CN106501434A - A kind of HPLC finger print measuring methods of Double Harmonizing Decoction standard soup - Google Patents
A kind of HPLC finger print measuring methods of Double Harmonizing Decoction standard soup Download PDFInfo
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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
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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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- 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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
Abstract
The invention provides a kind of HPLC finger print measuring methods of Double Harmonizing Decoction standard soup, belong to technical field of traditional Chinese medicines, the preparation of (1) test sample solution；(2) preparation of mixed reference substance solution；(3) preparation of single medicinal material negative controls solution；(4) accurate test sample solution, mixed reference substance solution and single medicinal material negative controls solution injection high performance liquid chromatograph of drawing is measured respectively, respectively obtains the liquid chromatogram of test sample solution, mixed reference substance solution and single medicinal material negative controls solution；(5) the similarity evaluation software that is formulated using Chinese Pharmacopoeia Commission, Data Matching is carried out to the liquid chromatogram of test sample solution, mixed reference substance solution and single medicinal material negative controls solution, standard finger-print is obtained final product.The present invention is effectively controlled the quality of Double Harmonizing Decoction standard particle agent, it is ensured that the curative effect of medicine, makes classics recipe obtain more regular quality control.
Description
Technical field
The present invention relates to belong to technical field of traditional Chinese medicines, specifically a kind of HPLC determining fingerprint pattern sides of Double Harmonizing Decoction standard soup
Method.
Background technology
Double Harmonizing Decoction head is loaded in Southern Song Dynasty's period《The formulary of peaceful benevolent dispensary》In volume five, all void is controlled, be the newly-increased side in Baoqing.Former
Side is recited as RADIX PAEONIAE ALBA (seven two halves), Radix Angelicae Sinensis (washing, steeping in wine), the Radix Astragali (honey is processed), Ligusticum wallichii, prepared rhizome of rehmannia (washing, wine are steamed, each three
Two), Radix Glycyrrhizae (processing), Chinese cassia tree (peeling, loses fire, each 2 two 2 money half).Upper is smalls, often takes two money, water one and half, ginger three
Piece, one piece of jujube are decocted and go six points, hollow, clothes before food.Man, married woman's exhaustion or lesion of the five internal organs, sextupole, seven kinds of impairments is controlled, heart kidney is all empty, and essence and blood gas is few, then
Into consumptive disease.Bones of the body collectively is withered overworked, four limbs burnout, fevers and chills alternate, dry throat of coughing, and weary, yellow complexion is breathed heavily in action, slightly touched, easily into his disease.
Or hinder in cold, then place food does not disappear, spleen pain stomachache, and rush down dysentery is told inverse；Or hinder in heat, then dizzy feel dizzy, sputum shortness of breath is dysphoria in chestpalms-soles；
Or because of hungry full action, happiness anger is terrified, disease with and arrive, or empty swollen and do not think to eat, or many foods and not myogenic meat, vexed then abnormal sweating is stolen
Sweat, all consumptive diseases dare not take dry medicine person, and preferably take it.Informal dress is fostered the spirit of nobility in adjusting, and beneficial blood educates god, and stomach feed, and qi-restoratives is damaged.Avoid life
The things such as cold, fruit.
Song dynasty's period《The augmentation formulary of peaceful benevolent dispensary》Roll up in the newly-increased side in five Baoqing, qi-restoratives is damaged.Composition is same《Peaceful
The Bureau of People's Welfare Pharmacies side》.
Period in the Yuan Dynasty, Wei Yilin《The physicians from a family for generations obtain efficacious prescriptions》Roll up in the 80th side's arteries and veins specialty of miscellaneous diseases, deficient.Composition is same《Peaceful
The Bureau of People's Welfare Pharmacies side》.
Ming Dynasty's period, Dong Su's《Special effect good recipe》In 21 all empty logical sides of controlling of volume, man married woman, the exhaustion or lesion of the five internal organs seven is controlled
Wound, insufficiency of vital energy and blood, sallow complexion, four limbs be tired weary, will be the card of consumptive disease, and informal dress is fostered the spirit of nobility beneficial blood.Father's nozzle suitable for reading, often takes three money, water
One, three, ginger, one piece of jujube are decocted, hollow clothes.Composition is same《The formulary of peaceful benevolent dispensary》.
Qing Dynasty's period, Wu Qian's《Yizong Jinjian》Roll up 26 Ce Buming hospital opinion (), miscellaneous diseases heart method gist to roll up
40 consumptive disease therapies, gynaecology's heart method gist are rolled up 44 menstruation regulatings card and are controlled and gynaecology's heart method gist 44 menstruation regulatings of volume
Double and drink in Men Huifang, after controlling serious disease, consumptive disease gas is weary.Blood yiqi, not hot not cold, temperature and adjust it.Two money of the root of herbaceous peony, the Radix Astragali
Process a money half, seven points of liquorice, seven points of middle osmanthus, when normalizing money, one money of prepared rhizome of rehmannia, seven points of Ligusticum wallichii, three, ginger, two pieces of date,
Two, water, decocts one, warmly takes.Consumptive disease, if in anxious, abdomen do not have bitterly the person that is card, when with warm qi and blood invigorating.Fuke Tiaojing is demonstrate,proved
Control, put down and fill blood, i.e., Shiquan Dabu Tang subtracts ginseng, Poria cocos, the bighead atractylodes rhizome.Wu Qian's《Name hospital opinion》Also double and drink is recorded.
Modern Wang Shimin《Do not cut out office side》Chapter 6, Double Harmonizing Decoction is recorded in tonifying recipes, " temperature compensation qi and blood " (1992 editions).Thank
Hai Zhou's《Traditional Chinese medical science successive dynasties good recipe pandect》In, Double Harmonizing Decoction is《The formulary of peaceful benevolent dispensary》Side, also known as double and drink.The root of herbaceous peony, cultivated land,
The Radix Astragali, Radix Angelicae Sinensis are each 10 grams, and Ligusticum wallichii, honey-fried licorice root, Chinese cassia tree are each 4.5 grams.It is decocted in water for oral dose.Function tonifying yin blood, gas of establishing the yang function.The serious disease later stage is controlled,
Cloudy blood yang-energy is not multiple, and shortness of breath and fatigue, dizzy, palpitaition, tongue nature are light, and arteries and veins moistens weak.It is usually used in fatigue, prolonged illness physique on modern clinic empty
The symptom that weak, energy lacks.The clinical application research of Double Harmonizing Decoction has been reported in recent years：The graduate Ma Zhenlie of Korea Spro hospital of Korea
Et al. be prepared into two kinds of health foods using the lactobacillus fermented product of Double Harmonizing Decoction or Double Harmonizing Decoction, a kind of be applied to what alcohol caused
It is still drank after a night；Another kind is used for treating osteoporosis.
Main formulation of the Chinese medicine classics recipe decoction as traditional tcm clinical practice medication, true with reasonable recipe, curative effect
The advantages of cutting, be easy to absorb, working very fast, deep is trusted by extensive patients.But because allocating, carrying, decoct, be long placed in easily temporarily
Generation is mould to lose rotten, soup bitter and amount is big, and standard is difficult to unify, the shortcomings of have a strong impact on its clinical efficacy, it is impossible to suitable
Answer the life requirement of modern.In order to keep the advantage of decoction, a variety of deficiencies of decoction are overcome, " great new in the Ministry of Science and Technology
Under the support energetically of the scientific and technological key special subjects project of medicine initiative " and after academician, the discussion repeatedly of industry specialists, with classics recipe benchmark
The qualitative attribute of soup is evaluation index, produces the standard particle agent being consistent substantially with which in quality and drug effect.
" classics recipe standard particle " is meant with the Key Quality attribute of benchmark decoction as evaluation index, to particle preparation mistake
The critical processes such as the medicinal material extract of journey, concentration, drying are studied, and apply modern production technology to prepare the key with benchmark decoction
The basically identical particle of qualitative attribute.
According to《Classics recipe standard particle researcher common recognition benchmark decoction definition, preparation, qualitative attribute and application》
The relevant related investigation and research for requiring, carrying out Double Harmonizing Decoction benchmark soup.
Compared with the mass analysis method determined with index components content, finger-print can be than more fully reflecting Chinese medicine
The type and quantity for studying point, under the present situation that compound Chinese medicinal preparation active ingredient is not yet illustrated completely, can achieve in Chinese medicine
Effective control in the overall merit of quality and to its overall material, is the effective means of current Chinese medicine and its quality of the pharmaceutical preparations control
One of.The detection method of traditional Chinese medicine fingerprint has chromatography, spectroscopic methodology, spectral method etc..Chromatography mainly includes thin-layer chromatography, height
Effect liquid phase chromatogram, gas-chromatography, Capillary Electrophoresis etc., wherein high performance liquid chromatography have efficient, quick, sensitive, reappearance
Good the characteristics of, with UV-detector (UV), diformazan pipe array detector (DAD), EISD (ELSD) and mass spectrum
Multiple detector combinations such as detector (MS), can be used for the analysis detection of Various Complex composition in Chinese medicine, have become Chinese medicine and referred to
The main stream approach of line collection of illustrative plates research.
Content of the invention
In view of this, the present invention is intended to provide a kind of HPLC finger print measuring methods of Double Harmonizing Decoction standard soup, effectively
Control the quality of Double Harmonizing Decoction standard particle agent, it is ensured that the curative effect of medicine, make classics recipe obtain more regular quality
Control.
For reaching above-mentioned purpose, the technical scheme is that and be achieved in that：A kind of HPLC of Double Harmonizing Decoction standard soup refers to
Line collection of illustrative plates assay method, comprises the steps：
(1) preparation of test sample solution：Precision measures the standard soup of the Double Harmonizing Decoction of different batches, loads on and activates
SPE posts, first eluted with the pure water of 30 volume parts, discard eluent, then the methanol-eluted fractions with 10 parts by weight, collected and elute
Liquid, eluent low temperature is concentrated to dryness, and is finally dissolved with the methyl alcohol of 2 volume parts, with filtering with microporous membrane, is taken subsequent filtrate, obtain
Test sample solution, standby；
(2) preparation of mixed reference substance solution：Precision weighs 5-HMF, Paeoniflorin, Calycosin-7-O-BETA-D-glucoside, liquiritin, asafoetide
Acid, cinnaldehydrum, glycyrrhizic acid, 6-gingerol reference substance are appropriate, plus methyl alcohol is configured to every 1 volume parts containing 5-HMF, Paeoniflorin, Mao Rui
Isoflavone aglycone, liquiritin, forulic acid, cinnaldehydrum, glycyrrhizic acid, 6-gingerol be respectively 0.01,0.12,0.03,0.01,0.01,
0.04th, the mixed reference substance solution of 0.05 and 0.03 parts by weight, shakes up, filtration, standby；
(3) preparation of single medicinal material negative controls solution：Each single medicinal powder is weighed according to 3 times of recipe quantities, is crushed,
Sieve to obtain meal, takes 3 times of recipe quantity meal into full-automatic decocting medicine pot, and precision measures pure water, immersion, decocts, stirs during decoction
Mix, filter while hot, filtrate is well mixed, take appropriate pure water and be settled in 250mL volumetric flasks as single medicinal material negative control
Product solution, standby；
(4) accurate test sample solution, mixed reference substance solution and the single medicinal material negative controls solution drawn is noted respectively
Enter high performance liquid chromatograph to be measured, respectively obtain test sample solution, mixed reference substance solution and single medicinal material feminine gender right
Liquid chromatogram according to product solution；
(5) the similarity evaluation software that is formulated using Chinese Pharmacopoeia Commission, to supplying examination
The liquid chromatogram of sample solution, mixed reference substance solution and single medicinal material negative controls solution carries out Data Matching, obtains final product mark
Quasi- finger-print.
The parts by weight are g/mL with the relation of the volume parts.
Further, the chromatographic condition of step (4) is as follows：
Chromatographic column：Accurasil C18 chromatographic columns, 4.6mm × 250mm, 5 μm；
Mobile phase：- 0.1% phosphate aqueous solution of acetonitrile；
Flow velocity：1.0mL/min；
Wavelength：280nm；
Sample size：10μL；
Column temperature：30℃；
Theoretical cam curve is calculated by Paeoniflorin peak and is not less than 7000；
Gradient elution program is shown in Table 1：
1 finger-print gradient elution program of table
Further, the standard finger-print includes 16 total peaks：From the root of herbaceous peony, peak 5 is from processing Huang at peak 2,3,4
Stilbene, peak 6,11,14 from honey-fried licorice root, peak 7,8,9,16 from prepared RADIX ANGELICAE SINENSIS with yellow rice wine and Ligusticum wallichii, peak 10,12,13 from Chinese cassia tree, peak 15 from
Ginger, peak 1, from wine cultivated land, Ligusticum wallichii, are with reference to peak with No. 4 peaks.
Further, in the standard finger-print, No. 1 peak is 5-HMF, and No. 4 peaks are Paeoniflorin, and No. 5 peaks are that Mao Ruiyi is yellow
Ketoside, No. 6 peaks are liquiritin, and No. 7 peaks are forulic acid, and No. 13 is cinnaldehydrum, and No. 14 peaks are glycyrrhizic acid, and No. 15 is 6-gingerol.
Further, with 0.22 μm of filtering with microporous membrane in step (1).
Further, the preparation method of the single medicinal material negative controls solution is as follows：Weigh respectively according to 3 times of recipe quantities
Single medicinal powder, crushes, and crosses 10-40 mesh sieves and obtains meal；3 times of recipe quantity meal are taken into full-automatic decocting medicine pot, precision is measured
900mL pure water is poured into, soaks 30min, decocts 75min, is stirred three times, while hot with 300 mesh filter-cloth filterings, filtrate body during decoction
Product is about 500mL, and filtrate is well mixed, and takes 1/3rd and is settled in 250mL volumetric flasks as single medicinal material feminine gender with pure water
Reference substance solution, standby.
Further, the preparation method of the standard soup of the Double Harmonizing Decoction is as follows：Nine taste medicinal materials, powder are weighed according to prescription ratio
Broken, cross 10-40 mesh sieves and obtain meal；Three times recipe quantity meal is taken into full-automatic decocting medicine pot, precision measures 900mL pure water and pours into,
Immersion 30min, decocts 75min, stirs three times during decoction, and while hot with 300 mesh filter-cloth filterings, filtrate volume is about 500mL, filter
Liquid is well mixed, and takes 1/3rd and is settled in 250mL volumetric flasks as standard Tangyuan County liquid with pure water, standby.
Present invention also offers application of the said method in the quality testing and quality control of the pharmaceutical preparation of Double Harmonizing Decoction.
Present invention also offers a kind of method of quality control of Double Harmonizing Decoction standard particle, comprises the following steps：
(1) standard finger-print of Double Harmonizing Decoction standard soup is set up according to said determination method；
(2) Double Harmonizing Decoction standard particle to be checked is taken, and finger-print is obtained according to said determination method；
(3) standard finger-print that the finger-print for obtaining step (2) is obtained with step (1) is contrasted, and is met i.e.
For qualified products, do not meet as substandard product.
The preparation of Double Harmonizing Decoction standard particle test sample solution：The Double Harmonizing Decoction standard particle under content uniformity item is taken, finely ground,
About 5g is taken, accurately weighed, put in 100mL measuring bottles, add water appropriate, ultrasonically treated (power 250W, frequency 50kHz) 10min makes molten
Solution, lets cool, is diluted with water to scale, shake up, and precision measures 4ml suspensions into 10mL volumetric flasks, plus methanol constant volume is to scale,
Ultrasonically treated (power 250W, frequency 50kHz) 10min, is then centrifuged for (rotating speed is 8000 turns per minute) 15min, and precision is pipetted
Supernatant, filtration, takes subsequent filtrate, obtains final product.
Relative to prior art, the present invention has the advantage that：
(1) present invention is during the finger-print for setting up Double Harmonizing Decoction standard particle, it is thus identified that 16 common characteristic peaks, and
Its relative retention time and relative peak area are studied, it is ensured that the chemical composition stability of preparation and use safety
Property.
(2) complex chemical composition in Double Harmonizing Decoction standard particle, will realize that the separating difficulty at its characteristic fingerprint peak is big, the present invention
During finger-print is set up, the method that employs gradient elution solves fingerprint characteristic peak and is difficult to separate and impurity
The interference problem at peak.
(3) finger-print of Double Harmonizing Decoction standard particle is set up, single component assay is overcome and is difficult to reflect overall containing
The defect of amount, can on the whole, macroscopically control the inherent quality of Double Harmonizing Decoction standard particle agent, it is ensured that the curative effect of medicine,
Classics recipe is made to have obtained more regular quality control.
(4) treated as an entirety using each active ingredient fingerprint graph in Double Harmonizing Decoction standard particle, focus on each feature
The tandem at peak and correlation, had both avoided and had judged that Double Harmonizing Decoction standard particle was whole because only determining one, two chemical compositions
The one-sidedness of weight, reduces the possibility artificially processed for requisite quality again.For complete, accurate evaluation Double Harmonizing Decoction standard
The quality of particle provides new ways and means.
(5) the inventive method good stability, precision height, favorable reproducibility, convenient and be easy to grasp.
Description of the drawings
Fig. 1 is that different manufacturers chromatographic column HPLC contrasts collection of illustrative plates.
Fig. 2 is different column temperature HPLC contrast collection of illustrative plates.
Fig. 3 is 200-400nm full wavelength scanner figures.
Fig. 4 is that different wave length HPLC contrasts collection of illustrative plates.
Fig. 5 is different gradient HPLC contrast collection of illustrative plates.
Fig. 6 is that different pre-treatments HPLC contrasts collection of illustrative plates.
Fig. 7 is that 10 crowdes of standard soup HPLC contrast collection of illustrative plates.
Fig. 8 is 10 batches of standards soup finger-print (after coupling).
Fig. 9 is 10 batches of standard soup finger-prints (common pattern collection of illustrative plates).
Figure 10 is mixing reference substance and full side HPLC contrasts collection of illustrative plates.
Figure 11 is full side and single medicinal material negative control finger-print Comparative map.
Specific embodiment
The HPLC finger print measuring methods of one Double Harmonizing Decoction standard soup of embodiment
1.1 instruments and reagent
Instrument：
Reagent：
1.2 sample preparation：
1.2.1 the preparation of sample and test sample solution
(1) preparation of sample：Nine taste medicinal materials are weighed according to prescription ratio, is crushed, crossed 10-40 mesh sieves and obtain meal；Take three times
Into full-automatic decocting medicine pot, precision measures 900mL pure water and pours into recipe quantity meal, soaks 30min, decocts 75min, during decoction
Stirring three times, while hot with 300 mesh filter-cloth filterings, filtrate volume is about 500mL, and filtrate is well mixed, and takes 1/3rd and uses pure water
It is settled in 250mL volumetric flasks and is standard Tangyuan County liquid, standby, according to the standard soup that the method prepares 10 batches of variant batches.
(2) preparation of test sample solution：From 10 batches of standard soup, precision measures 4mL respectively, loads on and has activated
SPE posts, are first eluted with 30mL pure water, discard eluent, then use 10mL methanol-eluted fractions, collect eluent, will be dense for eluent low temperature
Be reduced to dry, finally with 2mL methyl alcohol dissolve, with 0.22 μm of filtering with microporous membrane, take subsequent filtrate, obtain need testing solution, standby.
1.2.2 the preparation of mixed reference substance solution：Precision weigh 5-HMF, Paeoniflorin, Calycosin-7-O-BETA-D-glucoside, liquiritin, Ah
Wei's acid, cinnaldehydrum, glycyrrhizic acid, 6-gingerol reference substance are appropriate, plus methyl alcohol is configured to every 1mL containing 5-HMF, Paeoniflorin, Mao Ruiyi Huangs
Ketoside, liquiritin, forulic acid, cinnaldehydrum, glycyrrhizic acid, 6-gingerol be respectively 0.01,0.12,0.03,0.01,0.01,0.04,
0.05 and 0.03mg mixed reference substance solution, shakes up, filtration, standby.
Paeoniflorin (lot number：110736-201539 purity >=96.4%), forulic acid (lot number：110773-201313 purity
>=99.6%), liquiritin (lot number：11610-201106 purity >=93.7%), glycyrrhizic acid (lot number：110731-201418 purity
>=93.1%), cinnaldehydrum (lot number：110710-201408 purity >=99.4%) be purchased from National Institute for Food and Drugs Control；
5-HMF (lot numbers：H40807 purity >=99.0%), Calycosin-7-O-BETA-D-glucoside (lot number：AB019C purity >=98.0%), 6-gingerol
(lot number：AW025G01 purity >=99.0%) be purchased from one side Science and Technology Ltd. of Tianjin.
1.2.3 the preparation of single medicinal material negative controls solution：Each single medicinal powder, powder are weighed according to 3 times of recipe quantities
Broken, cross 10-40 mesh sieves and obtain meal；3 times of recipe quantity meal are taken into full-automatic decocting medicine pot, precision measures 900mL pure water and pours into, soaked
Bubble 30min, decocts 75min, stirs three times during decoction, and while hot with 300 mesh filter-cloth filterings, filtrate volume is about 500mL, filtrate
Be well mixed, take 1/3rd and as single medicinal material negative controls solution is settled in 250mL volumetric flasks with pure water, standby.
1.3 chromatographic condition
Chromatographic column：Accurasil C18 chromatographic columns, 4.6mm × 250mm, 5 μm；
Mobile phase：- 0.1% phosphate aqueous solution of acetonitrile；
Flow velocity：1.0mL/min；
Wavelength：280nm；
Sample size：10μL；
Column temperature：30℃；
Theoretical cam curve is calculated by Paeoniflorin peak and is not less than 7000；
Gradient elution program is shown in Table 1：
1 finger-print gradient elution program of table
1.3.1 the selection of chromatographic column
Shiseido C18 is respectively compared, as a result the chromatographic column of tri- producers of Cosmosil C18, Accurasil C18 is shown in figure
1.(A：PAK C18 chromatographic columns B：Cosmosil C18 chromatographic columns C：Accurasil C18 chromatographic columns)
As can be seen from Figure 1：The separating degree of sample each chromatographic peak under AccurasilC18 chromatographic columns is good, characteristic peak substantially and
Peak shape is preferable.Therefore chromatographic column of the final choice AccurasilC18 chromatographic column as HPLC finger-prints.
1.3.2 the selection of column temperature
Respectively 20 DEG C, 30 DEG C and 40 DEG C of column temperature condition is screened and is optimized, as a result seen Fig. 2.(A：20℃B：40℃
C：30℃)
As can be seen from Figure 2：Under the conditions of 30 DEG C of column temperature, chromatographic peak separating degree is good, and the factor that is disturbed affects little.Therefore final choosing
Select 30 DEG C of optimum column temperature conditions as HPLC finger-prints of column temperature.
1.3.3 the selection of Detection wavelength
Full wavelength scanner in the range of 200-400nm is carried out to sample using PDA detectors, to 230,254,280nm wavelength
Under chromatogram be compared, as a result see Fig. 3, Fig. 4.(A：Wavelength 230nm B：Wavelength 254nm C：Wavelength 280nm)
From the graph 3, Fig. 4 understands：Under three wavelength, the number of chromatographic peak, absorption intensity, separating degree have differences, and comprehensively examine
Consider, when wavelength is in 280nm, at most, each chromatographic peak absorption intensity is average for chromatographic peak number, and separating degree is good, therefore
Final choice 280nm wavelength is best detection wavelength.
1.3.4 the selection of mobile phase
First to flow phase system water-acetonitrile, 0.1% phosphate aqueous solution-acetonitrile, 1% acetic acid-acetonitrile, water-methanol,
0.1% phosphate aqueous solution-methyl alcohol, 1% aqueous acetic acid-methyl alcohol is screened.As a result 0.1% phosphate aqueous solution-acetonitrile is separated
Degree is good, and substantially, final determination 0.1% phosphate aqueous solution-acetonitrile is flow phase system to characteristic peak.Secondly optimize not on year-on-year basis again
Example gradient, gradient 1,2,3 such as following table 2-1, table 2-2, table 2-3, is as a result shown in Fig. 5.(A：Gradient 1B：Gradient 2C：Gradient
3)
Table 2-1 Double Harmonizing Decoction HPLC finger-prints gradient 1 elutes table
Table 2-2 Double Harmonizing Decoction HPLC finger-prints gradient 2 elutes table
Table 2-3 Double Harmonizing Decoction HPLC finger-prints gradient 3 elutes table
As can be seen from Figure 5：Under the conditions of gradient 3, chromatographic peak separating degree is good, and retention time is suitable, therefore final choice ladder
Degree 3 is used as optimal gradient.
1.3.5 the selection of sample pre-treatments
Sample stoste, 60% methyl alcohol alcohol deposition method and SPE solid phase extractions are screened, Fig. 6 is as a result seen.(A：SPE is solid
B is mutually extracted：60% first alcohol deposition method 2C：Sample stoste)
As can be seen from Figure 6：It is more that enriched sample chromatographic peak number under chromatographic condition is followed the example of in SPE SPEs, and each chromatogram
Peak UV absorption and separating degree are good, and therefore final choice SPE solid phase extraction concentration method is optimal pretreatment process.
1.4 methodological study
1.4.1 instrument precision test
Take method below 1.2.2 items and prepare mixed reference substance solution, by the chromatographic condition under 1.3, continuous sample introduction 5 times is every
10 μ L of secondary sample introduction, using the retention time of Paeoniflorin chromatographic peak (No. 4 peaks) and peak area as reference, calculate the relative of each total peak
The RSD values of retention time and relative peak area, RSD are respectively 0.4% and 2.2%, respectively less than 3.0%, show this instrument precision
Degree is good.
1.4.2 stability test
Take legal system available test agent solution below 1.2.1 (2) item, by the chromatographic condition under 1.3, respectively 0,2,4,8,
12nd, 24h sample introductions 1 time, 10 μ L of each sample introduction, using the retention time of Paeoniflorin chromatographic peak and chromatographic peak as reference, are calculated each common
There are the RSD values of the relative retention time and relative peak area at peak, RSD to be respectively 0.7% and 2.8%, respectively less than 3.0%, show
The sample is good in 24h internal stabilities.
1.4.3 replica test
Press Double Harmonizing Decoction original prescription composition, parallel weigh 5 parts of each taste medicine, prepare by method below 1.2.1 (1) item, and press 1.2.1
(2) 5 parts of legal system available test agent solution below item, by the chromatographic condition under 1.3, every part of 10 μ L of need testing solution sample introduction, with
The retention time of Paeoniflorin chromatographic peak and peak area are used as reference, each total peak relative retention time of calculating and relative peak area
Relative standard deviation RSD value, RSD are respectively 1.3% and 2.5%, respectively less than 3.0%, show that this method repeatability is good.
The foundation of 1.5 HPLC finger-prints and technical parameter analysis
1.5.1 collection of illustrative plates collection
10 batches of standard soup that below 1.2.1 (1) item prepared by method are taken, molten by legal system available test agent below 1.2.1 (1) item
Liquid, is measured by the chromatographic condition under 1.3,10 μ L of sample size, is recorded HPLC finger-prints, is as a result seen Fig. 7.
1.5.2 with reference to the selection at peak
Paeoniflorin is the main active of the monarch drug in a prescription root of herbaceous peony first, secondly knowable to need testing solution finger-print, Chinese herbaceous peony
Glycosides is known chemical composition, and stable chemical nature, and, in each chromatographic peak, separating degree is preferably and peak area is larger for its chromatographic peak
, therefore No. 4 peaks (Paeoniflorin) are chosen as the reference peak of finger-print.
1.5.3 the calculating of the relative retention time and relative peak area of the demarcation and total peak at peak is had
The similarity evaluation software (2012 editions) that is formulated using Chinese Pharmacopoeia Commission, right
10 batches of decoction collection of illustrative plates carry out Data Matching, as a result see Fig. 8.As seen from Figure 8, wherein 16 peaks are that 10 batches of decoctions are common, therefore
Determine that 16 peaks are total chromatographic peak, common pattern is determined with median method, Fig. 9 is as a result seen, with the guarantor at Paeoniflorin peak (No. 4 peaks)
It is the relative retention time and relative peak area for calculating total peak with reference to peak to stay time and chromatographic peak area, the results are shown in Table 3, table
4.
3 Double Harmonizing Decoction standard decoction of table has peak relative retention time
4 Double Harmonizing Decoction standard decoction of table has peak relative peak area
From table 3, table 4：Relative retention time RSD≤0.82% at the total peak of 10 batches of Double Harmonizing Decoction standard decoctions, phase
To peak area RSD≤0.82%, both of which is less than 3%, and therefore the method can be used for the HPLC determining fingerprint patterns of Double Harmonizing Decoction.
1.5.4 characteristic peak is pointed out
Characteristic peak is carried out initially with mixing reference substance comparison method to point out, accurate absorption need testing solution, mixing are right respectively
According to each 10 μ L of product solution, high performance liquid chromatograph is injected, record chromatogram, structure is shown in Figure 10.A(1：5-HMF 4：Paeoniflorin 5：
Calycosin-7-O-BETA-D-glucoside 6：Liquiritin 7：Forulic acid 13：Cinnaldehydrum 14：Glycyrrhizic acid 15：6-gingerol)
As seen from Figure 10, No. 1 peak is determined for 5-HMF, No. 4 peaks are Paeoniflorin, and No. 5 peaks are Calycosin-7-O-BETA-D-glucoside, and No. 6 peaks are
Liquiritin, No. 7 peaks are forulic acid, and No. 13 is cinnaldehydrum, and No. 14 peaks are glycyrrhizic acid, and No. 15 is 6-gingerol, it is thus determined that this 8 peaks
Characteristic peak for Double Harmonizing Decoction HPLC finger-prints.
1.5.5 medicinal material attribution analysis
Take the single medicinal material that below No. 1 decoction test sample solution and the 1.2.3 items under 1.2.1 (2) item prepared by method negative
The each 10 μ L of reference substance solution, are measured according to the chromatographic condition under 1.3, obtain each single medicinal material feminine gender in full side and side right
According to the HPLC collection of illustrative plates of liquid, Figure 11 is as a result seen.(A：Full side B：Root of herbaceous peony negative control C：Radix Angelicae Sinensis negative control D：Ligusticum wallichii negative control E：
Cultivated land negative control F：Radix Astragali negative control G：Radix Glycyrrhizae negative control H：Chinese cassia tree negative control I：Ginger negative control J：Date is cloudy
Property control)
From Figure 11：By contrasting relative retention time, the source for having peak in Double Harmonizing Decoction standard decoction is chased after
Tracing back, appearance 2,3,4 being obtained from the monarch drug in a prescription root of herbaceous peony, from astragalus root, from honey-fried licorice root, peak 7,8,9,16 is from wine at peak 6,11,14 at peak 5
Radix Angelicae Sinensis and Ligusticum wallichii, from Chinese cassia tree, from ginger, peak 1 is from wine cultivated land, Ligusticum wallichii at peak 15 at peak 10,12,13.
3.7.6 10 batches of Double Harmonizing Decoction standard soup sample similarity evaluations
The similarity evaluation software (2012 editions) that is formulated using Chinese Pharmacopoeia Commission, with
The chromatographic peak of control spectrum chart display carries out Supplements, and result of calculation similarity, the results are shown in Table 5 as match point.
5 10 batches of Double Harmonizing Decoction standard decoction Similarity Measure results of table
As seen from Table 5：Between 0.938-0.983, mean value is the similarity of 10 batches of Double Harmonizing Decoction standard soup finger-prints
0.978, as a result show：10 batches of Double Harmonizing Decoction standard decoction quality conformances are higher.
The method of quality control of two Double Harmonizing Decoction standard particle of embodiment
A kind of method of quality control of Double Harmonizing Decoction standard particle, comprises the following steps：
(1) Double Harmonizing Decoction standard soup is prepared according to the method in 1.2.1 (1) in embodiment one, using the survey in embodiment one
The method of determining sets up the standard finger-print of Double Harmonizing Decoction standard soup；
(2) Double Harmonizing Decoction standard particle to be checked is taken, and finger-print is obtained according to the assay method in embodiment one；
(3) standard finger-print that the finger-print for obtaining step (2) is obtained with step (1) is contrasted, and is met i.e.
For qualified products, do not meet as substandard product.
The preparation of Double Harmonizing Decoction standard particle test sample solution：The Double Harmonizing Decoction standard particle under content uniformity item is taken, finely ground,
About 5g is taken, accurately weighed, put in 100mL measuring bottles, add water appropriate, ultrasonically treated (power 250W, frequency 50kHz) 10min makes molten
Solution, lets cool, is diluted with water to scale, shake up, and precision measures 4ml suspensions into 10mL volumetric flasks, plus methanol constant volume is to scale,
Ultrasonically treated (power 250W, frequency 50kHz) 10min, is then centrifuged for (rotating speed is 8000 turns per minute) 15min, and precision is pipetted
Supernatant, filtration, takes subsequent filtrate, obtains final product.
Presently preferred embodiments of the present invention is the foregoing is only, not in order to limit the present invention, all in essence of the invention
Within god and principle, any modification, equivalent substitution and improvements that is made etc. should be included within the scope of the present invention.
Claims (9)
1. a kind of HPLC finger print measuring methods of Double Harmonizing Decoction standard soup, it is characterised in that：Comprise the steps：
(1) preparation of test sample solution：Precision measures the standard soup of the Double Harmonizing Decoction of different batches, loads on and has activated
SPE posts, are first eluted with the pure water of 30 volume parts, discard eluent, then the methanol-eluted fractions with 10 parts by weight, collect wash-out
Liquid, eluent low temperature is concentrated to dryness, and is finally dissolved with the methyl alcohol of 2 volume parts, with filtering with microporous membrane, is taken subsequent filtrate, obtain
Test sample solution, standby；
(2) preparation of mixed reference substance solution：Precision weigh 5-HMF, Paeoniflorin, Calycosin-7-O-BETA-D-glucoside, liquiritin, forulic acid,
Cinnaldehydrum, glycyrrhizic acid, 6-gingerol reference substance are appropriate, plus methyl alcohol is configured to every 1 volume parts containing 5-HMF, Paeoniflorin, Mao Ruiyi Huangs
Ketoside, liquiritin, forulic acid, cinnaldehydrum, glycyrrhizic acid, 6-gingerol be respectively 0.01,0.12,0.03,0.01,0.01,0.04,
The mixed reference substance solution of 0.05 and 0.03 parts by weight, shakes up, filtration, standby；
(3) preparation of single medicinal material negative controls solution：Each single medicinal powder is weighed according to 3 times of recipe quantities, is crushed, is sieved
Meal being obtained, 3 times of recipe quantity meal being taken into full-automatic decocting medicine pot, precision measures pure water, immersion is decocted, and stirs, take advantage of during decoction
Heat filtering, filtrate are well mixed, and take appropriate pure water and are settled in 250mL volumetric flasks that to be single medicinal material negative controls molten
Liquid, standby；
(4) accurate test sample solution, mixed reference substance solution and the single medicinal material negative controls solution drawn injects height respectively
Effect liquid phase chromatogram instrument is measured, and respectively obtains test sample solution, mixed reference substance solution and single medicinal material negative controls
The liquid chromatogram of solution；
(5) the similarity evaluation software that is formulated using Chinese Pharmacopoeia Commission, to test sample
The liquid chromatogram of solution, mixed reference substance solution and single medicinal material negative controls solution carries out Data Matching, and the standard of obtaining final product refers to
Line collection of illustrative plates.
The parts by weight are g/mL with the relation of the volume parts.
2. HPLC finger print measuring methods of Double Harmonizing Decoction standard soup according to claim 1, it is characterised in that：The step
Suddenly the chromatographic condition of (4) is as follows：
Chromatographic column：Accurasil C18 chromatographic columns, 4.6mm × 250mm, 5 μm；
Mobile phase：- 0.1% phosphate aqueous solution of acetonitrile；
Flow velocity：1.0mL/min；
Wavelength：280nm；
Sample size：10μL；
Column temperature：30℃；
Theoretical cam curve is calculated by Paeoniflorin peak and is not less than 7000；
Gradient elution program is shown in Table 1：
1 finger-print gradient elution program of table
3. HPLC finger print measuring methods of Double Harmonizing Decoction standard soup according to claim 1, it is characterised in that：The mark
Quasi- finger-print includes 16 total peaks：From the root of herbaceous peony, from astragalus root, peak 6,11,14 is from honey-fried licorice root, peak at peak 5 at peak 2,3,4
7th, 8,9,16 from prepared RADIX ANGELICAE SINENSIS with yellow rice wine and Ligusticum wallichii, peak 10,12,13 from Chinese cassia tree, peak 15 from ginger, peak 1 from wine cultivated land, Ligusticum wallichii,
It is with reference to peak with No. 4 peaks.
4. HPLC finger print measuring methods of Double Harmonizing Decoction standard soup according to claim 1, it is characterised in that：The mark
In quasi- finger-print, No. 1 peak is 5-HMF, and No. 4 peaks are Paeoniflorin, and No. 5 peaks are Calycosin-7-O-BETA-D-glucoside, and No. 6 peaks are liquiritin, No. 7
Peak is forulic acid, and No. 13 is cinnaldehydrum, and No. 14 peaks are glycyrrhizic acid, and No. 15 is 6-gingerol.
5. HPLC finger print measuring methods of Double Harmonizing Decoction standard soup according to claim 1, it is characterised in that：The step
Suddenly with 0.22 μm of filtering with microporous membrane in (1).
6. HPLC finger print measuring methods of Double Harmonizing Decoction standard soup according to claim 1, it is characterised in that：The list
The preparation method of taste medicinal material negative controls solution is as follows：Each single medicinal powder is weighed according to 3 times of recipe quantities, is crushed, cross 10-
40 mesh sieves obtain meal；3 times of recipe quantity meal are taken into full-automatic decocting medicine pot, precision measures 900mL pure water and pours into, soak 30min,
75min is decocted, is stirred three times during decoction, while hot with 300 mesh filter-cloth filterings, filtrate volume is about 500mL, and filtrate mixing is
Even, take 1/3rd as single medicinal material negative controls solution is settled in 250mL volumetric flasks with pure water, standby.
7. HPLC finger print measuring methods of Double Harmonizing Decoction standard soup according to claim 1, it is characterised in that：Described double
As follows with the preparation method of the standard soup of soup：Nine taste medicinal materials are weighed according to prescription ratio, is crushed, crossed 10-40 mesh sieves and obtain meal；Take
Into full-automatic decocting medicine pot, precision measures 900mL pure water and pours into three times recipe quantity meal, soaks 30min, decocts 75min, decocts
Period stirs three times, and while hot with 300 mesh filter-cloth filterings, filtrate volume is about 500mL, and filtrate is well mixed, and takes 1/3rd use
Pure water is settled in 250mL volumetric flasks and is standard Tangyuan County liquid, standby.
8. the method described in any one of claim 1-7 in the quality testing and quality control of the pharmaceutical preparation of Double Harmonizing Decoction should
With.
9. a kind of method of quality control of Double Harmonizing Decoction standard particle, it is characterised in that：Comprise the following steps：
(1) standard finger-print of Double Harmonizing Decoction standard soup is set up according to the assay method described in claim 1-7；
(2) Double Harmonizing Decoction standard particle to be checked is taken, and finger-print is obtained according to the assay method described in claim 1-7；
(3) standard finger-print that the finger-print for obtaining step (2) is obtained with step (1) is contrasted, and is met as closing
Lattice product, does not meet as substandard product.
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