor, sieve, obtain Dendrobium, precision takes Dendrobium 1.000g, be placed in 100ml conical flask, add 50mL75% methyl alcohol (V water: V methyl alcohol=25:75), take out after ultrasonic 30min under room temperature, filter, filtrate concentrated by rotary evaporation is to dry, dissolve with 75% methanol solvate (V water: V methyl alcohol=25:75), then constant volume in 5ml volumetric flask is transferred to, shake up, with 0.45 μm of filtering with microporous membrane, obtain the accurate sample solution of the standard stem of noble dendrobium of such different batches, the preparation process of the test sample solution that step is 1. described is: get for examination stem of noble dendrobium dry sample, pulverize with comminutor, sieve, obtain Dendrobium, precision takes Dendrobium 1.000g, be placed in 100ml conical flask, add 50mL75% methyl alcohol (V water: V methyl alcohol=25:75), take out after ultrasonic 30min under room temperature, filter, filtrate concentrated by rotary evaporation is to dry, dissolve with 75% methanol solvate (V water: V methyl alcohol=25:75), be then transferred to constant volume in 5ml volumetric flask, shake up, with 0.45 μm of filtering with microporous membrane, obtain test sample solution.
5. the quality evaluating method of stem of noble dendrobium medicinal material according to claim 1 and 2, is characterized in that: described precision takes weighing error≤0.2% of Dendrobium; The described sieve sieved as crossing aperture 0.335mm; Described monohydroxy alcohol is methyl alcohol or ethanol; Described room temperature ultrasonic time is 10-40min.
6. the quality evaluating method of stem of noble dendrobium medicinal material according to claim 1 and 2, is characterized in that: mobile phase is 0.4% acetic acid+20mmol/L ammonium acetate solution (A) and acetonitrile (B).
7. the quality evaluating method of stem of noble dendrobium medicinal material according to claim 1 and 2, is characterized in that: described standard stem of noble dendrobium medicinal material can be any one in dendrobium candidum, Dendrobidium huoshanness, Dendrobium aphyllum (Roxb.) C. E. Fisch., dendrobium devonianum, HERBA DENDROBII, Herba Dendrobii, Dendrobium Chrysotoxum Lindl, dendrobium loddigesii Rolfe and Dendrobium fimbriatum Hook.
8. the quality evaluating method of stem of noble dendrobium medicinal material according to claim 5, is characterized in that: described gradient is as follows:
Number of theoretical plate is pressed schaftoside and is calculated, and should be not less than 10000.
9. the quality evaluating method of stem of noble dendrobium medicinal material according to claim 1 and 2, it is characterized in that: containing 11 characteristic peaks in the standard finger-print of the described stem of noble dendrobium, retention time is respectively: 10.83 ± 0.3min, 13.01 ± 0.3min, 21.22 ± 0.3min, 24.15 ± 0.3min, 27.84 ± 0.3min, 28.80 ± 0.3min, 43.32 ± 0.3min, 44.64 ± 0.3min, 52.67 ± 0.3min, 56.37 ± 0.3min and 66.15 ± 0.3min, wherein, the characteristic peak of retention time to be the peak of 24.15 ± 0.3min be schaftoside reference substance.
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