CN109342579A - A kind of HPLC fingerprint atlas detection method of relax bowel and defecation Chinese medicine - Google Patents
A kind of HPLC fingerprint atlas detection method of relax bowel and defecation Chinese medicine Download PDFInfo
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- CN109342579A CN109342579A CN201811083139.1A CN201811083139A CN109342579A CN 109342579 A CN109342579 A CN 109342579A CN 201811083139 A CN201811083139 A CN 201811083139A CN 109342579 A CN109342579 A CN 109342579A
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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
- G01N30/86—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
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
Abstract
The invention discloses a kind of fingerprint atlas detection methods of relax bowel and defecation Chinese medicine, instrument of the present invention to measurement finger-print, chromatographic column, sample solution preparation method, mobile phase, the conditions such as Detection wavelength are groped, it establishes liquid-phase fingerprint determination condition and has carried out methodological study, the standard finger-print of the Chinese medicine has been formulated according to more batches of mass production samples, it can effectively instruct to feed intake in process of production, strictly regulate production operation, really ensure the safety of clinical application, effectively, reliably, have compared with other detection methods easy to operate, the advantages that quick.
Description
Technical field
The invention belongs to field of traditional Chinese medicine detection, are related to a kind of HPLC fingerprint atlas detection method of relax bowel and defecation Chinese medicine.
Background technique
Finger-print is a kind of quantifiable method for detecting Chinese medicine and Chinese materia medica preparation, is mainly used for discerning the false from the genuine and comment
The homogeneity and stability of valence crude drug, semi-finished product and the quality of the pharmaceutical preparations.With the mass analysis method phase of index components content measurement
It can be than more fully reflecting the type and quantity of chemical composition of Chinese materia medica, in compound Chinese medicinal preparation effective component than, finger-print
, it can be achieved that overall merit to Chinese medicine inherent quality and effective control to its whole substance under the status not yet illustrated completely,
It is the most effective means of current Chinese medicine and its quality of the pharmaceutical preparations control.The detection method of traditional Chinese medicine fingerprint have chromatography, spectroscopic methodology,
Spectral method etc..Chromatography mainly includes thin-layer chromatography, high performance liquid chromatography, gas-chromatography, Capillary Electrophoresis etc., wherein efficient liquid
Phase chromatography has the characteristics that efficient, quick, sensitive, favorable reproducibility, has become the main stream approach of traditional Chinese medicine fingerprint research.
Trifoliate orange art ease constipation particle be Jian Min medicine company Group Plc research and development six kind new medicine of Chinese medicine, this product by the dried immature fruit of citron orange,
Rhizoma Atractylodis Macrocephalae, cassia seed, four taste Chinese medicine of semen armeniacae amarae are made, preparation method mainly include medicinal material add water to cook extraction, alcohol precipitation, be added it is auxiliary
Material pelletizing forming and etc..For the quality control of such relax bowel and defecation compound Chinese medicinal preparation, generally use is to single at present
Ingredient carries out qualitative or quantitative, it is difficult to product quality is fully and effectively controlled, to not can guarantee curative effect.
Summary of the invention
The purpose of the invention is to fully and effectively control product quality, a kind of HPLC fingerprint of relax bowel and defecation is established
Map detection method.
To achieve the above object, the present invention uses following technological means:
A kind of HPLC fingerprint atlas detection method of relax bowel and defecation Chinese medicine, the relax bowel and defecation Chinese medicine is by following parts by weight
At being grouped as: 15-30 parts of the dried immature fruit of citron orange, 50-100 parts of Rhizoma Atractylodis Macrocephalae, 15-30 parts of cassia seed, 10-20 parts of semen armeniacae amarae, the detection method packet
Include following steps:
(1) by Chinese medicine it is finely ground after extracted with organic solvent, chromatographic column on obtained extract is carried out with water as eluant, eluent
Chromatographic isolation collects eluent and is configured to test solution；
(2) accurate to draw test solution, upper high performance liquid chromatograph is detected, and the high performance liquid chromatograph contains
UV detector, the UV detector set Detection wavelength as 250-300nm, the stationary phase of the high performance liquid chromatograph
For C18Chromatographic column, mobile phase is the mixed solution of acetonitrile and buffer salt, using gradient elution, flow velocity 0.5-2ml/min, column temperature
It is 25~35 DEG C, number of theoretical plate is not less than 4000；
(3) chromatogram for recording test solution, is commented using Chinese Pharmacopoeia Commission's chromatographic fingerprints of Chinese materia medica similarity
Chromatogram is passed through data importing, multiple spot correction and Data Matching respectively and referred to get standard finger-print and by standard by valence system
The finger-print of line map and sample to be tested carries out similarity analysis.
Preferably, the organic solvent is 40-90% (volume) methanol, preferably 50% methanol.
Preferably, described to be extracted as ultrasonic extraction.
Preferably, the chromatographic column is polyamide column.
Preferably, the UV detector sets Detection wavelength as 280nm.
Preferably, in the gradient elution, volume ratio shared by buffer salt phase is respectively as follows: 0 in each period and mobile phase
~7min, buffer salt phase 92%；7~20min, buffer salt phase 92~80%；20~36min, buffer salt phase 80%；36~
55min, buffer salt phase 80~52%；55~70min, buffer salt phase 52~38%.
Preferably, the buffer salt are as follows: potassium dihydrogen phosphate 0.8g, dodecyl sodium sulfate 1.0g, glacial acetic acid 1ml add water
Dissolve and be diluted to 1000ml, PH 3.0.
Preferably, there are 14 characteristic peaks in the finger-print, by comparing with reference substance map, wherein No. 1 peak is pungent
Fu Lin, No. 9 peaks are aurantio-obtusin.
The beneficial effects of the present invention are:
Chinese medicine is applied under the theoretical direction of Chinese medicine, and any single active ingredient cannot reflect what Chinese medicine was embodied
Whole curative effect, especially compound preparation are to play curative effect, single survey by the mutual synergistic effect between multicomponent, multiple target point
Fixed one or several index ingredients can not reflect the inherent quality of Chinese medicine compound prescription comprehensively.And finger-print can be than more comprehensive
The chemical information that reflection Chinese medicine is included establishes the HPLC finger-print of trifoliate orange art ease constipation particle, measures simultaneously in the present invention
10 batches of trifoliate orange art ease constipation particles, have marked 14 shared peaks and a standard finger-print, obtained chromatogram similarity reaches
To 0.96 or more；Come computational stability, repeatability and precision with its relative retention time and relative peak area, when retaining relatively
Between RSD value be respectively less than 2.0%, the RSD value of relative peak area is respectively less than 5.0%；In 14 ingredients, 2 ingredients are identified,
It is synephrine and aurantio-obtusin respectively.
Trifoliate orange art ease constipation particle finger-print standard provided by the invention can effectively instruct to feed intake in process of production, sternly
Lattice specification production operation, really ensure clinical application safely, effectively, reliably, compared with other detection methods have operation
The advantages that convenient, fast.
Detailed description of the invention
Fig. 1 is the HPLC map after sample to be tested methanol ultrasonic extraction.
Fig. 2 is the HPLC map after sample to be tested EtOH Sonicate extracts.
Fig. 3 is the HPLC map after sample to be tested n-butanol ultrasonic extraction.
Fig. 4 is the HPLC map after sample to be tested refluxing extraction.
Fig. 5 sample crosses the HPLC map after neutral alumina column.
Fig. 6 acetonitrile-sodium dihydrogen phosphate mobile phase HPLC map.
Fig. 7 is the HPLC map that 210nm Detection wavelength obtains.
Fig. 8 is the HPLC map that 250nm Detection wavelength obtains.
Fig. 9 is the HPLC map that 280nm Detection wavelength obtains.
Figure 10 is the HPLC map that 300nm Detection wavelength obtains.
Figure 11 is the HPLC map that 330nm Detection wavelength obtains.
Figure 12 is the HPLC standard finger-print of trifoliate orange art ease constipation particle.
Specific embodiment
The present invention is described in detail below by specific embodiment.
Used trifoliate orange art ease constipation particle is provided by Jian Min medicine company Group Plc in following embodiment.
Prescription: dried immature fruit of citron orange 266.67g Rhizoma Atractylodis Macrocephalae 1000g semen armeniacae amarae 200g cassia seed 266.67g
Preparation method: above four taste adds water to cook extraction, and it is 1.06~1.08 that extracting solution, which is concentrated into relative density, room to be cooled to
Temperature adds ethyl alcohol alcohol precipitation, and supernatant after taking alcohol precipitation is concentrated under reduced pressure into thick paste, be added into thick paste Icing Sugar, dextrin, fruit essence,
Sucralose, mix, granulation, be made 1000 grams of particles to get.
1. instrument and reagent
Waters e2695 high performance liquid chromatograph, quaternary pump, online vacuum degassing system, autosampler, column oven,
UV detector；AB204-E electronic balance (Shanghai plum Teller-support benefit Instrument Ltd.).
The trifoliate orange art ease constipation particle (180601-05,180701-05, totally 10 crowdes) of 10 batches；Synephrine reference substance is (for containing
It surveys and uses, National Institute for Food and Drugs Control's purchase, lot number: 110727-201608)；Aurantio-obtusin reference substance is (for containing survey
With National Institute for Food and Drugs Control's purchase, lot number: 111900-201605)；Acetonitrile is chromatographic grade, and water is purified water.
2. method and step
(1) preparation of test solution: trifoliate orange art ease constipation particle to be measured is finely ground, 1g is taken, accurately weighed, precision is added 50%
Methanol 50ml, weighed weight, 40 minutes (power 250W, frequency 40kHz) of ultrasound are let cool, then weighed weight, are mended with 50% methanol
The weight of sufficient less loss, shakes up, and filtration, precision measures subsequent filtrate 20ml, is evaporated, residue adds water 25ml to make to dissolve, and passes through polyamide
Column (60~90 mesh, 2.5g, internal diameter 1.5cm, dry column-packing) is eluted with water 25ml, is collected eluent, is transferred to 25ml measuring bottle
In, add water to scale, shake up to get.
(2) accurate to draw 10 μ l of test solution, upper high performance liquid chromatograph is detected, the high performance liquid chromatograph
Containing UV detector, the UV detector sets Detection wavelength as 280nm, the stationary phase of the high performance liquid chromatograph
For C18Chromatographic column, mobile phase be acetonitrile and buffer salt (potassium dihydrogen phosphate 0.8g, dodecyl sodium sulfate 1.0g, glacial acetic acid 1ml,
Be dissolved in water and be diluted to 1000ml, PH 3.0) mixed solution, using gradient elution, flow velocity 1ml/min, column temperature 30
DEG C, number of theoretical plate is not less than 4000；
(4) precision test, stability test, repetitive test methodological study: are carried out according to the requirement of finger-print；
(5) sample measures: it is molten to prepare 10 parts of test samples according to step (1) method respectively for access batch trifoliate orange art ease constipation particle
Liquid, it is each it is accurate draw 10 μ l, be measured using the chromatographic condition of step (3), record 0-70min chromatogram, in chromatogram with
Aurantio-obtusin peak (No. 9 peaks) is to calculate relative retention time and relative peak area referring to peak；
(6) foundation of finger-print and peak attribution analysis is carried out: batch trifoliate orange art ease constipation particulate samples of fetching respectively, by step
(1) test solution is prepared under item, be measured by the chromatographic condition of step (3) and record 70min chromatogram, as a result institute is coloured
Spectral peak concentrates in 70min, compares the chromatogram of batch sample, it is determined that 14 shared peaks, by being compared with reference substance map,
Confirmation No. 1 be synephrine, No. 9 be aurantio-obtusin；And under the conditions of finished product chromatographic fingerprinting, to every taste medicinal material in prescription
Finger-print research is carried out, peak attribution analysis is carried out；
(7) sample similarity calculation: resulting 10 batch trifoliate orange art ease constipation particulate chromatography figure importing National Pharmacopeia committee member is issued
2004 editions " similarity evaluations " of cloth, selection " time window " width is 0.1min, by multiple spot
Correction and Data Matching generate chromatographic fingerprinting common pattern, carry out similarity analysis to the finger-print of 10 batches of samples.
3. prepared by test solution: the main purpose that test sample extracts is to reduce checked for impurities (including in albumen, tannin etc.
Auxiliary material in medicine impurity and preparation) influence to characteristic peak peak shape, make characteristic peak separating degree with higher and peak area.It influences
The principal element of extraction effect is Extraction solvent, extracting method and purification process.We according to the prescription of trifoliate orange art ease constipation particle and
Preparation characteristic has been investigated ethyl alcohol, methanol and n-butanol as Extraction solvent respectively, has been compared by analysis, and methanol extracts gained and supplies
Test sample solution can more comprehensively reflect the main component in finished product, and peak shape and repeatability are preferable, so determining methanol conduct
Extraction solvent (Fig. 1,2,3)；Extracting method (ultrasound is heated to reflux) is investigated again, finds the test sample of refluxing extraction
Finger-print (Fig. 4) peak area and peak number are respectively less than ultrasonic extraction；In addition also purification process is investigated, discovery, which is worked as, adopts
Chromatographic separation and purification is carried out with polyamide column, impurity peaks can be further reduced, improves the peak shape of characteristic peak, while again will not be to spy
The peak area and peak number for levying peak have an impact, and purification effect is better than neutral alumina column (Fig. 5).
It is final to determine preparation method of test article are as follows: to take trifoliate orange art ease constipation particle finely ground, take about 1g, accurately weighed, precision is added
50% methanol 50ml, weighed weight are ultrasonically treated 40min (power 250W, frequency 40kHz), let cool, supplied and subtracted with 50% methanol
The weight of mistake, shakes up, and filtration, precision measures subsequent filtrate 20ml, is evaporated, residue adds water 25ml to make to dissolve, and passes through polyamide column (60
~90 mesh, 2.5g, internal diameter 1.5cm, dry column-packing), it is eluted with water 25ml, collects eluent, be transferred in 25ml measuring bottle, add
Water to scale, shake up to get.
4. the foundation of detection method
4.1 chromatographic columns: Agilent ZORBAX SB-C18, 4.6 × 250mm, 5 μm；Detection wavelength: 280nm；Sample volume 10
μl；Column temperature: 30 DEG C；Flow velocity: 1ml/min.
The selection of 4.2 mobile phases
We have investigated multiple groups mobile phase altogether, wherein first group of mobile phase is that acetonitrile-buffer salt (takes potassium dihydrogen phosphate
0.8g, dodecyl sodium sulfate 1.0g, glacial acetic acid 1ml are dissolved in water and are diluted to 1000ml, pH 3.0), second group of flowing
Mutually it is acetonitrile-sodium dihydrogen phosphate (being 4.4 with phosphoric acid regulating ph value), using identical gradient elution program, is compared, sieved
Choosing, liquid chromatogram baseline obtained by discovery acetonitrile-buffer salt system compared with steady, chromatographic peak peak shape compared with symmetrical, separating degree is preferable, it is bright
It is aobvious to be better than acetonitrile-sodium dihydrogen phosphate chromatogram (Fig. 6).
The optimization of 4.3 gradient elution programs: groping through system, optimize, it is found that following linear gradient elution program can be compared with
Chemical component in comprehensive detection preparation, and these ingredients can be made to obtain comparatively ideal separating effect:
1 gradient elution process of table
| Elution time | Buffer salt phase | Acetonitrile phase |
| 0~7min | 92% | 8% |
| 7~20min | 92 → 80% | 8 → 20% |
| 20~36min | 80% | 20% |
| 36~55min | 80 → 52% | 20 → 48% |
| 55~70min | 52 → 38% | 48 → 62% |
1 sample analysis program is completed, the record time is 0~70min.
The determination of 4.4 optimum determining wavelength: the comparative analysis through liquid chromatogram map finds to refer within the scope of 250-300nm
Line peak separating degree is good, and synephrine, aurantio-obtusin can also detect (Fig. 8,9,10), especially using 280nm as the fingerprint of Detection wavelength
Map can most reflect the ingredient (Fig. 9) of preparation comprehensively, and peak shape is best.And peak separating degree and color outside 250-300nm range
Number, baseline and the signal of spectral peak respond all weaker (Fig. 7,11).So determine that 250-300nm range is Detection wavelength,
280nm is best detection wavelength.
5. methodological study
5.1 stability tests: taking test solution according to condition under above-mentioned chromatography item, 0,4,8,12h, measure for 24 hours, examine
Examine the relative retention time at each shared peak and the RSD of relative peak area.The result shows that the relative retention time of each chromatographic peak is small
In 2.0%, the relative peak area of each chromatographic peak is respectively less than 2.0%, meets fingerprint pattern technology requirement.It is shown in Table 2-3.
2 trifoliate orange art ease constipation granule stability of table investigates relative retention time
3 trifoliate orange art ease constipation granule stability of table investigates relative peak area
5.2 repetitive tests: taking 6 parts of same sample lots, prepares 6 parts of confessions according to 1 lower sample solution preparation method
Test sample solution is measured under above-mentioned chromatographic condition, investigates the relative retention time and relative peak area at each shared peak
RSD.The result shows that the relative retention time of each chromatographic peak is respectively less than 2.0%, the relative peak area of each chromatographic peak is respectively less than
5.0%, meet fingerprint pattern technology requirement.It is shown in Table 4-5.
4 trifoliate orange art ease constipation particle repeatability of table investigates relative retention time
5 trifoliate orange art ease constipation particle repeatability of table investigates relative peak area
5.3 precision tests: it takes test solution according to condition under above-mentioned chromatography item, continuous sample introduction 6 times, investigates each shared
The relative retention time at peak and the RSD of relative peak area.The result shows that the relative retention time of each chromatographic peak is respectively less than 0.1%,
The relative peak area of each chromatographic peak is respectively less than 3.0%, meets fingerprint pattern technology requirement.It is shown in Table 6-7.
6 trifoliate orange art ease constipation particle precision of table investigates relative retention time
7 trifoliate orange art ease constipation particle precision of table investigates relative peak area
6. the foundation of finger-print: taking 10 batches of trifoliate orange art ease constipation particulate samples respectively, prepare test solution, measure and record
85min chromatogram, as a result all chromatographic peaks concentrate in 70min, compare the chromatogram of 10 batches of samples, it is determined that 14 shared
Peak.By confirmation, No. 1 be synephrine, No. 9 be aurantio-obtusin, because cassia seed be compound ease constipation main active, select
Aurantio-obtusin is reference peak；
6.1 sample similarity calculations: by 10 batches of trifoliate orange art ease constipation particulate chromatography figures import Chinese Pharmacopoeia Commission promulgation " in
Medicine chromatographic fingerprinting similarity evaluation system (2004A editions) ", selection " time window " width are 0.1min, are generated using sample 5
Control spectrum generates chromatographic fingerprinting common pattern, 10 batches of sample fingerprint similarities by multiple spot correction and Data Matching
Calculated result is shown in Table 8.
80 batches of sample similarities of table
| Lot number | Similarity |
| 180601 | 0.990 |
| 180602 | 0.981 |
| 180603 | 0.966 |
| 180604 | 0.988 |
| 180605 | 0.987 |
| 180701 | 0.972 |
| 180702 | 0.990 |
| 180703 | 0.991 |
| 180704 | 0.994 |
| 180705 | 0.989 |
| Reference fingerprint | 1 |
The formulation of 6.2 trifoliate orange art ease constipation particulate level finger-prints
More batches of trifoliate orange art ease constipation particles are taken, test solution is made by the preparation method of the test solution respectively, according to
Resulting more batches of detection datas are detected, the HPLC-UV detection of trifoliate orange art ease constipation particle is established, high-efficient liquid phase color spectral peak is established and retains
Then time and peak area value collect all detection datas, calculate the average value and opposite peak of each corresponding peak relative retention time
The average value of area and standard deviation etc., respectively with referring to peak Average residence time and average peak area be divided by, as standard
The opposite peak retention time and relative peak area value of finger-print export calculated result, formulate standard fingerprint data, draw
Standard finger-print, standard finger-print are shown in Figure 12, the results are shown in Table 9.
9 standard fingerprint data of table
Correlation between 6.3 medicinal materials and finished product finger-print
The preparation of medicinal material test solution: taking ingredients in prescription to extract according to granular preparation technique respectively, system
Medicinal extract is obtained, carries out synergy according to standard finger-print condition.It the results are shown in Table 10.
10 trifoliate orange art ease constipation particle of table and medicinal material correlation map
| Peak number | The dried immature fruit of citron orange | Rhizoma Atractylodis Macrocephalae | Semen armeniacae amarae | Cassia seed |
| 1 | + | |||
| 2 | + | |||
| 3 | + | + | + | |
| 4 | + | |||
| 5 | + | |||
| 6 | + | |||
| 7 | + | |||
| 8 | + | + | ||
| 9(s) | + | |||
| 10 | + | |||
| 11 | + | |||
| 12 | + | + | ||
| 13 | + | |||
| 14 | + |
Claims (8)
1. a kind of HPLC fingerprint atlas detection method of relax bowel and defecation Chinese medicine, which is characterized in that the relax bowel and defecation Chinese medicine by with
Lower parts by weight at being grouped as: 15-30 parts of the dried immature fruit of citron orange, 50-100 parts of Rhizoma Atractylodis Macrocephalae, 15-30 parts of cassia seed, 10-20 parts of semen armeniacae amarae, should
Detection method includes the following steps:
(1) by Chinese medicine it is finely ground after extracted with organic solvent, by chromatographic column on obtained extract, carry out chromatography as eluant, eluent with water
Separation collects eluent and is configured to test solution；
(2) accurate to draw test solution, upper high performance liquid chromatograph is detected, and the high performance liquid chromatograph contains ultraviolet
Detector, the UV detector set Detection wavelength as 250-300nm, and the stationary phase of the high performance liquid chromatograph is C18
Chromatographic column, mobile phase is the mixed solution of acetonitrile and buffer salt, using gradient elution, flow velocity 0.5-2ml/min, column temperature 25
~35 DEG C, number of theoretical plate is not less than 4000；
(3) chromatogram for recording test solution, utilizes chromatographic fingerprints of Chinese materia medica similarity evaluation system of Chinese Pharmacopoeia Commission
Chromatogram, is passed through that data import, multiple spot correction and Data Matching are to get standard finger-print and by standard fingerprint figure by system respectively
Spectrum and the finger-print of sample to be tested carry out similarity analysis.
2. the HPLC fingerprint atlas detection method of relax bowel and defecation Chinese medicine as described in claim 1, it is characterised in that: described organic molten
Agent is 40-90% methanol, preferably 50% methanol.
3. the HPLC fingerprint atlas detection method of relax bowel and defecation Chinese medicine as described in claim 1, it is characterised in that: described to be extracted as
Ultrasonic extraction.
4. the HPLC fingerprint atlas detection method of relax bowel and defecation Chinese medicine as described in claim 1, it is characterised in that: the chromatographic column
For polyamide column.
5. the HPLC fingerprint atlas detection method of relax bowel and defecation Chinese medicine as described in claim 1, it is characterised in that: the ultraviolet inspection
That surveys device sets Detection wavelength as 280nm.
6. the HPLC fingerprint atlas detection method of relax bowel and defecation Chinese medicine as described in claim 1, it is characterised in that: the gradient is washed
In de-, volume ratio shared by buffer salt phase is respectively as follows: 0~7min, buffer salt phase 92% in each period and mobile phase；7~
20min, buffer salt phase 92~80%；20~36min, buffer salt phase 80%；36~55min, buffer salt phase 80~52%；55~
70min, buffer salt phase 52~38%.
7. the HPLC fingerprint atlas detection method of relax bowel and defecation Chinese medicine as described in claim 1, it is characterised in that: the buffer salt
Are as follows: potassium dihydrogen phosphate 0.8g, dodecyl sodium sulfate 1.0g, glacial acetic acid 1ml are dissolved in water and are diluted to 1000ml, and pH is
3.0。
8. the HPLC fingerprint atlas detection method of relax bowel and defecation Chinese medicine as described in claim 1, it is characterised in that: the fingerprint image
There are 14 characteristic peaks in spectrum, by comparing with reference substance map, wherein No. 1 peak is synephrine, No. 9 peaks are aurantio-obtusin.
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Cited By (1)
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|---|---|---|---|---|
| CN113533563A (en) * | 2021-07-07 | 2021-10-22 | 健民药业集团股份有限公司 | Method for simultaneously detecting contents of four components of liver-soothing, stomach-harmonizing and pain-relieving traditional Chinese medicine |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101366849A (en) * | 2007-08-15 | 2009-02-18 | 未名天人中药有限公司 | Quality control method for traditional Chinese medicine citrus aurantium |
-
2018
- 2018-09-17 CN CN201811083139.1A patent/CN109342579B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101366849A (en) * | 2007-08-15 | 2009-02-18 | 未名天人中药有限公司 | Quality control method for traditional Chinese medicine citrus aurantium |
Non-Patent Citations (3)
| Title |
|---|
| 刘龙忠: "HPLC法测定肠舒灵胶囊中盐酸小檗碱含量", 《药物研究》 * |
| 张玲 等: "枳实配方颗粒、相应饮片及汤剂HPLC图谱对比分析", 《中国中医药信息杂志》 * |
| 柯雪红 等: "HPLC法测定苍芷喷鼻液及枳实药材中辛弗林的含量", 《中药新药与临床药理》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113533563A (en) * | 2021-07-07 | 2021-10-22 | 健民药业集团股份有限公司 | Method for simultaneously detecting contents of four components of liver-soothing, stomach-harmonizing and pain-relieving traditional Chinese medicine |
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