CN109946394A - The quality determining method of the HPLC characteristic spectrum and its construction method of the coptis and application, coptis - Google Patents
The quality determining method of the HPLC characteristic spectrum and its construction method of the coptis and application, coptis Download PDFInfo
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Abstract
The present invention provides the quality determining methods of the HPLC characteristic spectrum and its construction method of a kind of coptis and application, coptis, belong to characteristic spectrum technical field.The present invention provides a kind of HPLC characteristic spectrums of coptis, HPLC characteristic spectrum includes 8 characteristic peaks, it is control peak with No. 8 peaks jamaicin peak, the relative retention time of each characteristic peak are as follows: No. 1 peak: relative retention time 0.095, No. 2 peaks: relative retention time 0.359, No. 3 peaks: relative retention time 0.526, No. 4 peaks: relative retention time 0.551, No. 5 peaks: relative retention time 0.581, No. 6 peaks: relative retention time 0.653, No. 7 peaks: relative retention time 0.888, No. 8 peaks: relative retention time 1.000, each peak relative retention time, relative peak area is in 5% range.This feature map can be used for controlling the quality of coptis, strong operability.
Description
Technical field
The invention belongs to characteristic spectrum technical fields, and in particular to a kind of the HPLC characteristic spectrum and its construction method of the coptis
With the quality determining method of application, coptis.
Background technique
Standard decoction system follows traditional Chinese medical theory, standardizes according to clinical decoction decocting method and decocts, and is separated by solid-liquid separation, through suitable
Suitable method is dry to be made, as measure Chinese medicinal granule whether the marker almost the same with clinical decoction.Standard soup
Agent is made respectively by being no less than 15 batches of raw medicinal materials, calculates related mean value, and provides its acceptable range that makes a variation.Chinese medicine is matched
All studies of pharmacy of square particle must be compared with standard decoction, to guarantee and standard decoction quality conformance.Therefore, it marks
The quality standard research of quasi- decoction is particularly important to judge later period granule technological standards and quality standard, and standard decoction
Characteristic spectrum and amount matter transfer study are even more the most important thing.
The coptis is as common large herbal species, and the coptis has effects that following: heat-clearing and damp-drying drug, purging fire for removing toxin；For wet
Hot feeling of fullness, vomiting acid regurgitation, dysentery, jaundice, unconsciousness due to high fever, heart-fire hyperactivity, dysphoria and insomnia, blood-head tells nosebleed, hot eyes, toothache are quenched one's thirst,
Carbuncle swells furunculosis；Eczema, wet sore, purulent ear canal are controlled outside；It is burning hot that prepared RHIZOMA COPTIDIS with vino is apt to the clear part of the body cavity above the diaphragm housing the heart and lungs.For hot eyes, aphtha；Prepared RHIZOMA COPTIDIS with rhizoma zingiberis recens juice clearing stomach and
Stomach preventing or arresting vomiting；It is mutually tied for fever and chills, damp and hot middle resistance, feeling of fullness vomiting；Cornel coptis is relaxed liver anti-vomiting；For liver-stomach disharmony, vomiting is gulped down
Acid.It is existing in the market to there is Rhizoma Coptidis, coptis medicine materical crude slice, rhizoma extracting liquid, coptis concentrate, the coptis to be sprayed dried cream powder or the coptis
Particle etc., but there is presently no a kind of characteristic spectrum for reflecting coptis main component, it cannot fully and effectively measure coptis quality
Superiority and inferiority, and cannot rapidly and accurately judge the true and false of the coptis.
It is therefore desired to provide a kind of characteristic spectrum of coptis, it is able to solve at least one of above problem.
In consideration of it, the present invention is specifically proposed.
Summary of the invention
The first purpose of this invention is to provide a kind of HPLC characteristic spectrum of coptis, can overcome the above problem or
It at least is partially solved above-mentioned technical problem.
Second object of the present invention is to provide the construction method of the HPLC characteristic spectrum of the above-mentioned coptis.
Third object of the present invention is to provide the HPLC feature of the HPLC characteristic spectrum of the above-mentioned coptis or the above-mentioned coptis
Application of the HPLC characteristic spectrum for the coptis that the construction method of map obtains in the quality testing of coptis.
Fourth object of the present invention is to provide a kind of quality determining method of coptis.
First aspect according to the present invention provides a kind of HPLC characteristic spectrum of coptis, the HPLC characteristic spectrum packet
8 characteristic peaks are included, are control peak, the relative retention time of each characteristic peak with No. 8 peaks jamaicin peak are as follows:
No. 1 peak: relative retention time 0.095；
No. 2 peaks: relative retention time 0.359；
No. 3 peaks: relative retention time 0.526；
No. 4 peaks: relative retention time 0.551；
No. 5 peaks: relative retention time 0.581；
No. 6 peaks: relative retention time 0.653；
No. 7 peaks: relative retention time 0.888；
No. 8 peaks: relative retention time 1.000；
The relative retention time independence ground error of each characteristic peak is in ± 5% range.
It preferably, is control peak, the relative peak area of each characteristic peak with No. 8 peaks jamaicin peak are as follows:
No. 1 peak: relative peak area 0.0097；
No. 2 peaks: relative peak area 0.0257；
No. 3 peaks: relative peak area 0.0696；
No. 4 peaks: relative peak area 0.0670；
No. 5 peaks: relative peak area 0.1742；
No. 6 peaks: relative peak area 0.2815；
No. 7 peaks: relative peak area 0.2527；
No. 8 peaks: relative peak area 1.000；
The relative peak area independence ground error of each characteristic peak is in ± 5% range.
Preferably, amount mass exchange coefficient K value=K of each characteristic peak of the coptiss/Ko, value >=0.5 K；
Wherein, KsThe peak area of each characteristic peak measured under identical chromatographic conditions for coptis, coptis are Huang
Even medicinal material, coptis medicine materical crude slice, rhizoma extracting liquid, coptis concentrate, the coptis are sprayed dried cream powder or coptis particle, KoFor coptis medicine materical crude slice with
The peak area of corresponding characteristic peak.
Preferably, No. 1 peak is magnoflorine, and No. 3 peaks are jateorrhizine, and No. 4 peaks are jateorrhizine, and No. 5 peaks are table barberry
Alkali, No. 6 peaks are coptisine, and No. 7 peaks are palmatine, and No. 8 peaks are jamaicin.
The second aspect according to the present invention provides the construction method of the HPLC characteristic spectrum of the above-mentioned coptis, including following
Step:
Test sample is prepared using the coptis, test sample is detected using HPLC, when obtaining the opposite reservation of 8 chromatographic peaks
Between, construct the HPLC characteristic spectrum of the coptis；
Preferably, test sample is prepared using the coptis, test sample is detected using HPLC, obtains the phase of 8 chromatographic peaks
To retention time and relative peak area, the HPLC characteristic spectrum of the coptis is constructed.
Preferably, the test sample preparation method the following steps are included:
(a) coptis is added to the water, after boiling by intense fire, 15-25min, isolated filtrate and the dregs of a decoction is cooked by slow fire, by medicine
Slag is added to the water, and after boiling by intense fire, is cooked by slow fire 10-20min, isolated filtrate merges filtrate twice；
(b) filtrate that step (a) obtains is concentrated, obtains test sample after dry.
Preferably, the testing conditions of the HPLC are as follows:
The Detection wavelength of UV detector is 300-400nm in the HPLC；
The chromatographic column of the HPLC is C18 chromatographic column；
The mobile phase of the HPLC is made of acetonitrile, 3.2-3.8g/L potassium dihydrogen phosphate and lauryl sodium sulfate,
The volume ratio of acetonitrile and 3.2-3.8g/L potassium dihydrogen phosphate is 38-42:55-65, and the concentration of lauryl sodium sulfate is
0.12%-0.18%g/mL；
The column temperature of the HPLC is 30-40 DEG C；
The number of theoretical plate of the HPLC calculates >=5000 by Berberine hydrochloride peak；
Preferably, the Detection wavelength of the UV detector is 345nm；
Preferably, the mobile phase of the HPLC is by acetonitrile, 3.5g/L potassium dihydrogen phosphate and lauryl sodium sulfate group
At the volume ratio of acetonitrile and 3.5g/L potassium dihydrogen phosphate is 40:60, and the concentration of lauryl sodium sulfate is 0.15%g/
mL。
According to the present invention in terms of third, the HPLC characteristic spectrum of the above-mentioned coptis or the HPLC feature of the above-mentioned coptis are provided
Application of the HPLC characteristic spectrum for the coptis that the construction method of map obtains in the quality testing of coptis.
Preferably, the coptis includes Rhizoma Coptidis, coptis medicine materical crude slice, rhizoma extracting liquid, coptis concentrate, coptis spray
Mist dried cream powder or coptis particle.
4th aspect according to the present invention, provides a kind of quality determining method of coptis, comprising the following steps:
(A) the HPLC characteristic spectrum of coptis to be detected is obtained using HPLC, and the use of jamaicin is control peak, meter
Calculate the relative retention time of each chromatographic peak；
(B) relative retention time of the HPLC characteristic spectrum of the relative retention time for obtaining step (A) and the above-mentioned coptis
Or the relative retention time of the HPLC characteristic spectrum of the coptis that the construction method of the HPLC characteristic spectrum of the above-mentioned coptis obtains carries out
Compare；
(C) quality of coptis to be detected is judged according to the result of step (B)；
Preferably, the coptis quality determining method the following steps are included:
(A) the HPLC characteristic spectrum of coptis to be detected is obtained using HPLC, and the use of jamaicin is control peak, meter
Calculate the relative retention time and relative peak area of each chromatographic peak；
(B) relative retention time of the HPLC characteristic spectrum of the relative retention time for obtaining step (A) and the above-mentioned coptis
The HPLC characteristic spectrum of the coptis obtained with the construction method of relative peak area or the HPLC characteristic spectrum of the above-mentioned coptis it is opposite
Retention time and relative peak area are compared；
(C) quality of coptis to be detected is judged according to the result of step (B).
The present invention provides a kind of HPLC characteristic spectrum of coptis, which gives 8 features of the coptis
The relative retention time at peak, the relative standard deviation of the relative retention time of each characteristic peak is in 5% range, the HPLC of the coptis
Characteristic spectrum can be realized the quality for preferably controlling coptis, and strong operability can effectively make up existing coptis
The deficiency of Quality Control Technology.
The present invention also provides the construction method of the HPLC characteristic spectrum of the coptis, this method is simple and convenient, favorable reproducibility, each
The transmitting of component amount matter is stablized, and the peak shape of obtained each characteristic peak is good.The HPLC characteristic spectrum that this method obtains can comprehensively react
Coptis root dispensing granule production overall process in in change procedure, to effectively can instruct to feed intake in process of production, mention
Take, be concentrated, drying, overall process of pelletizing, really ensure clinical application safely, effectively, reliably, for formulate coptis root dispensing granule
Technological standards, quality standard provide science, rational basis.In addition, the building side of the HPLC characteristic spectrum of the coptis through the invention
The similarity for the characteristic spectrum that method obtains is >=99%.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art
Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below
Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor
It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is the HPLC characteristic spectrum of 23 batches of coptis standard decoction freeze-dried powders；
Fig. 2 is coptis standard decoction compare feature TuPu method map (peak 1: magnoflorine, peak 3: jateorrhizine, peak
4: jateorrhizine, peak 5: epiberberine, peak 6: coptisine, peak 7: palmatine, peak 8 (S): jamaicin)；
Fig. 3 is WL-03 standard decoction freeze-dried powder and the HPLC chromatogram that mixes reference substance；
Fig. 4 is that ((a) be the full wavelength scanner figure at peak 1, (b) is that magnoflorine is complete for peak 1 and magnoflorine full wavelength scanner figure
Length scanning figure)；
Fig. 5 is that ((a) be the full wavelength scanner figure at peak 3, (b) is calumba for peak 3 and jateorrhizine full wavelength scanner figure
Alkali full wavelength scanner figure)；
Fig. 6 is that ((a) be the full wavelength scanner figure at peak 4, (b) is jateorrhizine all-wave length for peak 4 and jateorrhizine full wavelength scanner figure
Scanning figure)；
Fig. 7 is that ((a) be the full wavelength scanner figure at peak 5, (b) is that epiberberine is complete for peak 5 and epiberberine full wavelength scanner figure
Length scanning figure)；
Fig. 8 is that ((a) be the full wavelength scanner figure at peak 6, (b) is coptisine all-wave length for peak 6 and coptisine full wavelength scanner figure
Scanning figure)；
Fig. 9 is that ((a) be the full wavelength scanner figure at peak 7, (b) is palmatine all-wave length for peak 7 and palmatine full wavelength scanner figure
Scanning figure)；
Figure 10 is that ((a) be the full wavelength scanner figure at peak 8, (b) is jamaicin all-wave for peak 8 and jamaicin full wavelength scanner figure
Long scan figure)；
Figure 11 be WL-03 batch standard decoction amount matter transfer characteristic map (S1: medicinal material, S2: medicine materical crude slice, S3: extracting solution, S4:
Concentrate, S5: standard decoction freeze-dried powder, R: control map)；
Figure 12 is that (S1: medicinal material, S2: S3: medicine materical crude slice extracts WL-09 batch coptis root dispensing granule amount matter transfer characteristic map
Liquid, S4: concentrate, S5: spraying dried cream powder, S6: particle, R: control map)；
Figure 13 is each peak K value of each workshop section of WL-09 batch coptis root dispensing granule.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with examples and drawings, but those skilled in the art
Member will be understood that the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not infused in embodiment
Bright actual conditions person, carries out according to conventional conditions or manufacturer's recommended conditions.Production firm is not specified in agents useful for same or instrument
Person is the conventional products that can be obtained by commercially available purchase.
First aspect according to the present invention, provides a kind of HPLC characteristic spectrum of coptis, and HPLC characteristic spectrum includes 8
Characteristic peak is control peak, the relative retention time of each characteristic peak with No. 8 peaks jamaicin peak are as follows:
No. 1 peak: relative retention time 0.095；
No. 2 peaks: relative retention time 0.359；
No. 3 peaks: relative retention time 0.526；
No. 4 peaks: relative retention time 0.551；
No. 5 peaks: relative retention time 0.581；
No. 6 peaks: relative retention time 0.653；
No. 7 peaks: relative retention time 0.888；
No. 8 peaks: relative retention time 1.000；
The relative retention time independence ground error of each characteristic peak is in ± 5% range.
It is understood that the relative retention time independence ground error of each characteristic peak refers to each spy in ± 5% range
The fluctuation range for levying peak is no more than 5%, such as the relative retention time at No. 1 peak is 0.095 ± (0.095 × 5%), as
0.095±0.00475。
It is understood that in the HPLC characteristic spectrum of the coptis equally with No. 8 peaks jamaicin peak be control peak, it can be deduced that
The relative peak area of each characteristic peak are as follows:
No. 1 peak: relative peak area 0.0097；
No. 2 peaks: relative peak area 0.0257；
No. 3 peaks: relative peak area 0.0696；
No. 4 peaks: relative peak area 0.0670；
No. 5 peaks: relative peak area 0.1742；
No. 6 peaks: relative peak area 0.2815；
No. 7 peaks: relative peak area 0.2527；
No. 8 peaks: relative peak area 1.000；
The relative peak area independence ground error of each characteristic peak is in ± 5% range.
The present invention provides a kind of HPLC characteristic spectrum of coptis, which gives 8 features of the coptis
The relative retention time at peak, the relative standard deviation of the relative retention time of each characteristic peak in ± 5% range, the coptis
HPLC characteristic spectrum can be realized the quality for preferably controlling coptis, and strong operability can effectively make up the existing coptis
The deficiency of quality of the pharmaceutical preparations control technology.
In a preferred embodiment, amount mass exchange coefficient K value=K of each characteristic peak of the coptiss/Ko, value >=0.5 K；
Wherein, KsThe peak area of each characteristic peak measured under identical chromatographic conditions for coptis, coptis are Huang
Even medicinal material, coptis medicine materical crude slice, rhizoma extracting liquid, coptis concentrate, the coptis are sprayed dried cream powder or coptis particle, KoFor coptis medicine materical crude slice with
The peak area of corresponding characteristic peak.
For example, in Rhizoma Coptidis each characteristic peak of the coptis at No. 1 peak amount mass exchange coefficient K value=peak of Rhizoma Coptidis 1
The peak area at No. 1 peak of peak area ÷ coptis medicine materical crude slice, the amount mass exchange coefficient K of each characteristic peak of the coptis at No. 3 peaks in rhizoma extracting liquid
The peak area at No. 3 peaks of peak area ÷ coptis medicine materical crude slice at No. 3 peaks of value=rhizoma extracting liquid.
In a preferred embodiment, No. 1 peak is magnoflorine, and No. 3 peaks are jateorrhizine, and No. 4 peaks are medicine root
Alkali, No. 5 peaks are epiberberine, and No. 6 peaks are coptisine, and No. 7 peaks are palmatine, and No. 8 peaks are jamaicin.
It is generated using similarity evaluation software (2012.130723 version) shared by 8
The compare feature map that peak is constituted, and similarity is greater than 0.99 between each test sample and compare feature map, passes through standard items mark
Fixed wherein peak 1 is magnoflorine, and peak 3 is jateorrhizine, and peak 4 is jateorrhizine, and peak 5 is epiberberine, and peak 6 is coptisine, peak 7
For palmatine, peak 8 is jamaicin.
The second aspect according to the present invention provides the construction method of the HPLC characteristic spectrum of the above-mentioned coptis, including following
Step:
Test sample is prepared using the coptis, test sample is detected using HPLC, when obtaining the opposite reservation of 8 chromatographic peaks
Between, construct the HPLC characteristic spectrum of the coptis.
The present invention also provides the construction method of the HPLC characteristic spectrum of the coptis, this method is simple and convenient, favorable reproducibility, each
The transmitting of component amount matter is stablized, and the peak shape of obtained each characteristic peak is good.The HPLC characteristic spectrum that this method obtains can comprehensively react
Coptis root dispensing granule production overall process in in change procedure, to effectively can instruct to feed intake in process of production, mention
Take, be concentrated, drying, overall process of pelletizing, really ensure clinical application safely, effectively, reliably, for formulate coptis root dispensing granule
Technological standards, quality standard provide science, rational basis.
In a preferred embodiment, test sample is prepared using the coptis, test sample is detected using HPLC, is obtained
To the relative retention time and relative peak area of 8 chromatographic peaks, the HPLC characteristic spectrum of the coptis is constructed.
In a preferred embodiment, test sample preparation method the following steps are included:
(a) coptis is added to the water, after boiling by intense fire, 15-25min, isolated filtrate and the dregs of a decoction is cooked by slow fire, by medicine
Slag is added to the water, and after boiling by intense fire, is cooked by slow fire 10-20min, isolated filtrate merges filtrate twice；
(b) filtrate that step (a) obtains is concentrated, obtains test sample after dry.
In step (a), the concrete operations for preparing filtrate are not construed as limiting, and are commonly extracted using those skilled in the art
Operation, for example, it may be, the 100g coptis is added in 900mL water, is placed in cooking pot for herbs, after boiling by intense fire, is cooked by slow fire
20min obtains filtrate and the dregs of a decoction after 200 mesh filtered through gauze, and the dregs of a decoction are added in 700mL water, after boiling by intense fire, are cooked by slow fire
10-20min is boiled, isolated filtrate merges filtrate twice.
In step (b), the solid-liquid ratio after the concrete operations and concentration of concentration is not construed as limiting, for example, can use rotation
Turn evaporimeter to be concentrated, being concentrated into solid-liquid ratio is 1:1, and thickening temperature can be 60 DEG C.
In step (b), dry specific method is not construed as limiting, using the common drying means of those skilled in the art
, for example, it may be freeze-drying.
In a preferred embodiment, the testing conditions of HPLC are as follows: the Detection wavelength of UV detector is in HPLC
300-400nm；The chromatographic column of HPLC is C18 chromatographic column；The mobile phase of HPLC is by acetonitrile, 3.2-3.8g/L potassium dihydrogen phosphate
It being formed with lauryl sodium sulfate, the volume ratio of acetonitrile and 3.2-3.8g/L potassium dihydrogen phosphate is 38-42:55-65,12
The concentration of sodium alkyl sulfate is 0.12%-0.18%g/mL；The column temperature of HPLC is 30-40 DEG C；The number of theoretical plate of HPLC presses hydrochloric acid
Jamaicin peak calculates >=5000.
By reasonably adjusting and optimizing the testing conditions of HPLC, be conducive to obtain the better HPLC characteristic spectrum of accuracy.
In a preferred embodiment, the Detection wavelength of UV detector is 345nm.
In a preferred embodiment, the mobile phase of HPLC is by acetonitrile, 3.5g/L potassium dihydrogen phosphate and 12
The volume ratio of sodium alkyl sulfate composition, acetonitrile and 3.5g/L potassium dihydrogen phosphate is 40:60, the concentration of lauryl sodium sulfate
For 0.15%g/mL
Using the Detection wavelength of 345nm, map baseline will not drift about, and shown three characteristic peak peak width,
Peak height optimum, separating effect are more preferable.
According to the present invention in terms of third, the HPLC characteristic spectrum of the above-mentioned coptis or the HPLC feature of the above-mentioned coptis are provided
Application of the HPLC characteristic spectrum for the coptis that the construction method of map obtains in the quality testing of coptis.
The coptis that the construction method of the HPLC characteristic spectrum of the above-mentioned coptis or the HPLC characteristic spectrum of the above-mentioned coptis is obtained
HPLC characteristic spectrum be applied to coptis quality testing in, can effectively judge the superiority and inferiority and the true and false of coptis.
The type of coptis is not construed as limiting, it is dense to can be Rhizoma Coptidis, coptis medicine materical crude slice, rhizoma extracting liquid, the coptis
Contracting liquid, the coptis are sprayed dried cream powder or coptis particle.
4th aspect according to the present invention, provides a kind of quality determining method of coptis, comprising the following steps:
(A) the HPLC characteristic spectrum of coptis to be detected is obtained using HPLC, and the use of jamaicin is control peak, meter
Calculate the relative retention time of each chromatographic peak；
(B) relative retention time of the HPLC characteristic spectrum of the relative retention time for obtaining step (A) and the above-mentioned coptis
Or the relative retention time of the HPLC characteristic spectrum of the coptis that the construction method of the HPLC characteristic spectrum of the above-mentioned coptis obtains carries out
Compare；
(C) quality of coptis to be detected is judged according to the result of step (B).
If step (A) obtains the relative retention time of each chromatographic peak and when retaining relatively of the HPLC characteristic spectrum of the coptis
Between similarity it is high, then illustrate the good quality of coptis to be detected, similarity is higher, the quality of coptis to be detected
It is more excellent.
By the quality determining method of coptis, the direct quality of the coptis can be fast and effeciently judged, be quality system
The quality of requirements of agent provides science, rational basis.
In a preferred embodiment, coptis quality determining method the following steps are included:
(A) the HPLC characteristic spectrum of coptis to be detected is obtained using HPLC, and the use of jamaicin is control peak, meter
Calculate the relative retention time and relative peak area of each chromatographic peak；
(B) relative retention time of the HPLC characteristic spectrum of the relative retention time for obtaining step (A) and the above-mentioned coptis
The HPLC characteristic spectrum of the coptis obtained with the construction method of relative peak area or the HPLC characteristic spectrum of the above-mentioned coptis it is opposite
Retention time and relative peak area are compared；
(C) quality of coptis to be detected is judged according to the result of step (B).
If step (A) obtains the relative retention time of each chromatographic peak and the HPLC characteristic spectrum of relative peak area and the coptis
Relative retention time and relative peak area similarity it is high, then illustrate that the good quality of coptis to be detected, similarity are got over
The quality of height, coptis to be detected is more excellent.
Technical solution of the present invention is described further below in conjunction with embodiment.
The HPLC characteristic spectrum of 1 coptis of embodiment
A kind of HPLC characteristic spectrum of the coptis, HPLC characteristic spectrum include 8 characteristic peaks, are pair with No. 8 peaks jamaicin peak
According to peak, the relative retention time of each characteristic peak are as follows:
No. 1 peak: relative retention time 0.095；
No. 2 peaks: relative retention time 0.359；
No. 3 peaks: relative retention time 0.526；
No. 4 peaks: relative retention time 0.551；
No. 5 peaks: relative retention time 0.581；
No. 6 peaks: relative retention time 0.653；
No. 7 peaks: relative retention time 0.888；
No. 8 peaks: relative retention time 1.000.
It is control peak, the relative peak area of each characteristic peak with No. 8 peaks jamaicin peak are as follows:
No. 1 peak: relative peak area 0.0097；
No. 2 peaks: relative peak area 0.0257；
No. 3 peaks: relative peak area 0.0696；
No. 4 peaks: relative peak area 0.0670；
No. 5 peaks: relative peak area 0.1742；
No. 6 peaks: relative peak area 0.2815；
No. 7 peaks: relative peak area 0.2527；
No. 8 peaks: relative peak area 1.000.
No. 1 peak is magnoflorine, and No. 3 peaks are jateorrhizine, and No. 4 peaks are jateorrhizine, and No. 5 peaks are epiberberine, No. 6 peaks
For coptisine, No. 7 peaks are palmatine, and No. 8 peaks are jamaicin.
The building of the HPLC characteristic spectrum of 2 coptis of embodiment
(1) coptis is acquired
Acquire qualified Rhizoma Coptidis 30 batches of the main genuine place of production of Hubei, Sichuan, the coptiss such as Chongqing, and by each batch medicinal material
It is processed into qualified coptis medicine materical crude slice 23 batches.Unqualified medicinal material is directly rejected, and medicinal material acquires information, and see Table 1 for details.
1 different batches Rhizoma Coptidis place of production information of table
(2) preparation of test solution
Each batch each 100g of coptis medicine materical crude slice is weighed, is placed in cooking pot for herbs, 900mL pure water is added, after boiling by intense fire, mild fire is again
20min is decocted, for extracting solution after 200 mesh filtered through gauze, the dregs of a decoction add pure water 700mL, after boiling by intense fire, be cooked by slow fire 15min again,
Merge filtrate twice.It is about 1:1 that each batch filtrate, which is concentrated into solid-liquid ratio through Rotary Evaporators, and thickening temperature is set as 60 DEG C.
Each batch concentrate is placed in pallet, frozen drying, is crushed, weighed to get test sample.
Test sample (crossing No. three sieves) about 0.1g is taken, it is accurately weighed, it sets in stuffed conical flask, methanol-hydrochloric acid is added in precision
The mixed solution 25ml of (100:1), close plug, weighed weight, ultrasonic treatment (power 250W, frequency 40kHz) 30 minutes are let cool,
Weighed weight again is supplied the weight of less loss with methanol, is shaken up, and filtration, precision measures subsequent filtrate 2ml, sets in 10ml measuring bottle, adds first
Alcohol shakes up to scale, filters, take subsequent filtrate to get test solution.
(3) preparation of reference substance solution
Magnoflorine, jateorrhizine, Jatrorrhizine chloride, hydrochloric acid epiberberine, hydrochloric acid coptisine, hydrochloric acid bar horse are taken respectively
Spit of fland and Berberine hydrochloride, add methanol, and reference substance solution is made.
Respectively contain 29.57 μ g magnoflorines, 32.52 μ g jateorrhizines, 34.45 μ g hydrochloric acid medicines in every 1ml reference substance solution
Root alkali, 56.94 μ g hydrochloric acid epiberberines, 21.57 μ g hydrochloric acid coptisines, 25.45 μ g palmatin hydrochlorides and 114.85 μ g hydrochloric acid are small
Bark of a cork tree alkali.
(4) reference substance solution and each 5 μ l of test solution are taken respectively, injects liquid chromatograph, and measurement records chromatogram.
23 batches of sample chromatogram figures are imported into similarity evaluation software (2012.130723
Version), establishing 23 batches of coptis standard decoction HPLC characteristic spectrums with median method, (see Fig. 1, in Fig. 1, curve S1 (8) is corresponding
Correspond to WL-04 in WL-03, curve S2 (8), curve S3 (8) corresponds to WL-05, and curve S4 (8) corresponds to WL-06, curve S5
(8) correspond to WL-07, curve S6 (8) corresponds to WL-08, and curve S7 (8) corresponds to WL-09, and curve S8 (8) corresponds to WL-
10, curve S9 (8) correspond to WL-11, and curve S10 (8) corresponds to WL-12, and curve S11 (8) corresponds to WL-14, curve S12
(8) correspond to WL-15, curve S13 (8) corresponds to WL-16, and curve S14 (8) corresponds to WL-19, and curve S15 (8) corresponds to
WL-21, curve S16 (8) correspond to WL-22, and curve S17 (8) corresponds to WL-24, and curve S18 (8) corresponds to WL-25, curve
S19 (8) corresponds to WL-26, and curve S20 (8) corresponds to WL-27, and curve S21 (8) corresponds to WL-28, and curve S22 (8) is corresponding
Correspond to WL-30 in WL-29, curve S12 (8)), and generate the compare feature map being made of 8 shared peaks (see Fig. 2).
Using octadecylsilane chemically bonded silica as filler；It is (every with acetonitrile -3.5g/L potassium dihydrogen phosphate (40:60)
Lauryl sodium sulfate 1.5g in 1000mL) it is mobile phase；Detection wavelength is 345nm, and number of theoretical plate is based on Berberine hydrochloride peak
5000 should be not less than by calculating.
1 similarity of test example
The test solution and reference substance solution characteristic spectrum similarity of 23 batches of coptis standard decoctions in embodiment 2 are calculated,
Obtain that the results are shown in Table 2.
2 similarity value of table
As shown in Table 2, the similarity of 23 batches of coptis standard decoctions and reference substance solution >=99%.
The determination of 2 characteristic spectrum of test example each peak relative retention time and relative peak area
It is control peak with peak 8 (jamaicin peak), it is opposite calculates separately 23 each characteristic peaks of batch coptis standard decoction freeze-dried powder
Retention time and relative peak area, and average value is calculated, obtained result is as shown in Table 3 and Table 4.
Each characteristic spectrum relative retention time of table 3
| Sample | Peak 1 | Peak 2 | Peak 3 | Peak 4 | Peak 5 | Peak 6 | Peak 7 | Peak 8 |
| WL-03 | 0.097 | 0.359 | 0.527 | 0.552 | 0.582 | 0.653 | 0.888 | 1.000 |
| WL-04 | 0.097 | 0.359 | 0.527 | 0.551 | 0.582 | 0.653 | 0.888 | 1.000 |
| WL-05 | 0.097 | 0.36 | 0.527 | 0.551 | 0.582 | 0.653 | 0.888 | 1.000 |
| WL-06 | 0.097 | 0.36 | 0.527 | 0.552 | 0.582 | 0.653 | 0.889 | 1.000 |
| WL-07 | 0.097 | 0.36 | 0.527 | 0.552 | 0.582 | 0.653 | 0.889 | 1.000 |
| WL-08 | 0.097 | 0.36 | 0.527 | 0.552 | 0.583 | 0.653 | 0.889 | 1.000 |
| WL-09 | 0.097 | 0.36 | 0.528 | 0.552 | 0.583 | 0.653 | 0.891 | 1.000 |
| WL-10 | 0.097 | 0.36 | 0.528 | 0.552 | 0.583 | 0.653 | 0.889 | 1.000 |
| WL-11 | 0.097 | 0.36 | 0.527 | 0.552 | 0.582 | 0.653 | 0.892 | 1.000 |
| WL-12 | 0.097 | 0.36 | 0.527 | 0.552 | 0.582 | 0.653 | 0.888 | 1.000 |
| WL-14 | 0.097 | 0.36 | 0.527 | 0.551 | 0.582 | 0.653 | 0.888 | 1.000 |
| WL-15 | 0.097 | 0.36 | 0.526 | 0.551 | 0.582 | 0.653 | 0.888 | 1.000 |
| WL-16 | 0.097 | 0.36 | 0.526 | 0.551 | 0.582 | 0.653 | 0.887 | 1.000 |
| WL-19 | 0.097 | 0.36 | 0.527 | 0.551 | 0.582 | 0.653 | 0.887 | 1.000 |
| WL-21 | 0.097 | 0.359 | 0.527 | 0.551 | 0.582 | 0.653 | 0.888 | 1.000 |
| WL-22 | 0.097 | 0.359 | 0.526 | 0.551 | 0.582 | 0.653 | 0.887 | 1.000 |
| WL-24 | 0.097 | 0.36 | 0.527 | 0.551 | 0.582 | 0.653 | 0.887 | 1.000 |
| WL-25 | 0.097 | 0.359 | 0.526 | 0.55 | 0.581 | 0.653 | 0.886 | 1.000 |
| WL-26 | 0.097 | 0.359 | 0.525 | 0.55 | 0.581 | 0.653 | 0.886 | 1.000 |
| WL-27 | 0.097 | 0.359 | 0.526 | 0.55 | 0.581 | 0.654 | 0.885 | 1.000 |
| WL-28 | 0.097 | 0.36 | 0.527 | 0.551 | 0.582 | 0.653 | 0.888 | 1.000 |
| WL-29 | 0.098 | 0.36 | 0.527 | 0.551 | 0.582 | 0.653 | 0.888 | 1.000 |
| WL-30 | 0.098 | 0.36 | 0.527 | 0.552 | 0.582 | 0.653 | 0.888 | 1.000 |
| Mean value | 0.097 | 0.360 | 0.527 | 0.551 | 0.582 | 0.653 | 0.888 | 1.000 |
| RSD | 0.29% | 0.13% | 0.12% | 0.12% | 0.09% | 0.03% | 0.17% | 0.00% |
As shown in Table 3, relative retention time is peak 1:0.097, peak 2:0.360, peak 3:0.527, peak 4:0.551, peak
5:0.582, peak 6:0.653, peak 7:0.888, peak 8:1.000, within ± the 5% of specified value, RSD < 1%.
Each characteristic spectrum relative peak area of table 4
| Sample | Peak 1 | Peak 2 | Peak 3 | Peak 4 | Peak 5 | Peak 6 | Peak 7 | Peak 8 |
| WL-03 | 0.0094 | 0.0259 | 0.0683 | 0.0660 | 0.1727 | 0.2760 | 0.2497 | 1.0000 |
| WL-04 | 0.0090 | 0.0264 | 0.0693 | 0.0678 | 0.1732 | 0.2864 | 0.2534 | 1.0000 |
| WL-05 | 0.0097 | 0.0266 | 0.0701 | 0.0665 | 0.1728 | 0.2769 | 0.2488 | 1.0000 |
| WL-06 | 0.0096 | 0.0254 | 0.0721 | 0.0679 | 0.1737 | 0.2864 | 0.2478 | 1.0000 |
| WL-07 | 0.0100 | 0.0259 | 0.0703 | 0.0660 | 0.1727 | 0.2864 | 0.2534 | 1.0000 |
| WL-08 | 0.0099 | 0.0250 | 0.0683 | 0.0678 | 0.1732 | 0.2901 | 0.2497 | 1.0000 |
| WL-09 | 0.0094 | 0.0254 | 0.0683 | 0.0668 | 0.1726 | 0.2766 | 0.2566 | 1.0000 |
| WL-10 | 0.0096 | 0.0250 | 0.0700 | 0.0678 | 0.1740 | 0.2901 | 0.2499 | 1.0000 |
| WL-11 | 0.0098 | 0.0250 | 0.0687 | 0.0661 | 0.1727 | 0.2766 | 0.2534 | 1.0000 |
| WL-12 | 0.0098 | 0.0258 | 0.0701 | 0.0678 | 0.1800 | 0.2768 | 0.2602 | 1.0000 |
| WL-14 | 0.0101 | 0.0257 | 0.0689 | 0.0678 | 0.1732 | 0.2864 | 0.2537 | 1.0000 |
| WL-15 | 0.0094 | 0.0254 | 0.0701 | 0.0663 | 0.1801 | 0.2777 | 0.2491 | 1.0000 |
| WL-16 | 0.0094 | 0.0257 | 0.0701 | 0.0666 | 0.1732 | 0.2744 | 0.2534 | 1.0000 |
| WL-19 | 0.0103 | 0.0259 | 0.0694 | 0.0666 | 0.1729 | 0.2864 | 0.2591 | 1.0000 |
| WL-21 | 0.0093 | 0.0266 | 0.0701 | 0.0673 | 0.1732 | 0.2869 | 0.2603 | 1.0000 |
| WL-22 | 0.0094 | 0.0263 | 0.0694 | 0.0669 | 0.1735 | 0.2760 | 0.2534 | 1.0000 |
| WL-24 | 0.0101 | 0.0260 | 0.0683 | 0.0678 | 0.1723 | 0.2869 | 0.2495 | 1.0000 |
| WL-25 | 0.0094 | 0.0260 | 0.0701 | 0.0661 | 0.1754 | 0.2765 | 0.2534 | 1.0000 |
| WL-26 | 0.0102 | 0.0261 | 0.0708 | 0.0660 | 0.1768 | 0.2768 | 0.2491 | 1.0000 |
| WL-27 | 0.0098 | 0.0254 | 0.0694 | 0.0678 | 0.1799 | 0.2864 | 0.2534 | 1.0000 |
| WL-28 | 0.0101 | 0.0264 | 0.0701 | 0.0678 | 0.1732 | 0.2760 | 0.2477 | 1.0000 |
| WL-29 | 0.0094 | 0.0251 | 0.0686 | 0.0664 | 0.1732 | 0.2864 | 0.2534 | 1.0000 |
| WL-30 | 0.0094 | 0.0252 | 0.0701 | 0.0664 | 0.1727 | 0.2760 | 0.2534 | 1.0000 |
| Mean value | 0.0097 | 0.0257 | 0.0696 | 0.0670 | 0.1742 | 0.2815 | 0.2527 | 1.0000 |
| RSD | 3.57% | 2.00% | 1.36% | 1.12% | 1.43% | 2.00% | 1.47% | 0.00% |
As shown in Table 4, relative peak area be peak 1:0.0097, peak 2:0.0257, peak 3:0.0696, peak 4:0.0670,
Peak 5:0.1742, peak 6:0.2815, peak 7:0.2527, peak 8:1.0000, within ± the 5% of specified value, RSD < 4%.
Each chromatographic peak of 3 characteristic spectrum of test example is pointed out
(1) coptis main chemical compositions be alkaloids, mainly include jamaicin, epiberberine, coptisine, palmatine,
Still also containing magnoflorine, jateorrhizine, jateorrhizine etc..By the method for multicomponent, global quality control, respectively will more than
7 kinds of substance reference substances and the retinue control of standard decoction freeze-dried powder, determine related component by relative retention time.WL-03 is marked
Quasi- decoction freeze-dried powder and mixing reference substance (reference substance solution in embodiment 2) carry out HPLC detection, obtained WL-03 standard soup
Agent freeze-dried powder is as shown in Figure 3 with the HPLC chromatogram for mixing reference substance.
From the figure 3, it may be seen that magnoflorine is consistent with the retention time at peak 1, jateorrhizine is consistent with the retention time at peak 3,
Jateorrhizine is consistent with the retention time at peak 4, and epiberberine is consistent with the retention time at peak 5, the retention time one of coptisine and peak 6
It causes, palmatine is consistent with the retention time at peak 7, and jamaicin is consistent with the retention time at peak 8.
(2) more each chromatographic peak is swept for peak 1 with magnoflorine all-wave length with reference substance all-wave length absorption curve, Fig. 4 is mixed
Tracing, Fig. 5 are peak 3 and jateorrhizine full wavelength scanner figure, and Fig. 6 is peak 4 and jateorrhizine full wavelength scanner figure, Fig. 7 be peak 5 with
Epiberberine full wavelength scanner figure, Fig. 8 are peak 6 and coptisine full wavelength scanner figure, and Fig. 9 is peak 7 and palmatine full wavelength scanner
Figure, Figure 10 are peak 8 and jamaicin full wavelength scanner figure.
By Fig. 4-Figure 10 it is found that each peak all-wave length absorption curve is also consistent with hybrid standard product, each guarantor is sufficiently proved
Staying corresponding chromatographic peak under time conditions is reference substance substance.
4 each process characteristic spectrum similarity comparison of test example
Characteristic spectrum is carried out to the medicinal material of the WL-03 batches of coptiss, medicine materical crude slice, extracting solution, concentrate and standard decoction freeze-dried powder to grind
Study carefully, measures characteristic spectrum, and calculate the similarity of each sample characteristic spectrum Yu standard decoction compare feature map.WL-03 batch
Standard decoction amount matter transfer characteristic map is as shown in figure 11, and the results are shown in Table 5 for similarity calculation.
5 similarity calculation result of table
| Medicinal material | Medicine materical crude slice | Extracting solution | Concentrate | Freeze-dried powder | Compare map | |
| Medicinal material | 1 | 1 | 1 | 1 | 0.999 | 0.999 |
| Medicine materical crude slice | 1 | 1 | 0.999 | 1 | 1 | 0.999 |
| Extracting solution | 1 | 0.999 | 1 | 0.999 | 0.999 | 0.998 |
| Concentrate | 1 | 1 | 0.999 | 1 | 0.999 | 0.999 |
| Freeze-dried powder | 0.999 | 1 | 0.999 | 0.999 | 1 | 0.999 |
| Compare map | 1 | 1 | 1 | 1 | 1 | 1 |
By Figure 11 and table 5 it is found that Rhizoma Coptidis, medicine materical crude slice, extracting solution, concentrate, standard decoction freeze-dried powder chromatogram
There are identical 8 chromatographic peaks in corresponding position, show medicinal material to standard decoction main chemical compositions consistency；Each characteristic spectrum
Similarity shows to meet the requirements 0.99 or more.
Each chromatographic peak of 5 characteristic spectrum of test example is with respect to peak retention time transitive relation
WL-09 batch Rhizoma Coptidis is taken, qualified medicine materical crude slice is processed into, weighs coptis medicine materical crude slice 40kg, extracting in water 3 times, every time
Add 12 times of amount water, 1.5 hours every time, the filtration of 120 mesh merged filtrate three times, by filtrate decompression concentration (temperature: 60~65 DEG C, very
Reciprocal of duty cycle: -0.06~0.08MPa) to relative density be 1.10~1.15 (60 DEG C) medicinal extract, fan frequency 40Hz~
50Hz, atomizer frequency 40Hz~50Hz carry out spray drying under the conditions of 150-170 DEG C of inlet air temperature and get dry extract powder, dried cream powder
A certain amount of maltodextrin is added, particle 10kg is made in dry granulation, i.e., 1g granule is opposite works as 4g medicine materical crude slice.
By the medicinal material of the above WL-09 batch coptis, medicine materical crude slice, extracting solution, concentrate, spraying dried cream powder, particle and coptis mark
The quasi- resulting standard control characteristic spectrum of decoction is compared, obtained WL-09 batch coptis root dispensing granule amount matter transfer characteristic
Map is shown in Figure 12, and WL-09 batches of coptis characteristic peak relative retention times are shown in Table 6.
6 WL-09 of table batches of coptis characteristic peak relative retention times
| Sample | Peak 1 | Peak 2 | Peak 3 | Peak 4 | Peak 5 | Peak 6 | Peak 7 | Peak 8 |
| Medicinal material | 0.098 | 0.366 | 0.532 | 0.556 | 0.586 | 0.653 | 0.891 | 1.000 |
| Medicine materical crude slice | 0.098 | 0.366 | 0.531 | 0.555 | 0.584 | 0.655 | 0.890 | 1.000 |
| Extracting solution | 0.099 | 0.367 | 0.535 | 0.559 | 0.590 | 0.659 | 0.895 | 1.000 |
| Concentrate | 0.098 | 0.365 | 0.531 | 0.555 | 0.586 | 0.656 | 0.890 | 1.000 |
| Dried cream powder | 0.099 | 0.365 | 0.531 | 0.556 | 0.586 | 0.656 | 0.890 | 1.000 |
| Particle | 0.099 | 0.365 | 0.531 | 0.555 | 0.586 | 0.656 | 0.890 | 1.000 |
| RSD | 0.56% | 0.22% | 0.30% | 0.28% | 0.34% | 0.30% | 0.22% | 0.00% |
By table 6 and Figure 12 it is found that 8 shared peaks occurs in each link of production process, correlation is good, and each peak is opposite to be retained
Time is close to (using jamaicin retention time as reference), RSD < 1%, therefore the transmitting of coptis production process amount matter is stablized, and substance is real
Existing effect transmitting.
6 peak area ratio value coefficient of test example
Matter transmittance process is measured in production process in order to more clearly state, each process takes during making pellet in embodiment 5
Sample measures and calculates each each chromatographic peak total content, each peak total content peak total content corresponding with medicine materical crude slice in the process and be divided by, calculates gained
Value be defined as K value, according to the stability of K value, decision content matter transmits stability and regularity.Table 7 is WL-09 batches of coptis features
Peak is opposite to protect peak area K value, and Figure 13 is each peak K value of each workshop section of WL-09 batch coptis root dispensing granule.
7 WL-09 of table batches of coptis characteristic peaks are opposite to protect peak area K value
By table 7 and Figure 13 it is found that 8 chromatographic peak total contents lost from medicinal material to medicine materical crude slice it is very low, for process slicing processes
Normal loss, in controlled range；From medicine materical crude slice to extracting solution process because of Extraction solvent reason, cause fractions that cannot extract
It entirely, is normal phenomenon；From extract concentration, drying, pelletization loss it is less, content tends towards stability, K value >=0.5, example
Such as, the K value at No. 1 peak of Rhizoma Coptidis is 1.0311, and the K value at No. 2 peaks of coptis particle is 0.5578.And 8 colors of whole process
Spectral peak without obviously increasing or reducing phenomenon, illustrate 8 ingredients in the whole process without decompose, enrichment phenomenon, between each component compared with
Stablize, to reach stable amount matter transitive relation.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of HPLC characteristic spectrum of coptis, which is characterized in that the HPLC characteristic spectrum includes 8 characteristic peaks, with No. 8 peaks
Jamaicin peak is control peak, the relative retention time of each characteristic peak are as follows:
No. 1 peak: relative retention time 0.095；
No. 2 peaks: relative retention time 0.359；
No. 3 peaks: relative retention time 0.526；
No. 4 peaks: relative retention time 0.551；
No. 5 peaks: relative retention time 0.581；
No. 6 peaks: relative retention time 0.653；
No. 7 peaks: relative retention time 0.888；
No. 8 peaks: relative retention time 1.000；
The relative retention time independence ground error of each characteristic peak is in ± 5% range.
2. the HPLC characteristic spectrum of the coptis according to claim 1, which is characterized in that with No. 8 peaks jamaicin peak be control
Peak, the relative peak area of each characteristic peak are as follows:
No. 1 peak: relative peak area 0.0097；
No. 2 peaks: relative peak area 0.0257；
No. 3 peaks: relative peak area 0.0696；
No. 4 peaks: relative peak area 0.0670；
No. 5 peaks: relative peak area 0.1742；
No. 6 peaks: relative peak area 0.2815；
No. 7 peaks: relative peak area 0.2527；
No. 8 peaks: relative peak area 1.000；
The relative peak area independence ground error of each characteristic peak is in ± 5% range.
3. the HPLC characteristic spectrum of the coptis according to claim 1, which is characterized in that
Amount mass exchange coefficient K value=K of each characteristic peak of the coptiss/Ko, value >=0.5 K；
Wherein, KsThe peak area of each characteristic peak measured under identical chromatographic conditions for coptis, coptis are coptis medicine
Material, coptis medicine materical crude slice, rhizoma extracting liquid, coptis concentrate, the coptis are sprayed dried cream powder or coptis particle, KoFor coptis medicine materical crude slice with it is corresponding
Characteristic peak peak area.
4. the HPLC characteristic spectrum of the coptis according to claim 1-3, which is characterized in that No. 1 peak is magnolia
Alkali, No. 3 peaks are jateorrhizine, and No. 4 peaks are jateorrhizine, and No. 5 peaks are epiberberine, and No. 6 peaks are coptisine, and No. 7 peaks are bar horse
Spit of fland, No. 8 peaks are jamaicin.
5. the construction method of the HPLC characteristic spectrum of the described in any item coptiss of claim 1-4, which is characterized in that including following
Step:
Test sample is prepared using the coptis, test sample is detected using HPLC, obtains the relative retention time of 8 chromatographic peaks,
Construct the HPLC characteristic spectrum of the coptis；
Preferably, test sample is prepared using the coptis, test sample is detected using HPLC, obtain the opposite guarantor of 8 chromatographic peaks
Time and relative peak area are stayed, the HPLC characteristic spectrum of the coptis is constructed.
6. the construction method of the HPLC characteristic spectrum of the coptis according to claim 5, which is characterized in that the test sample
Preparation method the following steps are included:
(a) coptis is added to the water, after boiling by intense fire, is cooked by slow fire 15-25min, isolated filtrate and the dregs of a decoction, by the dregs of a decoction plus
Enter in water, after boiling by intense fire, is cooked by slow fire 10-20min, isolated filtrate merges filtrate twice；
(b) filtrate that step (a) obtains is concentrated, obtains test sample after dry.
7. the construction method of the HPLC characteristic spectrum of the coptis according to claim 5, which is characterized in that the inspection of the HPLC
Survey condition are as follows:
The Detection wavelength of UV detector is 300-400nm in the HPLC；
The chromatographic column of the HPLC is C18 chromatographic column；
The mobile phase of the HPLC is made of acetonitrile, 3.2-3.8g/L potassium dihydrogen phosphate and lauryl sodium sulfate, acetonitrile
Volume ratio with 3.2-3.8g/L potassium dihydrogen phosphate is 38-42:55-65, and the concentration of lauryl sodium sulfate is 0.12%-
0.18%g/mL；
The column temperature of the HPLC is 30-40 DEG C；
The number of theoretical plate of the HPLC calculates >=5000 by Berberine hydrochloride peak；
Preferably, the Detection wavelength of the UV detector is 345nm；
Preferably, the mobile phase of the HPLC is made of acetonitrile, 3.5g/L potassium dihydrogen phosphate and lauryl sodium sulfate, second
The volume ratio of nitrile and 3.5g/L potassium dihydrogen phosphate is 40:60, and the concentration of lauryl sodium sulfate is 0.15%g/mL.
8. HPLC characteristic spectrum or the described in any item coptiss of claim 5-7 of the described in any item coptiss of claim 1-4
HPLC characteristic spectrum application of the obtained HPLC characteristic spectrum of the coptis of construction method in the quality testing of coptis.
9. application according to claim 8, which is characterized in that the coptis includes Rhizoma Coptidis, coptis medicine materical crude slice, Huang
Even extracting solution, coptis concentrate, the coptis are sprayed dried cream powder or coptis particle.
10. a kind of quality determining method of coptis, which comprises the following steps:
(A) the HPLC characteristic spectrum of coptis to be detected is obtained using HPLC, and the use of jamaicin is control peak, calculated each
The relative retention time of chromatographic peak；
(B) the HPLC characteristic spectrum of the relative retention time for obtaining step (A) and the described in any item coptiss of claim 1-4
Relative retention time or the described in any item coptiss of claim 5-7 HPLC characteristic spectrum the obtained coptis of construction method
The relative retention time of HPLC characteristic spectrum be compared；
(C) quality of coptis to be detected is judged according to the result of step (B)；
Preferably, the coptis quality determining method the following steps are included:
(A) the HPLC characteristic spectrum of coptis to be detected is obtained using HPLC, and the use of jamaicin is control peak, calculated each
The relative retention time and relative peak area of chromatographic peak；
(B) the HPLC characteristic spectrum of the relative retention time for obtaining step (A) and the described in any item coptiss of claim 1-4
Relative retention time and relative peak area or the described in any item coptiss of claim 5-7 HPLC characteristic spectrum building side
The relative retention time and relative peak area of the HPLC characteristic spectrum for the coptis that method obtains are compared；
(C) quality of coptis to be detected is judged according to the result of step (B).
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Application publication date: 20190628 |