CN109900827A - Survey the methods for commenting method to identify prepared fleece flower root based on one more - Google Patents
Survey the methods for commenting method to identify prepared fleece flower root based on one more Download PDFInfo
- Publication number
- CN109900827A CN109900827A CN201910232891.6A CN201910232891A CN109900827A CN 109900827 A CN109900827 A CN 109900827A CN 201910232891 A CN201910232891 A CN 201910232891A CN 109900827 A CN109900827 A CN 109900827A
- Authority
- CN
- China
- Prior art keywords
- flower root
- prepared fleece
- fleece flower
- mobile phase
- rheum emodin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention discloses the methods for surveying more other prepared fleece flower roots of criticism based on one, check through methodology validation and provincial inspection body, and prepared fleece flower root sample reappears, and show that the method drafted is feasible.One be put forward for the first time surveys the data Analysis of check-up for commenting method to pass through for four years more, it is investigated from laboratory to medicine materical crude slice company, from same a collection of health product Preparata, the investigation of concocted time is carried out to traditional prepared fleece flower root " nine steam nine systems ", the F value limit obtained is feasible, using rheum emodin as reference substance, statistics indicate that F value is to process complete prepared fleece flower root no more than 0.6, because F value is in stable state below 0.6；Value >=1.0 F are health product characteristic, the incomplete prepared fleece flower root sample of processing of the F value between 0.6~1.0.The present invention solves prepared fleece flower root and cannot distinguish between whether process complete problem from appearance character.A survey simultaneously comments method to examine ingredient low, provides good support for the safe handling of bulk medicinal materials prepared fleece flower root.
Description
Technical field
The invention belongs to TCD identificafion technical fields, and in particular to a kind of to survey the sides for commenting method to identify prepared fleece flower root based on one more
Method.
Background technique
The fleece-flower root be polygonum multiflorum thunb PolygonummultiflorumThunb. dried root, have removing toxic substances,
Disappear carbuncle, preventing malaria, relax bowel and defecation the effect of.Prepared fleece flower root is the processed product of the fleece-flower root, and prepared fleece flower root and fleece-flower root effect are completely not
Same: prepared fleece flower root is widely used as bulk medicinal materials in tcm clinical practice, prepared fleece flower root have nourishing liver and kidney, benefiting essence-blood, black beard and hair,
Strengthening the bones and muscles, the effect of changing turbid lipid-loweringing；The effect of fleece-flower root has removing toxic substances, and disappear carbuncle, preventing malaria, relax bowel and defecation.
" collected statements on the herbal foundation ", which is recorded, " to be made non-nine times, its poison of not getting into bed.Non- semen sojae atricolor does not kill its gesture ".The concocting method of prepared fleece flower root
Referring to " Chinese Pharmacopoeia " versions in 2010 and " Beijing's Chinese medicine concocted specification ", the toxicity of multiflower knotweed tuber prepared product is with concocted time
Increase and significantly reduce.There is related seminar to report, in 30 batches of prepared fleece flower roots for studying its purchase, experimental result is shown
14 batches of toxicity prompts these processed products processing attenuation not yet in effect, Ke Nengzeng close to the control medicinal material of even higher than Radix Polygoni Multiflori
The risk for adding clinical hepatic injury seriously threatens patient clinical drug safety.However, current edition standards of pharmacopoeia prepared fleece flower root and what head
Black inspection project is similar, cannot distinguish between whether prepared fleece flower root processes completely.Prepared fleece flower root hepatotoxicity wind agitation report is continuously increased: in retrieval
National IP Network, nearly 5 years Document systems, 686 hepatotoxicity wind agitation adverse reactions.Therefore, incomplete prepared fleece flower root is processed from appearance character
It not can determine that whether prepared fleece flower root processes completely, thus be different from the identification of certified products and non-certified products.
The strong teacher seminar in Luoding assumed responsibility for the fleece-flower root in 2015 and quality analysis project is commented by the state of prepared fleece flower root, passed through
The documents and materials compared with are tested, find the fleece-flower root in concocting process, with the increase of concocted time, methods of glycosides is declining,
Corresponding aglycon ingredient is increasing.2016, by the way that fleece-flower root health product, prepared fleece flower root data Analysis of check-up, Luoding is waited by force
" tuber of multiflower knotweed rule ", i.e. rheum emodin -8-O- have been put forward for the first time in " Chinese medicine " the 10th phase " fleece-flower root quality analysis " paper of volume 39
The content summation and rheum emodin, Physcion content of β-D- glucopyranoside, Physcion -8-O- β-D- glucopyranoside
The ratio F of summation is fleece-flower root health product more than or equal to 1.0, otherwise is prepared fleece flower root.
Judged according to above-mentioned rule, when F value is less than 1.0, judgement should be prepared fleece flower root, still, with the seminar
Further research in recent years can not accurately determine whether it is to process complete prepared fleece flower root, big gun when finding F value less than 1.0
The hepatotoxicity wind agitation for making incomplete prepared fleece flower root still influences the extensive use of the drug.Therefore, existing method can not still solve
The certainly identification problem of prepared fleece flower root.
Summary of the invention
In order to overcome the disadvantages of the above prior art, survey the purpose of the present invention is to provide one kind based on one comments method to identify more
The method of prepared fleece flower root, being able to solve the prior art can not judge whether prepared fleece flower root processes complete problem.
In order to achieve the above object, the present invention is achieved by the following scheme:
Survey the methods for commenting method to identify prepared fleece flower root based on one the invention discloses a kind of more, comprising the following steps:
1) calculate relative correction factor: precision measures rheum emodin, Physcion, rheum emodin -8-O- β-D- glucopyra
Glycosides and Physcion -8-O- β-D- glucopyranoside, are prepared four kinds of reference substance solutions respectively, then use external standard method,
The standard curve of four reference substances is obtained, using rheum emodin as internal standard, calculates separately out Physcion, rheum emodin -8-O- β-D-
The relative correction factor of glucopyranoside and Physcion -8-O- β-D- glucopyranoside；
2) calculate each component content: prepared fleece flower root powder to be detected being taken to prepare test solution, using rheum emodin as pair
Reference substance solution is prepared according to product, gradient elution is carried out using high performance liquid chromatography, chromatogram is obtained, with rheum emodin reference substance
Peak area is control, and rheum emodin first is calculated in the relative correction factor for the tie element being then calculated according to step 1)
The content of ether, rheum emodin -8-O- β-D- glucopyranoside and Physcion -8-O- β-D- glucopyranoside；
3) it calculates F value and judges whether prepared fleece flower root to be detected processes completely, F value is calculated by formula (1):
F=rheum emodin -8-O- β-D- glucopyranoside content+Physcion -8-O- β-D- glucopyranoside content/big
Flavine content+Physcion content (1)
Then have:
As F≤0.6, prepared fleece flower root to be detected is judged to process complete prepared fleece flower root；
When F >=1.0, judge prepared fleece flower root to be detected for fleece-flower root health product；
As 0.6 < F < 1, prepared fleece flower root to be detected is judged to process incomplete prepared fleece flower root.
Preferably, the variation of F value and Preparation process time correlation, fleece-flower root health product concocted time >=8h, value≤0.6 F.
Preferably, high-efficient liquid phase chromatogram condition are as follows: using octadecylsilane chemically bonded silica as filler；It is flowing with acetonitrile
Phase A, using 0.1% phosphate aqueous solution as Mobile phase B, Detection wavelength 254nm.
It is further preferred that the variation ratio of mobile phase A and Mobile phase B is such as when using Gradient Elution
Under:
0~8min, mobile phase A: 18%~30%, Mobile phase B: 70%~82%；
8~24min, mobile phase A: 30%~36%, Mobile phase B: 64%~70%；
24~28min, mobile phase A: 36%~80%, Mobile phase B: 20%~64%；
28~39min, mobile phase A: 80%~95%, Mobile phase B: 5%~20%；
39~40min, mobile phase A: 18%~95%, Mobile phase B: 5%~82%；
40~45min, mobile phase A: 18%, Mobile phase B: 82%.
Preferably, step 1) the relative correction factor calculation method are as follows: using rheum emodin as internal standard compound, as the following formula (2)
Calculate Physcion, rheum emodin -8-O- β-D- glucopyranoside and Physcion -8-O- β-D- glucopyranoside
Relative correction factor fkm；
Wherein, AkFor rheum emodin peak area；WkFor rheum emodin concentration；AmFor the peak area of other components to be measured；WmFor other
The concentration of component to be measured；K is rheum emodin, and m is other components to be measured, fkFor the correction factor of rheum emodin, fmFor other components to be measured
Correction factor.Herein, other components to be measured refer to Physcion, rheum emodin -8-O- β-D- glucopyranoside and big
Flavine methyl ether -8-O- β-D- glucopyranoside.
It is further preferred that rheum emodin, Physcion, rheum emodin -8-O- β-D- glucopyranoside and Physcion -
The relative retention time and relative correction factor of 8-O- β-D- glucopyranoside are as follows:
Preferably, in step 2), test solution is that 50mL methanol, heating is added to 1g prepared fleece flower root powder to be detected
Reflow treatment 1h, it is cooling to be made.
Preferably, in step 2), reference substance solution is to be dissolved in rheum emodin concentration is made in methanol as the molten of 30 μ g/ml
Liquid.
Compared with prior art, the invention has the following advantages:
It is disclosed by the invention to survey the methods for commenting method to identify prepared fleece flower root based on one more, by largely testing accumulation and data
Analysis of check-up is investigated from laboratory to medicine materical crude slice company, from same a collection of health product Preparata, to " the nine of traditional prepared fleece flower root
The investigation that nine system of steaming " carries out concocted time, has obtained the feasible limit of F value, using rheum emodin as reference substance, statistics indicate that F value
It is to process complete prepared fleece flower root no more than 0.6, because F value is in stable state below 0.6；It makes a living value >=1.0 F
Product characteristic, the incomplete prepared fleece flower root sample of processing of the F value between 0.6~1.0.This method being capable of very specific system of identification
Whether the fleece-flower root can be processed completely with accurate judgement prepared fleece flower root, to guarantee that bulk medicinal materials prepared fleece flower root is used in clinical safety
Provide effective identification means.Meanwhile one reference substance of rheum emodin is used only in this method, inspection cost is very low, saves money
Source.
Detailed description of the invention
Fig. 1 is that 6 batches of fleece-flower root sample F values change line chart.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, below in conjunction in the embodiment of the present invention
Attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only
The embodiment of a part of the invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people
The model that the present invention protects all should belong in member's every other embodiment obtained without making creative work
It encloses.
It should be noted that description and claims of this specification and term " first " in above-mentioned attached drawing, "
Two " etc. be to be used to distinguish similar objects, without being used to describe a particular order or precedence order.It should be understood that using in this way
Data be interchangeable under appropriate circumstances, so as to the embodiment of the present invention described herein can in addition to illustrating herein or
Sequence other than those of description is implemented.In addition, term " includes " and " having " and their any deformation, it is intended that cover
Cover it is non-exclusive include, for example, the process, method, system, product or equipment for containing a series of steps or units are not necessarily limited to
Step or unit those of is clearly listed, but may include be not clearly listed or for these process, methods, product
Or other step or units that equipment is intrinsic.
The invention will be described in further detail with reference to the accompanying drawing:
One, existing prepared fleece flower root standard and fleece-flower root health product quality standard compare
Standard comparing is shown in Table 1.
1 fleece-flower root of table is compared with prepared fleece flower root current standard
In terms of standard comparing, examine project similar, the fleece-flower root and prepared fleece flower root contain combined anthraquinone and dissociated anthraquinone, no
Big with the place of production fleece-flower root and prepared fleece flower root content difference, the assay project of part health product, which also complies with, to be measured containing for prepared fleece flower root
Fixed limit degree cannot effectively distinguish whether prepared fleece flower root processes completely.
Two, a survey comments method to identify prepared fleece flower root
1, instrument: BP211D electronic analytical balance (Sartorius AG)；(Switzerland's plum Teller-support benefit is public by ME204
Department)；LC-2030C 3D high performance liquid chromatograph (Japanese Shimadzu Corporation)；(Japanese Shimadzu is public for LC-30AD high performance liquid chromatograph
Department)；II high performance liquid chromatograph of Agilent 1260Infinity (Agilent company of the U.S.)；Empower chromatography working software.
2, material and reagent: rheum emodin reference substance (110756-201512, purity 98.7%), Physcion reference substance
(110758-201415, purity 99.1%), is provided by National Institute for Food and Drugs Control；Rheum emodin -8-O- β-D- pyrans
Heteroside reference substance (purity 97.0%) and Physcion -8-O- β-D- glucopyranoside reference substance (purity 98%) are purchased from upper
Hai Tongtian Biotechnology Ltd.；Acetonitrile, methanol are chromatographically pure, and water is ultrapure water；Remaining reagent is that analysis is pure.Second
Nitrile is chromatographically pure, other are pure to analyze, and water is deionized water.
3, sample source: prepared fleece flower root, fleece-flower root sample are drunk according to national special Sampling plan and 2020 editions Chinese Pharmacopoeias
Piece revises task, is inspected by random samples according to four annex 0211 of " Chinese Pharmacopoeia " version in 2015 " medicinal material and medicine materical crude slice sampling method ".Every batch of
Medicine materical crude slice is at least sampled 150g.In addition to Hong Kong, Macao, Taiwan, 22 provinces, 5 autonomous regions, 4 municipalities directly under the Central Government totally 31 are extracted altogether
Provincial administrative area fleece-flower root medicine materical crude slice 66 batches, it is related to manufacturing enterprise's number 51, is distributed in 19 provinces；Prepared fleece flower root medicine materical crude slice 106 batches,
It is related to manufacturing enterprise's number 100, is distributed in 26 provinces.
4, method
1) test solution is prepared: this product powder (crossing No. four sieves) about 1g is taken, it is accurately weighed, and it sets in stuffed conical flask, it is accurate
Methanol 50ml is added, weighed weight is heated to reflux 1h, takes out, lets cool, take subsequent filtrate as test sample.Separately rheum emodin is taken to compare
Product, it is accurately weighed, add methanol that the solution that every 1ml contains 30 μ g is made, as reference substance solution.
2) high-efficient liquid phase chromatogram condition: according to high performance liquid chromatography (four (general rules of " Chinese Pharmacopoeia " version in 2015
0512) it) tests, using octadecylsilane chemically bonded silica as filler；Using acetonitrile as mobile phase A, it is with 0.1% phosphate aqueous solution
Mobile phase B, the regulation according to the form below carry out gradient elution, Detection wavelength 254nm.Number of theoretical plate should not be low by rheum emodin peak calculating
In 5000.
When using Gradient Elution, the variation ratio of mobile phase A and Mobile phase B is as follows:
0~8min, mobile phase A: 18%~30%, Mobile phase B: 70%~82%；
8~24min, mobile phase A: 30%~36%, Mobile phase B: 64%~70%；
24~28min, mobile phase A: 36%~80%, Mobile phase B: 20%~64%；
28~39min, mobile phase A: 80%~95%, Mobile phase B: 5%~20%；
39~40min, mobile phase A: 18%~95%, Mobile phase B: 5%~82%；
40~45min, mobile phase A: 18%, Mobile phase B: 82%.
3) measurement and calculating: each 10 μ l of above-mentioned test solution and control solution is taken, liquid chromatograph is injected, records color
Spectrogram.It is control with the peak area of rheum emodin reference substance, the corresponding correction factor of according to the form below calculates Physcion, big respectively
The content of flavine -8-O- β-D- glucopyranoside, Physcion -8-O- β-D- glucopyranoside, with ingredient chromatographic peak to be measured
With the peak position of Physcion, rheum emodin -8-O- β-D- glucopyranoside, Physcion -8-O- β-D- glucopyranoside,
Relative retention time should be within ± 5% range of specified value (if relative retention time deviates more than 5%, with rheum emodin and what
Tuber of multiflower knotweed control medicinal material or the confirmation of corresponding reference substance).
4) calculating of relative correction factor:
The preparation of reference substance: precision weighs Physcion reference substance 10.08mg, is placed in 100mL measuring bottle, methanol is added to make
Dissolution, is settled to scale, shakes up, as No. 1 stock solution；Precision weighs rheum emodin reference substance 7.20mg, rheum emodin -8-O- β-D-
Glucopyranoside 11.16mg, Physcion -8-O- β-D- glucopyranoside 9.92mg are placed in 100mL measuring bottle, add methanol molten
Solution, is settled to scale, shakes up, as No. 2 stock solutions.No. 1 stock solution of accurate measurement, No. 2 each 1mL of stock solution are placed in 50mL respectively
In measuring bottle, with methanol dilution to scale, shake up, as No. 1 reference substance solution；It is accurate respectively to measure No. 1 stock solution, No. 2 storages
Standby liquid 2mL is placed in 50mL measuring bottle, with methanol dilution to scale, as No. 2 reference substance solutions；It is accurate respectively to measure No. 1 deposit
Liquid, No. 2 each 2mL of stock solution are placed in 25mL measuring bottle, use methanol constant volume to scale as No. 3 reference substance solutions；It is accurate respectively to measure 1
Number, No. 2 two kinds of each 1mL of stock solution are placed in 10ml measuring bottle, with methanol dilution to scale, as No. 4 reference substance solutions；Essence respectively
Close to measure No. 1, No. 2 two kinds of each 2mL of stock solution are respectively placed in 10mL measuring bottle, with methanol dilution to scale, as No. 5 reference substances
Solution；Accurate respectively to measure No. 1, No. 2 two kinds of each 2mL of stock solution are placed in 5mL measuring bottle, with methanol dilution to scale, as 6
Number reference substance solution；Precision measures No. 1, and No. 2 each 5ml of stock solution are placed in 10mL measuring bottle, with methanol dilution to scale, as 7
Number reference substance solution.
The preparation of test solution: taking test sample appropriate, crushes, and crosses No. four sieves, and accurately weighed test sample powder 1g sets three
In the bottle of angle, methanol 50mL is added in precision, and weighing is heated to reflux 1 hour, anti-cold, and the weight of less loss is supplied with methanol, filters, takes
Subsequent filtrate is as test solution.
The range of linearity: precision draws each 10 μ L of above-mentioned No. 1,2,3,4,5,6,7 mixed reference substance solutions and injects liquid chromatogram
Instrument is measured by above-mentioned chromatographic condition, records chromatographic peak area, is vertical sit with peak area (Y) with sample volume (X, μ g) for abscissa
Mark draws standard curve.4 kinds of standard curves are linear good in the linear range respectively, are shown in Table 2:
The standard curve of 2 four kinds of ingredients of table
Precision draws No. 6 10 μ L of mixed reference substance solution, sample introduction 3 times, records chromatographic peak area and retention time.With rheum officinale
Element be internal standard, using rheum emodin as internal standard, as the following formula (2) calculate Physcion, rheum emodin -8-O- β-D- glucopyranoside,
The relative correction factor of Physcion -8-O- β-D- glucopyranoside.
Wherein, AkFor rheum emodin peak area；WkFor rheum emodin concentration；AmFor the peak area of other components to be measured；WmFor other
The concentration of component to be measured；K is rheum emodin, and m is other components to be measured, fkFor the correction factor of rheum emodin, fmFor other components to be measured
Correction factor.As a result Physcion, rheum emodin -8-O- β-D- glucopyranoside, Physcion -8-O- β-D- pyrans
The relative correction factor of glucoside is 0.92,2.27,2.04 respectively.With rheum emodin retention time for 1.00, rheum officinale is calculated to obtain
The opposite reservation of plain methyl ether, rheum emodin -8-O- β-D- glucopyranoside, Physcion -8-O- β-D- glucopyranoside
Time is 1.11,0.47,0.61 respectively.
Relative retention time and relative correction factor see the table below 3:
3 property of table is to retention time and relative correction factor
Meanwhile by precision test, stability test, repetitive test and recovery test, meet equipment essence
Density requirements have good stability at room temperature, and repeatability is good, and measurement result is stablized.
5) correction factor durability is investigated
Investigate different sampling volumes, different chromatographic columns, influence of the different instruments to correction factor, RSD is respectively less than
3%, it is shown in Table 4 and table 5:
The correction factor of the different sampling volumes of table 4
The correction factor of the different instrument difference chromatographic columns of table 5
It in summary it can be seen, relative correction factor durability of the invention preferably passes through durability experiment test, as a result may be used
It leans on.
6) F value calculates:
F=rheum emodin -8-O- β-D- glucopyranoside content+Physcion -8-O- β-D- glucopyranoside content/big
Flavine content+Physcion content (1)
As F≤0.6, prepared fleece flower root to be detected is judged to process complete prepared fleece flower root；
When F >=1.0, judge prepared fleece flower root to be detected for fleece-flower root health product；
As 0.6 < F < 1, prepared fleece flower root to be detected is judged to process incomplete prepared fleece flower root.
According to the method described above, it is as follows to carry out specific experiment:
Commercially 10 batches of fleece-flower root health products, steam the prepared fleece flower root sample of different time respectively, and measurement result is shown in
Table 6:
Table 6 one is surveyed comments method compared with external standard method F value result more
Table 6 according between group in organizing the results show that analyze, and method and external standard method are commented in side of the invention more, and there was no significant difference,
But one reference substance of rheum emodin is used only, reference substance Expenses of laboratory examination has greatly saved detection funds less than 100 yuan.
Embodiment 1 (determination of F value limit)
6 batches of representative fleece-flower root health products are chosen respectively, and for F value 1.03~9.61, health product and decoction of black soybean profit stewing 8 are small
When, different time (0.2-0.4MPa) is steamed by Shaanxi Guanji hall Pharmaceutical Group limited liability company Preparation process.By foundation
Method is measured, and the results are shown in Table 7:
76 batches of fleece-flower root health product steaming times of table and F value
In conjunction with from above-mentioned table 7 and Fig. 1, it can be seen that the variation of F value is directly related with the Preparation process time, in the fleece-flower root
After health product steams 8h, i.e., F value is 0.6 hereinafter, F value is more and more stable.Therefore the present invention proposes the limit that F value is not more than 0.6, as
Process complete prepared fleece flower root.
Embodiment 2 (verifying of F value limit)
Data generaI investigation is carried out to 66 batches of fleece-flower root health products, the range of F value is verified, the results are shown in Table 8:
8 66 batches of fleece-flower root health product F value measurement results of table
By the data Analysis of check-up to 66 batches of fleece-flower root health product F values, value >=1.0 F are found.Illustrate that value >=1.0 F are health product
Characteristic, and the effect of health product is with processed product, is entirely different, and documents and materials are proved health product and process incomplete prepared fleece flower root
Hepatotoxic damage is significantly higher than and processes complete prepared fleece flower root.
Embodiment 3 (verifying of F value limit)
Data generaI investigation is carried out to 106 batches of prepared fleece flower roots, the range of analysis and verifying F value the results are shown in Table 9:
9 106 batches of prepared fleece flower root health product F value measurement results of table
By the limit 0.6 of the F value of foundation, it can clearly distinguish prepared fleece flower root sample in the market and process situation.By what is drafted
Method, qualification rate 84.9%, 10 batches of samples have health product characteristic, and 6 batches of prepared fleece flower roots are to process not exclusively.
Embodiment 4
By 3 batches, prepared fleece flower root sample send Heilungkiang food and medicine examine detection the result of the method for the present invention is answered
Core detection, according to the survey report (report number be HL2017Q4289, HL2017Q4290 and HL2017Q4290) provided,
It is able to confirm that the favorable reproducibility of the method for the present invention.
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press
According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention
Protection scope within.
Claims (8)
1. surveying the methods for commenting method to identify prepared fleece flower root based on one more, which comprises the following steps:
1) calculate relative correction factor: precision measure rheum emodin, Physcion, rheum emodin -8-O- β-D- glucopyranoside and
Physcion -8-O- β-D- glucopyranoside, is prepared four kinds of reference substance solutions respectively, then uses external standard method, obtains
The standard curve of four reference substances calculates separately out Physcion, rheum emodin -8-O- β-D- pyrans using rheum emodin as internal standard
The relative correction factor of heteroside and Physcion -8-O- β-D- glucopyranoside；
2) it calculates each component content: taking prepared fleece flower root powder to be detected to prepare test solution, using rheum emodin as reference substance
Reference substance solution is prepared, gradient elution is carried out using high performance liquid chromatography, chromatogram is obtained, with the peak face of rheum emodin reference substance
Product is control, the relative correction factor for the tie element being then calculated according to step 1), and Physcion, big is calculated
The content of flavine -8-O- β-D- glucopyranoside and Physcion -8-O- β-D- glucopyranoside；
3) it calculates F value and judges whether prepared fleece flower root to be detected processes completely, F value is calculated by formula (1):
F=rheum emodin -8-O- β-D- glucopyranoside content+Physcion -8-O- β-D- glucopyranoside content/rheum emodin
Content+Physcion content (1)
Then have:
As F≤0.6, prepared fleece flower root to be detected is judged to process complete prepared fleece flower root；
When F >=1.0, judge prepared fleece flower root to be detected for fleece-flower root health product；
As 0.6 < F < 1, prepared fleece flower root to be detected is judged to process incomplete prepared fleece flower root.
2. according to claim 1 survey the methods for commenting method to identify prepared fleece flower root based on one more, which is characterized in that the change of F value
Change and Preparation process time correlation, fleece-flower root health product concocted time >=8h, value≤0.6 F.
3. according to claim 1 survey the methods for commenting method to identify prepared fleece flower root based on one more, which is characterized in that efficient liquid phase
Chromatographic condition are as follows: using octadecylsilane chemically bonded silica as filler；Using acetonitrile as mobile phase A, it is with 0.1% phosphate aqueous solution
Mobile phase B, Detection wavelength 254nm.
4. according to claim 3 survey the methods for commenting method to identify prepared fleece flower root based on one more, which is characterized in that using efficient
When liquid chromatogram gradient elution, the variation ratio of mobile phase A and Mobile phase B is as follows:
0~8min, mobile phase A: 18%~30%, Mobile phase B: 70%~82%；
8~24min, mobile phase A: 30%~36%, Mobile phase B: 64%~70%；
24~28min, mobile phase A: 36%~80%, Mobile phase B: 20%~64%；
28~39min, mobile phase A: 80%~95%, Mobile phase B: 5%~20%；
39~40min, mobile phase A: 18%~95%, Mobile phase B: 5%~82%；
40~45min, mobile phase A: 18%, Mobile phase B: 82%.
5. according to claim 1 survey the methods for commenting method to identify prepared fleece flower root based on one more, which is characterized in that step 1) institute
State relative correction factor calculation method are as follows: using rheum emodin as internal standard compound, (2) calculate Physcion, rheum emodin -8- as the following formula
The relative correction factor f of O- β-D- glucopyranoside and Physcion -8-O- β-D- glucopyranosidekm；
Wherein, AkFor rheum emodin peak area；WkFor rheum emodin concentration；AmFor the peak area of other components to be measured；WmIt is to be measured for other
The concentration of component；K is rheum emodin, and m is other components to be measured, fkFor the correction factor of rheum emodin, fmFor the school of other components to be measured
Positive divisor.
6. according to claim 5 survey the methods for commenting method to identify prepared fleece flower root based on one more, which is characterized in that rheum emodin,
The opposite reservation of Physcion, rheum emodin -8-O- β-D- glucopyranoside and Physcion -8-O- β-D- glucopyranoside
Time and relative correction factor are as follows:
7. according to claim 1 survey the methods for commenting method to identify prepared fleece flower root based on one more, which is characterized in that step 2)
In, test solution is that 50mL methanol is added to 1g prepared fleece flower root powder to be detected, is heated to reflux processing 1h, cooling to be made.
8. according to claim 1 survey the methods for commenting method to identify prepared fleece flower root based on one more, which is characterized in that step 2)
In, reference substance solution is that rheum emodin is dissolved in the solution for being made that concentration is 30 μ g/ml in methanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910232891.6A CN109900827B (en) | 2019-03-26 | 2019-03-26 | Method for identifying radix polygoni multiflori preparata based on one-test-multiple evaluation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910232891.6A CN109900827B (en) | 2019-03-26 | 2019-03-26 | Method for identifying radix polygoni multiflori preparata based on one-test-multiple evaluation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109900827A true CN109900827A (en) | 2019-06-18 |
| CN109900827B CN109900827B (en) | 2022-02-11 |
Family
ID=66953448
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910232891.6A Active CN109900827B (en) | 2019-03-26 | 2019-03-26 | Method for identifying radix polygoni multiflori preparata based on one-test-multiple evaluation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109900827B (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1879756A (en) * | 2006-04-30 | 2006-12-20 | 石药集团中奇制药技术（石家庄）有限公司 | Quality control method of kidney-replenishing blood-nourishing soft capsule |
| CN101081251A (en) * | 2006-05-29 | 2007-12-05 | 广州中医药大学第二附属医院 | Polygonum multiflorum thunb processing method |
| US20090092697A1 (en) * | 2003-08-22 | 2009-04-09 | National Yang-Ming University | Extracts of polygonum multiflorum thunb., and preparation process and uses of the same |
| CN101554410A (en) * | 2009-04-22 | 2009-10-14 | 西南交通大学 | Quality control method of fresh fleece flower root and prepared fleece flower root |
| CN101574439A (en) * | 2009-05-18 | 2009-11-11 | 唐弟光 | Method for controlling quality of Runzao Zhiyang tablet |
| CN103018367A (en) * | 2012-12-13 | 2013-04-03 | 贵州大学 | Method for determining content of lecithin component in polygonum multiflorum medicinal material |
| WO2013074801A1 (en) * | 2011-11-18 | 2013-05-23 | Stemtech International, Inc. | Use of foti to enhance stem cell mobilization and proliferation |
| CN104655742A (en) * | 2014-01-06 | 2015-05-27 | 广西梧州三鹤药业有限公司 | Method for determining content of ferulic acid in pill |
| CN107490645A (en) * | 2017-07-03 | 2017-12-19 | 中国人民解放军第三〇二医院 | A kind of safe mass control method of prepared fleece flower root and application |
-
2019
- 2019-03-26 CN CN201910232891.6A patent/CN109900827B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090092697A1 (en) * | 2003-08-22 | 2009-04-09 | National Yang-Ming University | Extracts of polygonum multiflorum thunb., and preparation process and uses of the same |
| CN1879756A (en) * | 2006-04-30 | 2006-12-20 | 石药集团中奇制药技术（石家庄）有限公司 | Quality control method of kidney-replenishing blood-nourishing soft capsule |
| CN101081251A (en) * | 2006-05-29 | 2007-12-05 | 广州中医药大学第二附属医院 | Polygonum multiflorum thunb processing method |
| CN101554410A (en) * | 2009-04-22 | 2009-10-14 | 西南交通大学 | Quality control method of fresh fleece flower root and prepared fleece flower root |
| CN101574439A (en) * | 2009-05-18 | 2009-11-11 | 唐弟光 | Method for controlling quality of Runzao Zhiyang tablet |
| WO2013074801A1 (en) * | 2011-11-18 | 2013-05-23 | Stemtech International, Inc. | Use of foti to enhance stem cell mobilization and proliferation |
| CN103018367A (en) * | 2012-12-13 | 2013-04-03 | 贵州大学 | Method for determining content of lecithin component in polygonum multiflorum medicinal material |
| CN104655742A (en) * | 2014-01-06 | 2015-05-27 | 广西梧州三鹤药业有限公司 | Method for determining content of ferulic acid in pill |
| CN107490645A (en) * | 2017-07-03 | 2017-12-19 | 中国人民解放军第三〇二医院 | A kind of safe mass control method of prepared fleece flower root and application |
Non-Patent Citations (6)
| Title |
|---|
| THANH-TAM等: "Enhanced production of phenolic compounds in hairy root cultures of Polygonum multiflorum and its metabolite discrimination using HPLC and FT-IR methods", 《APPLIED MICROBIOLOGY AND BIOTECHNOLOGY》 * |
| 何美丹等: "双波长融合HPLC法评价制何首乌质量方法研究", 《亚太传统医药》 * |
| 罗定强等: "何首乌与制何首乌的质量分析", 《中药材》 * |
| 赵余庆等: "《食疗与保健食品原料功能因子手册》", 31 January 2013, 中国医药科技出版社 * |
| 陈庆堂等: "何首乌炮制过程中5种化学成分的含量变化", 《中国实验方剂学杂志》 * |
| 陈艳: "何首乌炮制程度与内在质量相关性的研究", 《中国优秀硕士学位论文全文数据库》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109900827B (en) | 2022-02-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111443137B (en) | Method for detecting content of gan Jiang Ling Zhu soup | |
| CN109406645A (en) | A kind of Antisathmatic oral liquid for child epheday intermedia, the detection method for frying semen armeniacae amarae, Radix Glycyrrhizae, radix scutellariae | |
| CN106198782A (en) | A kind of can realize the content analysis of 18 components in Folium Ilicis and the method for quality control of similarity evaluation simultaneously | |
| CN106124639A (en) | The multicomponent content assaying method of Eucommia ulmoides | |
| CN106404942B (en) | A kind of construction method and its standard finger-print of kidney-healing particle finger-print | |
| CN104062374B (en) | The detection method of the Chinese medicine composition of invigorating Qi and tonifying kidney | |
| CN105067747B (en) | The detection method of Styrax flavour of a drug ingredients fingerprint and its application in a kind of Heart pill of Musk | |
| CN104280493A (en) | Detection method of radix isatidis drug | |
| CN106802327B (en) | A method of it establishing youngster and rushes down the finger-print for stopping pharmaceutical preparation | |
| CN104730158B (en) | A kind of content assaying method of JIAWEI HUOXIANG ZHENGQI RUANJIAONANG | |
| CN106501396B (en) | A kind of detection method of hemorrhoid medicine index components content | |
| CN104316613A (en) | Method for establishing fingerprint spectrum of wind-dispelling and detoxifying capsules | |
| CN112666277B (en) | HPLC (high Performance liquid chromatography) characteristic spectrum construction and detection method for rhizoma cyperi medicinal materials, decoction pieces, standard decoction and formula granules | |
| CN104155383B (en) | The detection method of blue or green Pu granule | |
| CN106290645B (en) | A kind of construction method and its standard finger-print of Lhasa rhubarb finger-print | |
| CN110568111B (en) | Method for detecting oligosaccharide in morinda officinalis formula particles | |
| CN107389830B (en) | A kind of hemorrhoid complicated by anal fistula smokes the quality determining method of lotion | |
| CN109900827A (en) | Survey the methods for commenting method to identify prepared fleece flower root based on one more | |
| CN106370750A (en) | Content detection method for hesperidin, naringin and neohesperidin in endothelium-corneum-gigeriae-galli and mangnolia-officinalis accumulation dispersing particles | |
| CN106770785B (en) | A method of establishing the finger-print of madder rattan medicinal material | |
| CN109709222A (en) | A kind of component detection method of cold drug and compound cold drug | |
| CN104597168B (en) | Ramulus Mori refines decoction pieces content assaying method | |
| CN107449848A (en) | A kind of method of La Ruia extracts in discriminating cosmetic material | |
| CN106168608A (en) | The detection method of EGCG content in a kind of tea polyphenols | |
| CN108008023A (en) | A kind of detection method of brain-tonifying and kidney-nourishing Chinese medicine composition |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |