CN110243988A - The method for building up of strong medicine white flower nine inner bright HPLC finger-print - Google Patents
The method for building up of strong medicine white flower nine inner bright HPLC finger-print Download PDFInfo
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- G—PHYSICS
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- 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
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- 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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Abstract
The invention belongs to Fingerprint of Chinese medicine materia fields, and in particular to a kind of method for building up of strong medicine white flower nine inner bright HPLC finger-print.The method for building up of the strong medicine white flower nine inner bright HPLC finger-print obtains strong medicine white flower nine inner bright common pattern finger-print using white flower nine inner bright main component caffeic acid as object of reference accordingly.Finger-print shares chromatographic peak 10, chemical component in white flower nine inner bright medicinal material can sufficiently be reacted, information content is relatively abundant, method reproducibility is good, stronger theoretical foundation is provided to control quality of medicinal material and identification medicinal material superiority and inferiority, quality control and the true and false identification for improving strong medicine white flower nine inner bright are horizontal, realize quickly, accurately identify the true and false superiority and inferiority of white flower nine inner bright.
Description
[technical field]
The present invention relates to Fingerprint of Chinese medicine materia fields, and in particular to a kind of strong medicine white flower nine inner bright HPLC finger-print
Method for building up.
[background technique]
White flower nine inner bright is composite family Blumea balsamifera platymiscium Blumea megacephala (Randeria) Chang et
The aerial part of Tseng originates in the province such as Yunnan, Sichuan, Guizhou, Guangxi, Guangdong, Southern Hunan, South Jiangxi, Fujian and Taiwan
Area.White flower nine inner bright common is decocted in water for oral dose that treat puerperal hemorrhage excessive Zhuang nationality in Guangxi is civil.
Traditional Chinese medicine fingerprint (fingerprinting) is to borrow DNA fingerprinting to develop.Grow up at first
It is chemical composition of Chinese materia medica chromatographic fingerprinting, especially high performance liquid chromatography (HPLC) finger-print.HPLC has very high point
From degree, complicated chemical component can be separated and form the different peak of height and form a chromatogram, these chromatographic peaks
Height and peak area have respectively represented various different chemical compositions and its content.The research and foundation of traditional Chinese medicine fingerprint, for
Traditional Chinese medicine quality is improved, the modernization of Chinese medicine is promoted to be of great significance.
Strong medicine white flower nine inner bright has been substantially carried out character identification, microscopical characters, physical and chemical identification and assay etc. at present, this
A little methods there are information content small, sample chemical ingredient embodies not comprehensively, distinctive compound lazy weight the problems such as, therefore can not show
Strong medicine white flower nine inner bright total quality.Such as Ning little Qing (Ning little Qing, Lu Rumei, the such as yellow beautiful chastity strengthen medicine white flower nine inner bright chemistry at
Divide research [J] Chinese medicine, 2016,39 (11): 2536-2538.) white flower nine inner bright effective component is studied, to catechu
Acid, chlorogenic acid and coffee acid content are determined.It only determines the quality of medicinal material using the content of wherein several ingredients as index
Superiority and inferiority.However, strong medicine (Chinese medicine) has complicated chemical component, effective component is more, and non-principal component is more, heterogeneity or effect it
Between influence each other, any active constituent all can not comprehensively reflect the overall quality and curative effect of the medicine, thus be difficult only according to
The validity and specificity of Chinese medicine are evaluated by one or more of ingredients.
U.S. Food and Drug Administration (FDA) is in related botanical medicine substance and botanical drug product part, by fingerprint image
Spectrum is introduced into quality control；The World Health Organization (WHO) points out in its herbal medicine evaluation guide, the botanical medicine mass spectrum that cannot identify
With the effective component of final products, chromatographic fingerprinting diagnostic characteristics ingredient or blending constituent can be used, guarantee product quality
Consistency.
The current research to strong medicine white flower nine inner bright finger-print both at home and abroad is there is not yet any report, the present invention are white to strong medicine
Hua Jiuli carries out high-efficiency liquid-phase fingerprint research, compensates for the blank under white flower nine inner bright quality standard item, is in white flower nine
The quality evaluation of bright medicinal material provides foundation, and uses white flower nine inner bright for more scientific, reasonable, specification ground, improves its clinic
The safety of medication provides reference.
[summary of the invention]
The object of the present invention is to provide a kind of method for building up of strong medicine white flower nine inner bright HPLC finger-print.The method energy
Enough reliable basis is provided for the identification of white flower nine inner bright and quality control.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of method for building up of strong medicine white flower nine inner bright HPLC finger-print, comprising the following steps:
(1) preparation of reference substance solution: taking caffeic acid reference substance, adds methanol dissolution that reference substance solution is made；
(2) preparation of test solution: precision weighs strong medicine white flower nine inner bright medicinal material coarse powder, adds water, ultrasonic extraction is let cool
To room temperature, the weight of less loss is supplied with water, is shaken up, filter, take subsequent filtrate to get；
(3) high performance liquid chromatography measures: the test sample of the reference substance solution of accurate aspiration step (1) and step (2) respectively
Each 10-20 μ l injection high performance liquid chromatograph of solution, measurement record chromatogram, are referring to peak, by dividing with caffeic acid chromatographic peak
Analysis relatively determines that feature shares peak to get the white flower nine inner bright HPLC finger-print；
Wherein, chromatographic condition are as follows: using the alkyl linked silica gel of C18 as filler；Using acetonitrile as mobile phase A, with phosphoric acid solution
Gradient eluent for Mobile phase B composition carries out gradient elution；Detection wavelength is 300-350nm.
Further, the step (1) is carried out by following operation: being taken caffeic acid reference substance, is added methanol dissolution that every 1ml is made
The reference substance solution of the 20 μ g containing caffeic acid.
Further, the step (2) is carried out by following operation: precision weighs white flower nine inner bright medicinal material coarse powder 1g, adds water
20-40ml, close plug, weighed weight, ultrasonic extraction 20-40min are let cool to room temperature, then weighed weight, and the weight of less loss is supplied with water
Amount, shake up, filter, take subsequent filtrate to get.
Preferably, the step (2) is carried out by following operation: precision weighs white flower nine inner bright medicinal material coarse powder 1g, adds water
20ml, close plug, weighed weight, ultrasonic extraction 30min are let cool to room temperature, then weighed weight, and the weight of less loss is supplied with water, is shaken
It is even, with 0.45 μm of filtering with microporous membrane, take subsequent filtrate to get.
Further, the chromatographic condition of the step (3) are as follows: using the alkyl linked silica gel of C18 as filler；It is stream with acetonitrile
Dynamic phase A, the gradient eluent formed using 0.1% phosphoric acid solution as Mobile phase B carry out gradient elution；Column temperature is 25 DEG C；Detect wave
A length of 300-350nm；Flow velocity is 1.0ml/min；Analysis time is 60min, and sample volume is 10-20 μ l.
Further, it is eluted using following gradient elution mode:
1 gradient elution program table of table
The present invention establishes white flower nine inner bright medicinal materials fingerprint, is made of 10 shared fingerprint peaks, the finger-print 10
The relative retention time and standard deviation such as the following table 2 of a shared fingerprint peaks.
The retention time and relative standard deviation of table 2 finger-print, 10 shared fingerprint peaks
To improve white flower nine inner bright quality of medicinal material controlled level, inventor uses high performance liquid chromatography, with white flower nine inner bright
Middle principle active component caffeic acid is object of reference, researches and develops white flower nine inner bright HPLC fingerprint, obtains strong medicine accordingly
The finger-print of white flower nine inner bright common pattern, finger-print share chromatographic peak 10, can sufficiently react white flower nine inner bright medicinal material
Common pattern finger-print, finger-print share chromatographic peak 10, can sufficiently react chemical component in white flower nine inner bright, information is rich
Richness, method reproducibility is good, to control quality of medicinal material and identifies medicinal material superiority and inferiority offer theoretical foundation.
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are:
(1) white flower nine inner bright medicinal materials fingerprint method of the present invention is simple to test article treating method, and characteristic chemical constituent is protected
It stays completely, test solution is stablized.
(2) high performance liquid chromatography precision of the present invention is higher, and reproducibility is good, and specificity is strong.
(3) present invention, which establishes standard finger-print, 10 shared peaks, and information content is larger, changes in more complete reservation test liquid
It studies point.
(4) pass through similarity evaluation, selected Guangxi difference counties and cities white flower nine inner bright fingerprint similarity is both greater than
0.90, it has good correlation.
(5) present invention establishes white flower nine inner bright medicinal materials fingerprint method, can get white flower nine inner bright medicine by this method
Material standard finger-print, whether there is or not can be effectively controlled white flower nine inner bright quality, improve white flower nine inner bright quality of medicinal material at relatively more shared peak
Appraisement system, for white flower nine inner bright quality of medicinal material comprehensively, effectively control theoretical and time basis is provided.
[Detailed description of the invention]
Fig. 1 is the HPLC finger-print of reference substance solution, in figure: 6 be caffeic acid；
Fig. 2 is the HPLC finger-print of white flower nine inner bright medicinal material；
Fig. 3 is that each batch of strong medicine white flower nine inner bright Herbal HPLC Fingerprint integrates stacking chart；
Fig. 4 is that white flower nine inner bright test sample HPLC finger-print precision investigates stacking chart；
Fig. 5 is white flower nine inner bright test sample HPLC finger-print study on the stability stacking chart；
Fig. 6 is that white flower nine inner bright test sample HPLC finger-print repeatability investigates stacking chart.
[specific embodiment]
13 batches of separate sources white flower nine inner bright medicinal materials are established finger-print under the conditions of same finger-print by inventor respectively,
Then finger-print is merged, determines shared fingerprint characteristic figure, increases finger-print information content, to improve fingerprint identification energy
Power realizes the comprehensive overall evaluation of finger-print.Below by specific embodiment, the invention will be further described, these embodiments
It is merely to illustrate the present invention, is not intended to limit the scope of the invention.
Embodiment 1
1 experimental material and instrument
1.1 medicinal materials: the place of production and collecting time such as table 3.
The 3 white flower nine inner bright medicinal material place of production of table and collecting time
| Medicinal material number | Crude drug source (place of production) | Collecting time |
| 1 | Mengshan | 2014.11 |
| 2 | Nanning peak | 2014.11 |
| 3 | Bar horse | 2014.11 |
| 4 | Nanning peak | 2014.03 |
| 5 | It etc. | 2015.11 |
| 6 | Bar horse | 2015.11 |
| 7 | Beiliu City | 2015.11 |
| 8 | Napo County | 2013.06 |
| 9 | Chongzuo | 2013.11 |
| 10 | Nanning tiger ridge | 2015.11 |
| 11 | Beiliu City | 2016.10 |
| 12 | Anti- city | 2015.11 |
| 13 | Luchuan | 2016.10 |
1.2 instruments: Agilent1260 high performance liquid chromatograph (including G1311C quaternary pump, G1329B autosampler,
G1316A column oven, G1315D DAD detector, Agilengt1260 chromatographic work station (Agilent Technologies, the U.S.))；In
Type ultrasonic cleaner (Elma Schmidbauer GmbH, P300H)；(Sai Duolisi scientific instrument (Beijing) have electronic balance
Limit company, SQP)；" similarity evaluation 2004 A editions (Chinese Pharmacopoeia Commission) ".
1.3 reagents: caffeic acid reference substance (being purchased from National Institute for Food and Drugs Control) lot number: 5WZE-RZUW；Mobile phase
Acetonitrile (being purchased from silent winged scientific and technological (China) Co., Ltd of generation that of match) lot number: A998-4；Phosphoric acid (is purchased from Tianjin recovery fine chemistry industry
Research institute) lot number: 25447-33-0.
2 high performance liquid chromatography
2.1 chromatographic conditions: chromatographic column is using octadecylsilane chemically bonded silica as filler (Agilent chromatographic column (4.6mm
× 150mm, 5 μm))；Using gradient elution, elution program such as table 4
4 mobile phase elution program of table
Mobile phase A: acetonitrile；Mobile phase B: 0.1% phosphoric acid；Detection wavelength 325nm, flow velocity 1ml/min；25 DEG C of column temperature；Into
10 μ l of sample amount；Detection time is 60min, and theoretical cam curve is not less than 3000 in terms of caffeic acid.
The preparation of 2.2 reference substance solutions: precision weighs caffeic acid 0.2mg, until 10ml volumetric flask, is dissolved and be diluted to methanol
Scale, ultrasonic 5min to get.
The preparation of 2.3 test solutions: precision weighs each place of production and strengthens medicine white flower nine inner bright coarse powder 1g, sets stuffed conical flask respectively
In, precision plus water 20ml, close plug, weighed weight, ultrasonic extraction 30min lets cool to room temperature, weighed weight, after mending weight with water, shakes
It is even, with 0.45 μm of filtering with microporous membrane, take subsequent filtrate to get.
2.4 measurements: accurate absorption test solution and each 10 μ l of reference substance solution inject high performance liquid chromatograph respectively, shine
High effective liquid chromatography for measuring records 60 minutes chromatograms (Fig. 1, Fig. 2).
Embodiment 2
13 batch of white flower nine inner bright medicinal material (medicinal material number 1-13) is taken, by legal system available test sample solution below " 2.3 " item, is pressed
Chromatographic condition and measuring method under " 2.4 " item are measured under " 2.1 " item, obtain 13 crowdes of sample HPLC finger-print stacking charts,
As shown in Figure 3.By this 13 batches of HPLC trace analysis, similarity evaluation is carried out, determine that feature shares peak: finger-print there are 10
Feature shares peak, retention time, peak area average value and account for total peak area ratio and be summarized as follows:
No. 1 peak, retention time 2.726min, RSD%0.66%, peak area 156.555, RSD%47.01%；Zhan is total
The 1.520% of peak area；
No. 2 peaks, retention time 3.483min, RSD%0.17%, peak area 674.258, RSD%90.55%；Zhan is total
The 6.544% of peak area；
No. 3 peaks, retention time 4.599min, RSD%0.29%, peak area 376.808, RSD%84.76%；Zhan is total
The 3.657% of peak area；
No. 4 peaks, retention time 10.375min, RSD%0.31%, peak area 1340.542, RSD%36.52%；It accounts for
The 13.011% of total peak area；
No. 5 peaks, retention time 17.489min, RSD%0.33%, peak area 2192.841, RSD%46.25%；It accounts for
The 21.284% of total peak area；
No. 6 peaks, retention time 19.26min, RSD%0.28%, peak area 3517.345, RSD%52.59%；Zhan is total
The 34.139% of peak area；
No. 7 peaks, retention time 25.687min, RSD%0.22%, peak area 163.423, RSD%48.73%；Zhan is total
The 1.586% of peak area；
No. 8 peaks, retention time 34.223min, RSD%0.31%, peak area 319.89, RSD%129.86%；Zhan is total
The 3.105% of peak area；
No. 9 peaks, retention time 36.628min, RSD%0.3%, peak area 376.507, RSD%83.26%；Zhan is total
The 3.654% of peak area；
No. 10 peaks, retention time 37.756min, RSD%0.3%, peak area 148.143, RSD%61.28%；Zhan is total
The 1.438% of peak area；
As it can be seen that 10 characteristic peaks in strong medicine white flower nine inner bright medicinal materials fingerprint, No. 6 compare peak for caffeic acid, and map is total
Length 60min.Wherein, the super total peak area of unimodal area 1% has 10, they are the peaks 1-13；The unimodal super total peak area of area
5% peak has 4, they are No. 2 peaks, No. 4 peaks, No. 5 peaks, No. 6 peaks；The peak of the unimodal super total peak area 10% of area has 3, it
Be No. 4 peaks, No. 5 peaks, No. 6 peaks.
Similarity evaluation: the similarity evaluation software recommended using the Chinese Pharmacopoeia committee
2004A editions, overall merit is carried out to HPLC map, similarity evaluation result is shown in Fig. 3 and table 5.
The evaluation of table 5HPLC fingerprint similarity
Remarks: S1-S13 respectively represents 13 batches of strong medicine white flower nine inner bright medicinal material test sample serial numbers.
As a result: 13 batches of strong medicine white flower nine inner bright Herbal HPLC Fingerprint similarities are all larger than 0.90.
Embodiment 3
3 methodological studies
3.1 Precision Experiment
Precision is drawn with a test solution (by numbering the white flower nine inner bright medicinal powder for being No. 1 by below " 2.3 " item
Method is prepared), by measuring method sample introduction 6 times under chromatographic condition under " 2.1 " item and " 2.4 " item, finger-print is recorded, sees Fig. 4.
It is that the relative retention time RSD value at each peak is calculated referring to peak for 0.01%-0.48% with No. 6 peaks (caffeic acid), each peak phase
To peak area RSD value in 0.3%-2.04%.Related coefficient is shown in Table 6.
6 Precision Experiment similarity result of table
As seen from Table 6, Precision Experiment related coefficient is all larger than 0.95, and similarity count results show the instrument precision
Degree is good, meets finger-print testing requirements.
3.2 stability experiment
Precision is drawn with a test solution (by numbering the white flower nine inner bright medicinal powder for being No. 1 by below " 2.3 " item
Method is prepared), after preparation 0,4,6,8,12,16, for 24 hours, by being surveyed under chromatographic condition under " 2.1 " item and " 2.4 " item
Determine method measurement, investigates the repeatability of experimental method, see Fig. 5.It is that each chromatography is calculated referring to peak with No. 6 peaks (caffeic acid)
Peak relative retention time RSD is in 0.01%-0.19%, and each peak relative peak area RSD value is in 0.05%-1.96%.Related coefficient
It is shown in Table 7.
7 stability test similarity result of table
As can be seen from Table 7, each finger-print related coefficient is all larger than 0.95, the results showed that sample solution ingredient in for 24 hours
Stablize, meets finger-print testing requirements.
3.3 repeated experiment
The white flower nine inner bright medicinal powder that number is No. 1 is taken, 6 parts is prepared by method below " 2.3 " item, presses " 2.1 " Xiang Xiase
Measuring method measures under spectral condition and " 2.4 " item, investigates experimental method repeatability, sees Fig. 6.With No. 6 peaks (caffeic acid) for reference
Each chromatographic peak relative retention time RSD is calculated in 0.04%-0.21% in peak, and each peak relative peak area RSD value exists
0.66%-1.74%.Related coefficient is shown in Table 8.
8 repetitive test similarity result of table
As seen from Table 8, repetitive test related coefficient is all larger than 0.95, and this method repeats similarity calculation as the result is shown
Property is fine, meets finger-print testing requirements.
Above description is the detailed description for the present invention preferably possible embodiments, but embodiment is not limited to this hair
Bright patent claim, it is all the present invention suggested by technical spirit under completed same changes or modifications change, should all belong to
In the covered the scope of the patents of the present invention.
Claims (7)
1. the method for building up of strong medicine white flower nine inner bright HPLC finger-print, which comprises the following steps:
(1) preparation of reference substance solution: taking caffeic acid reference substance, adds methanol dissolution that reference substance solution is made；
(2) preparation of test solution: precision weighs strong medicine white flower nine inner bright medicinal material coarse powder, adds water, and ultrasonic extraction is let cool to room
Temperature is supplied the weight of less loss with water, is shaken up, filtration, take subsequent filtrate to get；
(3) high performance liquid chromatography measures: the test solution of the reference substance solution of accurate aspiration step (1) and step (2) respectively
Each 10-20 μ l injects high performance liquid chromatograph, and measurement records chromatogram, is referring to peak, by analyzing ratio with caffeic acid chromatographic peak
More determining feature shares peak to get the white flower nine inner bright HPLC finger-print；
Wherein, chromatographic condition are as follows: using the alkyl linked silica gel of C18 as filler；It is stream with phosphoric acid solution using acetonitrile as mobile phase A
The gradient eluent of dynamic phase B composition carries out gradient elution；Detection wavelength is 300-350nm.
2. the method for building up of strong medicine white flower nine inner bright HPLC finger-print according to claim 1, which is characterized in that described
Step (1) is carried out by following operation: being taken caffeic acid reference substance, is added methanol dissolution that the reference substance of every 1ml 20 μ g containing caffeic acid is made
Solution.
3. the method for building up of strong medicine white flower nine inner bright HPLC finger-print according to claim 1, which is characterized in that described
Step (2) is carried out by following operation: precision weighs white flower nine inner bright medicinal material coarse powder 1g, adds water 20-40ml, close plug, weighed weight,
Ultrasonic extraction 20-40min, lets cool to room temperature, then weighed weight, and the weight of less loss is supplied with water, is shaken up, and filtration takes subsequent filtrate,
To obtain the final product.
4. the method for building up of strong medicine white flower nine inner bright HPLC finger-print according to claim 1, which is characterized in that described
Step (2) is carried out by following operation: precision weighs white flower nine inner bright medicinal material coarse powder 1g, adds water 20ml, close plug, and weighed weight surpasses
Sound extracts 30min, lets cool to room temperature, then weighed weight, the weight of less loss is supplied with water, is shaken up, with 0.45 μm of miillpore filter mistake
Filter, take subsequent filtrate to get.
5. the method for building up of strong medicine white flower nine inner bright HPLC finger-print according to claim 1, which is characterized in that described
The chromatographic condition of step (3) are as follows: using the alkyl linked silica gel of C18 as filler；Using acetonitrile as mobile phase A, with 0.1% phosphoric acid solution
Gradient eluent for Mobile phase B composition carries out gradient elution；Column temperature is 25 DEG C；Detection wavelength is 300-350nm；Flow velocity is
1.0ml/min；Analysis time is 60min, and sample volume is 10-20 μ l.
6. the method for building up of strong medicine white flower nine inner bright HPLC finger-print according to claim 1, which is characterized in that described
Gradient elution program is set as time gradient 0min → 5min → 10min → 25min → 40min → 60min；Corresponding gradient eluent
It is made of by following volumes ratio mobile phase A acetonitrile and 0.1% phosphoric acid solution of Mobile phase B, the percentage by volume gradient of mobile phase A
8% → 11% → 10% → 21% → 24% → 30%, Mobile phase B percentage by volume gradient 92% → 89% → 90% → 79%
→ 76% → 70%.
7. the method for building up of strong medicine white flower nine inner bright HPLC finger-print according to claim 1, which is characterized in that described
Finger-print include 10 shared peaks, retention time be respectively 2.726min, 3.483min, 4.599min, 10.375min,
17.489min、19.26min、25.687min、34.223min、36.628min、37.756min。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114113364A (en) * | 2021-10-25 | 2022-03-01 | 湖南春光九汇现代中药有限公司 | Traditional Chinese medicine network pharmacology prediction method |
| CN114371228A (en) * | 2021-11-17 | 2022-04-19 | 西南民族大学 | Method for distinguishing pseudodongfeng grass or dongfeng grass as Zhuang medicinal material |
| CN115060841A (en) * | 2022-07-28 | 2022-09-16 | 吉首大学 | HPLC fingerprint identification method for paulownia leaves |
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| CN114371228B (en) * | 2021-11-17 | 2023-05-23 | 西南民族大学 | Method for distinguishing strong medicinal materials false east wind grass or east wind grass |
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| CN115060841B (en) * | 2022-07-28 | 2023-12-22 | 吉首大学 | HPLC fingerprint identification method for paulownia tomentosa leaves |
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