CN106770832B - Ginseng and pilose antler strengthening the essence tablet quality control method - Google Patents
Ginseng and pilose antler strengthening the essence tablet quality control method Download PDFInfo
- Publication number
- CN106770832B CN106770832B CN201710007091.5A CN201710007091A CN106770832B CN 106770832 B CN106770832 B CN 106770832B CN 201710007091 A CN201710007091 A CN 201710007091A CN 106770832 B CN106770832 B CN 106770832B
- Authority
- CN
- China
- Prior art keywords
- solution
- ginsenoside
- ginseng
- butanol
- methanol
- 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.)
- Expired - Fee Related
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of ginseng and pilose antler strengthening the essence tablet quality control methods, identify Radix Astragali and ginseng in drug including the use of thin-layered chromatography；Using main active ginsenoside Rg in high effective liquid chromatography for measuring drug1(C42H72O14) and ginsenoside Re (C48H82O18) content.Ginseng and pilose antler strengthening the essence tablet quality control method of the invention has stronger specificity and good reproducibility, can preferably control drug quality, really meet the requirement that drug safety is effective, quality controllable.
Description
Technical field
The invention belongs to technical field of pharmaceuticals, specifically, being related to a kind of ginseng and pilose antler strengthening the essence tablet quality control method.
Background technique
In recent years, China's Cancer Mortality, the death rate are in sustainable growth trend.According to national tumor center's epidemiology
Research report: 20 years from now on, the morbidity and mortality of China's malignant tumour will also persistently rise.If do not adopted an effective measure,
The year two thousand twenty, China's pathogenesis of cancer number and death toll will rise to 4,000,000 people and 3,000,000 people；The year two thousand thirty will rise to 5,000,000 people and
3500000 people.Surgical operation, radiation and chemotherapy are the common methods of current clinical treatment malignant tumour.But radiation and chemotherapy is being controlled
Often cause serious side effect while treatment, causes the symptoms such as oligoleukocythemia, hemoglobin reduction.According to another report, China's hepatitis,
Hepatitis B disease incidence shows lasting ascendant trend, accounts for the 20% of outpatient service viral hepatitis patient's total amount, leads to cirrhosis, liver cancer
Major incentive.Hepatitis C early stage non-evident sympton, is easily ignored by patient, and there is no effective hcv vaccine at present, more
Number patient is medical in cirrhosis compensatory phase, Decompensated stage, has missed best occasion for the treatment, prognosis is poor.Hepatitis B be widely current in
Countries in the world seriously threaten human health, and main infringement children and person between twenty and fifty, small number of patients can be converted into cirrhosis or liver cancer.
Hepatitis B can fall ill throughout the year without specific epizootic modeling, be current China's prevalence the most extensively, the disease of harmfulness most serious it
One.Interferon and Ribavirin are usually used in the clinical treatment of hepatitis and hepatitis B, but often patient are caused leucocyte, hemoglobin occur
The side effects such as reduction.
Ginseng and pilose antler strengthening the essence piece prescription in the case where the famous expert Miao Ming tri- in China is instructed；The party by American Ginseng, Radix Astragali, the fruit of glossy privet, when
Return, Radix Salviae Miltiorrhizae, Rhizoma Atractylodis Macrocephalae, Chinese yam, Schisandra chinensis, garden burnet, hawthorn, cynomorium songaricum, pilose antler, Radix Ophiopogonis, the 14 taste Chinese medicinal compositions such as fructus lycii.Its function
It can be veins takes off admittedly, tonifying spleen and liver, shengjin nourishing, tranquilize the mind and promote the intelligence invigorating kidney yang, benefiting essence-blood, strengthening the bones and muscles.Suffer from suitable for hepatitis, hepatitis B
The oligoleukocythemia occurred after person's conventional therapy or tumor patient chemicotherapy, hemoglobin is low and altitude sickness and indigestion
Etc. symptoms.14 medicines share, collect veins takes off admittedly, tonifying spleen and liver, shengjin nourishing, tranquilize the mind and promote the intelligence invigorating kidney yang, benefiting essence-blood, strengthening the bones and muscles it
Function Yu Yiti both payes attention to dredging vascular, to improve internal organs blood supply, and can improve human body allomeric function and metabolism, reach righting and dispel
The purpose of heresy.The prescription is first used for some patientss by prescriptions of traditional Chinese medicine, obtains satisfactory effect.After producing and processing into preparation, in clinic
Upper small range is on probation, curative for effect.
According to the ginseng and pilose antler strengthening the essence tablet quality standard of formulation, guarantee the stability and curative effect of preparation.Ginseng and Radix Astragali are ginseng and pilose antler
Main flavour of a drug in strengthening the essence piece, this law is using ginsenoside Rg in high-efficient liquid phase technique other side1Assay is carried out with Re, with thin layer color
Spectrum is respectively to ginseng and Radix Astragali Qualitive test.The long-term stable experiment of preparation the result shows that, in 24 months, the quality of preparation without
Significant change provides strong evidence to formulate the validity period of preparation.
Summary of the invention
In view of this, technical problem to be solved by the invention is to provide a kind of method of quality control of ginseng and pilose antler strengthening the essence piece,
This method can fast and accurately identify the Radix Astragali and ginseng in ginseng and pilose antler strengthening the essence piece, and be joined by high effective liquid chromatography for measuring
Ginsenoside Rg in fine and soft strengthening the essence piece1With the content of ginsenoside Re.
The invention discloses a kind of ginseng and pilose antler strengthening the essence tablet quality control methods, carry out Radix Astragali identification including the use of thin-layered chromatography
Identify with ginseng；Ginsenoside Rg is carried out using high performance liquid chromatography1With ginsenoside Re's assay.
Further, the Radix Astragali discrimination method are as follows: ginseng and pilose antler strengthening the essence piece 3g is taken, coating is removed, it is finely ground at powder；To described
Methanol 20ml is added in powder, is heated to reflux 1h, filters, and filtrate is evaporated, and residue adds water 30ml to dissolve, and then uses n-butanol water saturation
Solution extracts 2 times, each 20ml, merges n-butanol extracting liquid, is washed with water the n-butanol extracting liquid 2 times, each 20ml, abandons
Aqueous is gone, the n-butanol liquid after washing is evaporated, residue adds methanol 0.5ml to dissolve, as test solution；
Astragaloside IV is taken, adds methanol that reference substance solution of every 1ml containing 1mg is made；
Take methanol as negative control solution；
It is tested according to thin-layered chromatography, draws above-mentioned each 2 μ l of three kinds of solution, put respectively on same silica gel g thin-layer plate, with body
Product is solvent in 10 DEG C of lower layer's solution arranged below than chloroform-methanol-water for 13:7:2, is unfolded, and takes out, dries in the air
It is dry, it sprays with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot development at 105 DEG C；
Silica gel g thin-layer plate is observed, is inspected under fluorescent lamp, in sample chromatogram, at the position corresponding to the chromatogram of the reference substance,
The sepia spot of aobvious same color.
Further, the ginseng discrimination method are as follows: ginseng and pilose antler strengthening the essence piece 5g is taken, coating is removed, it is finely ground at powder；It will be described
Powder is set in stuffed conical flask, and methanol 50ml is added, is heated to reflux 2h, lets cool, and is filtered, and is measured subsequent filtrate 25ml and is evaporated, residue
Add water 30ml to dissolve, extracted 2 times, each 30ml with chloroform, discards chloroform liquid, then shaken with n-butanol water saturation solution
Extraction 5 times, each 20ml is shaken, merges n-butanol extracting liquid, is washed 2 times, each 30ml with ammonia solution, then with n-butanol water saturation
Solution 30ml washing, takes n-butanol liquid to be evaporated, and residue adds methanol 1ml to dissolve, as test solution；
Take ginsenoside Rg_1 and Re that methanol is added every 1ml to be made respectively containing the mixed reference substance solution of 2mg,
Take methanol as negative control solution；
It is tested according to thin-layered chromatography, draws 10 μ l of the test solution, the 5 μ l of reference substance solution, negative control is molten
5 μ l of liquid, point are arranged below at 10 DEG C for n-butanol-ethyl acetate-water of 4:1:5 with volume ratio on same silica gel g thin-layer plate
Upper solution be solvent, be unfolded, take out, dry, spray with 10% ethanol solution of sulfuric acid, be heated to spot development at 105 DEG C
Clearly；
Silica gel g thin-layer plate is observed, sets and is inspected under fluorescent lamp, in sample chromatogram, in position corresponding with reference substance chromatography
On, show the spot of same color.
Further, the ginsenoside Rg1With ginsenoside Re's content assaying method are as follows:
Chromatographic condition and system suitability: using octadecylsilane chemically bonded silica as filler；It is flowing with acetonitrile
Phase A carries out gradient elution using water as Mobile phase B；Column temperature is 40 DEG C；Flow velocity 1.0ml/min, Detection wavelength 203nm, it is theoretical
The number of plates calculates >=6000 by ginsenoside Rg1 peak；
The gradient are as follows:
| Time (min) | Mobile phase A % | Mobile phase B % |
| 0-45 | 18 | 82 |
| 45-70 | 18→28 | 82→72 |
| 70-100 | 28→40 | 72→60 |
The preparation of reference substance solution: precision weighs 0.2mg ginsenoside Rg respectively1Reference substance, ginsenoside Re's reference substance,
Add 1ml methanol, shake up be made mixed solution to get；
The preparation of test solution: taking ginseng and pilose antler strengthening the essence piece 10g, removes coating, finely ground to set in stuffed conical flask at powder,
Methanol 50ml is added, is heated to reflux 2h, lets cool, filters, measures subsequent filtrate 25ml and is evaporated, residue adds water 30ml to dissolve, with positive fourth
The shaking of alcohol water saturation solution is extracted 5 times, each 20ml, is merged n-butanol extracting liquid, is washed 2 times, each 30ml with ammonia solution, then
It is washed with n-butanol water saturation solution 30ml, n-butanol liquid is taken to be evaporated, residue adds methanol to dissolve and is transferred in 10ml measuring bottle, adds
Methanol dilution shakes up to scale, filters, take subsequent filtrate to get；
Measuring method: it is accurate respectively to draw reference substance solution and each 10 μ l of test solution, inject liquid chromatograph, record
Chromatogram, by external standard method with ginsenoside Rg in calculated by peak area test sample1With the total amount of ginsenoside Re, this product every contains people
Ginseng is with ginsenoside Rg1(C42H72O14) and ginsenoside Re (C48H82O18) total amount meter be no less than 0.20mg.
Compared with prior art, the present invention can be obtained including following technical effect:
1) ginseng and pilose antler strengthening the essence tablet quality control method of the invention provides the method for identifying ginseng and Radix Astragali in drug, and
Use in high-efficient liquid phase technique other side main flavour of a drug ginseng with ginsenoside Rg1(C42H72O14) and ginsenoside Re (C48H82O18) be
Index carries out assay.
2) method of quality control of the invention can preferably control the quality of drug, have stronger specificity and good
It is effective, quality controllable really to embody drug safety for reproducibility.
Certainly, implementing any of the products of the present invention must be not necessarily required to reach all the above technical effect simultaneously.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present invention, constitutes a part of the invention, this hair
Bright illustrative embodiments and their description are used to explain the present invention, and are not constituted improper limitations of the present invention.In the accompanying drawings:
Fig. 1 show Radix Astragali in the embodiment of the present invention 1 and identifies thin-layer chromatogram (fluorescent lamp)；
Fig. 2 show ginseng in the embodiment of the present invention 2 and identifies thin-layer chromatogram (fluorescent lamp)；
Fig. 3 show ginsenoside Rg in the embodiment of the present invention 31With ginsenoside Re's assay reference substance efficient liquid phase
Chromatogram；
Fig. 4 show ginsenoside Rg in the embodiment of the present invention 31With ginsenoside Re's assay test sample efficient liquid phase
Chromatogram；
Fig. 5 show ginsenoside Rg in the embodiment of the present invention 31With the efficient liquid of ginsenoside Re's assay negative control
Phase chromatogram.
Specific embodiment
Carry out the embodiment that the present invention will be described in detail below in conjunction with accompanying drawings and embodiments, how the present invention is applied whereby
Technological means solves technical problem and reaches the realization process of technical effect to fully understand and implement.
Embodiment 1, the identification of Radix Astragali
Ginseng and pilose antler strengthening the essence piece 3g is taken, coating is conventionally removed, it is finely ground at powder, methanol 20ml is added into powder,
It is heated to reflux 1h, is filtered, filtrate is evaporated, and residue adds water 30ml to dissolve, and then uses n-butanol water saturation solution extraction 2 times, every time
20ml, merge n-butanol extracting liquid, be washed with water n-butanol extracting liquid 2 times, each 20ml discards aqueous, by after washing just
Butanol liquid is evaporated, and residue adds methanol 0.5ml to dissolve, as test solution.
Astragaloside IV is taken, adds methanol that reference substance solution of every 1ml containing 1mg is made.
Take methanol as negative control solution.
It is tested according to thin-layered chromatography, draws above-mentioned each 2 μ l of three kinds of solution, put respectively on same silica gel g thin-layer plate, with three
Chloromethanes-methanol-water (volume ratio 13:7:2) is solvent in 10 DEG C of lower layer's solution arranged below, is unfolded, and takes out, dries in the air
Dry, with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot development at 105 DEG C for spray, inspects silica gel g thin-layer plate under fluorescent light.
Inspect result under fluorescent lamp as shown in Figure 1, in figure 1 be Astragaloside IV reference substance, 2,3,4 be test sample, 5 for feminine gender
Control sample.In figure in sample chromatogram, on position corresponding with Astragaloside IV reference substance chromatography, the spot of same color is shown
Point.In negative control sample chromatography, on Astragaloside IV reference substance chromatography corresponding position, corresponding spot is had no.Show to join
Contain Radix Astragali in fine and soft strengthening the essence piece.
Embodiment 2, the identification of ginseng
Ginseng and pilose antler strengthening the essence piece 5g is taken, coating is conventionally removed, it is finely ground to be set in stuffed conical flask at powder, first is added
Alcohol 50ml, is heated to reflux 2h, lets cool, filtration, measures subsequent filtrate 25ml and is evaporated, and residue adds water 30ml to dissolve, and is transferred to liquid separation leakage
It in bucket, is extracted 2 times, each 30ml with chloroform shaking, discards chloroform liquid, then mentioned with the shaking of n-butanol water saturation solution
It takes 5 times, each 20ml, merges n-butanol extracting liquid, washed 2 times, each 30ml with ammonia solution, then with n-butanol water saturation solution
30ml washing, takes n-butanol liquid to be evaporated, and residue adds methanol 1ml to dissolve, as test solution.
Ginsenoside Rg_1 and Re is taken to add methanol that every 1ml is made respectively containing the mixed reference substance solution of 2mg.
Take methanol as negative control solution.
It is tested according to thin-layered chromatography, draws 10 μ l of test solution, 5 μ l point of reference substance solution is in same silica gel g thin-layer plate
On, using n-butanol-ethyl acetate-water (volume ratio 4:1:5) in 10 DEG C of upper solutions arranged below as solvent, expansion,
It takes out, dries, with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot development at 105 DEG C for spray, inspects under fluorescent light.Solvent
As negative control.
As a result as shown in Fig. 2, in figure 1 be ginsenoside Rg1, Re mixing reference substance, 2,3,4 be test sample, and 5 be negative right
Product in the same old way.In figure in sample chromatogram, with ginsenoside Rg1, on the corresponding position of Re mixing reference substance chromatography, show identical face
The spot of color.In negative control sample chromatography, with ginsenoside Rg1, on Re reference substance chromatography corresponding position, have no corresponding
Spot.Show to contain ginseng in ginseng and pilose antler strengthening the essence piece.
Embodiment 3, ginsenoside Rg1With ginsenoside Re's assay
(1) method of assay
Ginseng is main flavour of a drug in ginseng and pilose antler strengthening the essence piece, and this law uses in high-efficient liquid phase technique other side ginseng with ginsenoside Rg1
It is that index carries out assay with ginsenoside Re.
Chromatographic condition and system suitability: using octadecylsilane chemically bonded silica as filler；It is flowing with acetonitrile
Phase A carries out gradient elution using water as Mobile phase B；Column temperature is 40 DEG C；Flow velocity 1.0ml/min, Detection wavelength 203nm, it is theoretical
The number of plates calculates >=6000 by ginsenoside Rg1 peak.
The gradient are as follows:
The preparation of reference substance solution: precision weighs 0.2mg ginsenoside Rg respectively1Reference substance, ginsenoside Re's reference substance,
Add 1ml methanol, shake up be made mixed solution to get.
The preparation of test solution: taking ginseng and pilose antler strengthening the essence piece 10g, conventionally removes coating, finely ground at powder, sets tool
It fills in conical flask, methanol 50ml is added, is heated to reflux 2h, lets cool, filter, measure subsequent filtrate 25ml and be evaporated, residue adds water 30ml
Dissolution, is transferred in separatory funnel, is extracted 5 times, each 20ml with the shaking of n-butanol water saturation solution, merges n-butanol and extracts
Liquid is washed 2 times, each 30ml with ammonia solution, then is washed with n-butanol water saturation solution 30ml, takes n-butanol liquid to be evaporated, residue
Add methanol to dissolve and be transferred in 10ml measuring bottle, methanol dilution is added to shake up to scale, filter, take subsequent filtrate to get.
Measuring method: the accurate each 10 μ l of test solution and control solution that draws is injected separately into liquid chromatograph respectively,
Measurement records chromatogram, goes out ginsenoside Rg in test sample by external standard method with calculated by peak area1With the total amount of ginsenoside Re.
This product every containing ginseng with ginsenoside Rg1(C42H72O14) and ginsenoside Re (C48H82O18) total amount meter it is many
In 0.20mg.
(2) methodological study of assay
The determination of 2.1 Detection wavelengths
Ginsenoside Rg1Without absorption maximum within the scope of 200-400nm, there are absorption, the selected detection of bibliography in end
Wavelength is 203nm.
2.2 system suitability
Under above-mentioned chromatographic condition, take reference substance solution, test solution and negative control solution (solvent) respectively, respectively into
10 μ l of sample, records chromatogram, and measurement result is as in Figure 3-5.Ginsenoside Rg in sample1Theoretical cam curve calculates: n=
16450 (> 6000)；The separating degree of main peak and impurity peaks is 1.455；Negative control solution is at reference substance absorption peak without absorption；
It is smaller to show that auxiliary material and various decomposition products interfere main peak, meets the requirement of system suitability.
The test of 2.3 linear relationships
Accurately weighed ginsenoside Rg respectively1Reference substance and ginsenoside Re's reference substance are placed in same measuring bottle, prepare adult
Join saponin(e Rg1, ginsenoside Re mixed reference substance solution (contain ginsenoside Rg1It is for 0.53mg/ml, ginsenoside Re
0.37mg/ml), accurate respectively to measure 1,2,3,4,5ml, it is placed in 10ml measuring bottle, adds dilution in acetonitrile to scale, shake up.It is accurate
Each 10 μ l of above-mentioned solution is measured, liquid chromatograph is injected separately into according to above-mentioned chromatographic condition, measures peak area.It is right with peak area (Y)
Sample introduction concentration (X, mg/ml) carries out linear regression, ginsenoside Rg1Regression equation is Y=840083x-3421.2, related coefficient
R=0.9999；Ginsenoside Re's regression equation be Y=891838x-1660, coefficient R=0.9999. the result shows that, ginseng
Saponin(e Rg1 concentration is within the scope of 0.053-0.265mg/ml, and ginsenoside Re's concentration is within the scope of 0.037-0.185mg/ml, peak
Area is good with concentration linear relationship, the results are shown in Table 1.
1 ginsenoside Rg of table1With ginsenoside Re's linear relationship test result
2.4 minimum detectable activity
No. 1 solution under item is tested in line taking sexual intercourse, and precision measures 2ml, sets in 10ml measuring bottle, mobile phase is added to be diluted to quarter
Degree, shakes up, and precision measures 10 μ l, is injected separately into liquid chromatograph, measures, in chromatogram, signal-to-noise ratio > 10:1, so minimum inspection
Output < 0.2 μ g/ml.
2.5 precision test
No. 3 solution under item are tested in line taking sexual intercourse, and precision measures 10 μ l, METHOD FOR CONTINUOUS DETERMINATION 6 times, the results are shown in Table 2, show this
Method precision is good.
2 Precision test result of table
2.6 stability test
Ginseng and pilose antler strengthening the essence piece is taken, is prepared into test solution by method below content determination item；Precision draw test solution with
Reference substance solution, distinguishes sample introduction in 0h, 1h, 2h, 4h, 8h and for 24 hours, and each 10 μ l of sample volume records peak area value.It the results are shown in Table
3, reference substance and sample test liquid are good in internal stability for 24 hours.
3 stability test result of table
| Measure number | Ginsenoside Rg1Peak area | Ginsenoside Re's peak area |
| 0 | 364589 | 300214 |
| 1 | 359831 | 303279 |
| 2 | 363962 | 297205 |
| 4 | 367921 | 298965 |
| 8 | 366965 | 303816 |
| 24 | 361918 | 299018 |
| Average value | 364198 | 300416 |
| RSD% | 0.83 | 0.87 |
2.7 reappearance test
Ginseng and pilose antler strengthening the essence piece is taken, 6 parts of test solutions are prepared by method below content determination item, respectively by below content determination item
Method measurement, calculates content.It the results are shown in Table 4, sample average content is 0.293mg/ml, RSD=0.89%, and investigated method repeats
Property is good.
4 reproducible test results of table
| Measure number | 1 | 2 | 3 | 4 | 5 | 6 |
| Total content (mg/ piece) | 0.291 | 0.294 | 0.296 | 0.295 | 0.293 | 0.289 |
2.8 recovery test
The sample of known content is taken, it is finely ground, 1g is taken, it is accurately weighed, add ginsenoside Rg1Reference substance solution (0.53mg/
Ml) 1ml and ginsenoside Re's reference substance solution (0.37mg/ml) 1ml is prepared by sample solution preparation method, measures peak face
Product calculates measured amount, the results are shown in Table 5, the sample average rate of recovery is 99.30%, RSD 1.04%.
5 recovery test result of table
Ginseng and pilose antler strengthening the essence tablet quality control method of the invention provides the method for identifying ginseng and Radix Astragali in drug, and adopts
With flavour of a drug ginseng main in high-efficient liquid phase technique other side with ginsenoside Rg1(C42H72O14) and ginsenoside Re (C48H82O18) it is to refer to
Mark carries out assay.Method of quality control of the invention can preferably control the quality of drug, have stronger specificity and
It is effective, quality controllable really to embody drug safety for good reproducibility.
As used some vocabulary in the specification and claims to censure special component or method.Art technology
Personnel are, it is to be appreciated that different regions may call the same ingredient with different nouns.This specification and claims are not
In such a way that the difference of title is as ingredient is distinguished.As the "comprising" mentioned by throughout the specification and claims is
One open language, therefore should be construed to " including but not limited to "." substantially " refer within the acceptable error range, this field
Technical staff can solve the technical problem within a certain error range, basically reach the technical effect.Specification is subsequent
It is described as implementing better embodiment of the invention, so the description is for the purpose of illustrating rule of the invention, not
To limit the scope of the invention.Protection scope of the present invention is as defined by the appended claims.
It should also be noted that, the terms "include", "comprise" or its any other variant are intended to nonexcludability
Include, so that commodity or system including a series of elements not only include those elements, but also including not clear
The other element listed, or further include for this commodity or the intrinsic element of system.In the feelings not limited more
Under condition, the element that is limited by sentence "including a ...", it is not excluded that in the commodity or system for including the element also
There are other identical elements.
Several preferred embodiments of the invention have shown and described in above description, but as previously described, it should be understood that the present invention
Be not limited to forms disclosed herein, should not be regarded as an exclusion of other examples, and can be used for various other combinations,
Modification and environment, and the above teachings or related fields of technology or knowledge can be passed through within that scope of the inventive concept describe herein
It is modified.And changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention, then it all should be in this hair
In the protection scope of bright appended claims.
Claims (1)
1. ginseng and pilose antler strengthening the essence tablet quality control method, which is characterized in that carry out Radix Astragali identification and ginseng including the use of thin-layered chromatography
Identify；Ginsenoside Rg1 and ginsenoside Re's assay are carried out using high performance liquid chromatography；
The ginseng discrimination method are as follows: ginseng and pilose antler strengthening the essence piece 5g is taken, coating is removed, it is finely ground at powder；The powder is set into tool plug cone
In shape bottle, methanol 50ml being added, is heated to reflux 2h, lets cool, filter, measures subsequent filtrate 25ml and be evaporated, residue adds water 30ml to dissolve,
It is extracted 2 times, each 30ml with chloroform, discards chloroform liquid, then with the shaking of n-butanol water saturation solution extraction 5 times, often
Secondary 20ml merges n-butanol extracting liquid, is washed 2 times, each 30ml with ammonia solution, then washed with n-butanol water saturation solution 30ml
It washs, n-butanol liquid is taken to be evaporated, residue adds methanol 1ml to dissolve, as test solution；
Ginsenoside Rg_1 and Re is taken to add methanol that every 1ml is made respectively containing the mixed reference substance solution of 2mg；
Take methanol as negative control solution；
It is tested according to thin-layered chromatography, draws test solution 10 the μ l, the 5 μ l of reference substance solution, 5 μ of negative control solution
L, point are arranged below upper at 10 DEG C for n-butanol-ethyl acetate-water of 4:1:5 with volume ratio on same silica gel g thin-layer plate
Layer solution is solvent, is unfolded, and takes out, dries, and sprays with 10% ethanol solution of sulfuric acid, it is clear to be heated to spot development at 105 DEG C；
Silica gel g thin-layer plate is observed, sets and is inspected under fluorescent lamp, in sample chromatogram, at the position corresponding to the chromatogram of the reference substance, is shown
The spot of same color;
The Radix Astragali discrimination method are as follows: ginseng and pilose antler strengthening the essence piece 3g is taken, coating is removed, it is finely ground at powder；Methanol is added to the powder
20ml is heated to reflux 1h, and filtration, filtrate is evaporated, and residue adds water 30ml to dissolve, and is then extracted 2 times with n-butanol water saturation solution,
Each 20ml merges n-butanol extracting liquid, the n-butanol extracting liquid is washed with water 2 times, each 20ml discards aqueous, will wash
N-butanol liquid after washing is evaporated, and residue adds methanol 0.5ml to dissolve, as test solution；
Astragaloside IV is taken, adds methanol that reference substance solution of every 1ml containing 1mg is made；
Take methanol as negative control solution；
It is tested according to thin-layered chromatography, draws above-mentioned each 2 μ l of three kinds of solution, put respectively on same silica gel g thin-layer plate, with volume ratio
In 10 DEG C of lower layer's solution arranged below it is solvent for chloroform-methanol-water of 13:7:2, is unfolded, take out, dry, sprays
With 10% ethanol solution of sulfuric acid, it is clear that spot development is heated at 105 DEG C；
Silica gel g thin-layer plate is observed, is inspected under fluorescent lamp, in sample chromatogram, at the position corresponding to the chromatogram of the reference substance, shows phase
With the sepia spot of color;
The ginsenoside Rg1 and ginsenoside Re's content assaying method are as follows:
Chromatographic condition and system suitability: using octadecylsilane chemically bonded silica as filler；Using acetonitrile as mobile phase A,
Using water as Mobile phase B, gradient elution is carried out；Column temperature is 40 DEG C；Flow velocity 1.0ml/min, Detection wavelength 203nm, theoretical tray
Number calculates >=6000 by ginsenoside Rg1 peak；
The gradient are as follows:
The preparation of reference substance solution: precision weighs 0.2mg ginsenoside Rg1 reference substance, ginsenoside Re's reference substance respectively, adds
1ml methanol, shake up be made mixed solution to get；
The preparation of test solution: taking ginseng and pilose antler strengthening the essence piece 10g, removes coating, finely ground to set in stuffed conical flask at powder, is added
Methanol 50ml, is heated to reflux 2h, lets cool, filtration, measures subsequent filtrate 25ml and is evaporated, residue adds water 30ml to dissolve, with n-butanol water
Saturated solution shaking is extracted 5 times, each 20ml, is merged n-butanol extracting liquid, is washed 2 times, each 30ml with ammonia solution, then with just
Butanol water saturation solution 30ml washing, takes n-butanol liquid to be evaporated, residue adds methanol to dissolve and is transferred in 10ml measuring bottle, adds methanol
Be diluted to scale, shake up, filter, take subsequent filtrate to get；
Measuring method: it is accurate respectively to draw reference substance solution and each 10 μ l of test solution, liquid chromatograph is injected, chromatography is recorded
Figure, by external standard method with the total amount of ginsenoside Rg1 and ginsenoside Re in calculated by peak area test sample, this product every containing ginseng with
The total amount meter of ginsenoside Rg1 and ginsenoside Re are no less than 0.20mg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710007091.5A CN106770832B (en) | 2017-01-05 | 2017-01-05 | Ginseng and pilose antler strengthening the essence tablet quality control method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710007091.5A CN106770832B (en) | 2017-01-05 | 2017-01-05 | Ginseng and pilose antler strengthening the essence tablet quality control method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106770832A CN106770832A (en) | 2017-05-31 |
| CN106770832B true CN106770832B (en) | 2019-03-29 |
Family
ID=58949655
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710007091.5A Expired - Fee Related CN106770832B (en) | 2017-01-05 | 2017-01-05 | Ginseng and pilose antler strengthening the essence tablet quality control method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106770832B (en) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008180539A (en) * | 2007-01-23 | 2008-08-07 | Kowa Co | Confirmation method of gincenoside in medicine preparation |
| ITMI20121727A1 (en) * | 2012-10-12 | 2014-04-13 | Indena Spa | FORMULATIONS FOR TREATMENT AND PREVENTION OF OBESITY |
| CN104483315A (en) * | 2014-11-14 | 2015-04-01 | 颈复康药业集团赤峰丹龙药业有限公司 | Traditional Chinese medicine preparation lumbus-strengthening kidney-tonifying pill detection method |
| CN104991022A (en) * | 2015-07-07 | 2015-10-21 | 中国人民解放军第一五二中心医院 | Kidney health oral liquid quality control method |
-
2017
- 2017-01-05 CN CN201710007091.5A patent/CN106770832B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN106770832A (en) | 2017-05-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105477166B (en) | A kind of preparation method and its method of quality control of duhuo jisheng decoction granule | |
| CN101513519B (en) | Chinese medicinal composition for invigorating Qi and nourishing blood, preparation method and quality control method thereof | |
| CN110455965A (en) | The preparation method and its HPLC fingerprint of pharmaceutical composition | |
| CN109342631A (en) | The construction method of the HPLC finger-print of Chinese medicine composition and the quality determining method of Chinese medicine composition | |
| CN103285306B (en) | Preparation method and detection method of traditional Chinese medicine composition for benefiting Qi and tonifying kidney | |
| CN102218122B (en) | Detection method for sea dragon and gecko oral liquid | |
| CN101496870B (en) | Chinese medicinal composition for resolving phlegm and suppressing cough as well as preparation method and quality control method thereof | |
| CN106324161A (en) | Quality detection method for traditional Chinese medicine composition capable of treating diabetic nephropathy | |
| CN103344737A (en) | Quality control method of traditional Chinese medicine tablet for treating nasosinusitis | |
| CN103169864B (en) | Zengye Tang granule and preparation method thereof, purposes and detection method | |
| CN101204434A (en) | Quality standard for thrombus dispelling pill and test method thereof | |
| CN102068598B (en) | Quality control method of Yangrong Baicao Wan for treating irregular menses caused by hemophthisis | |
| CN106370756A (en) | Detection method of traditional Chinese medicine preparation for preventing infectious bronchitis | |
| CN106770832B (en) | Ginseng and pilose antler strengthening the essence tablet quality control method | |
| CN112285241A (en) | Method for constructing HPLC fingerprint of adenophora stricta and ophiopogon japonicus decoction | |
| CN101391070B (en) | Quality control method of traditional Chinese medicine composition with anti-tumor action | |
| CN109298124A (en) | A kind of thin-layered chromatography detection method of ginseng and astragalus stomach strengthening granules | |
| CN101269203A (en) | Quality control testing method for brain-invigorating and heart-soothing capsule | |
| CN104458954B (en) | A kind of dodder formulation granule finger printing and method for building up thereof | |
| CN106728651A (en) | The preparation method and its method of quality control of a kind of rhizoma cyperi SIWU KELI | |
| CN112526045B (en) | Method for simultaneously detecting or identifying effective components in heart-soothing and lipid-lowering tablets | |
| CN107064402B (en) | A kind of nourishing qi and blood, tonifying kidney and strengthening yang pharmaceutical preparation detection method | |
| CN110095547A (en) | The detection method of paeoniflorin content in a kind of body strengthening paste that lengthens one's life | |
| CN101920001B (en) | Finger-print quality determination method on wuji powder preparation and intermediate thereof | |
| CN101422588A (en) | Quality control method of medicine for treating gynecologic disease |
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 | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190329 Termination date: 20200105 |