CN106770832A - 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
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Abstract
The invention discloses a kind of ginseng and pilose antler strengthening the essence tablet quality control method, using the Radix Astragali and ginseng in thin-layered chromatography discriminating medicine；Using main active ginsenoside Rg in high effective liquid chromatography for measuring medicine1(C42H72O14) and ginsenoside Re (C48H82O18) content.Ginseng and pilose antler strengthening the essence tablet quality control method of the invention, with stronger specificity and good reappearance, can better control over drug quality, really meet effective, the quality controllable requirement of drug safety.
Description
Technical field
The invention belongs to technical field of pharmaceuticals, specifically, it is related to a kind of ginseng and pilose antler strengthening the essence tablet quality control method.
Background technology
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 is the common method of current clinical treatment malignant tumour.But radiation and chemotherapy is being controlled
Often cause serious side effect while treatment, cause the symptoms such as Neuroleptic Leukocytopenia, hemoglobin reduction.According to another report, China's hepatitis,
The hepatitis B incidence of disease shows lasting ascendant trend, accounts for the 20% of outpatient service viral hepatitis patient's total amount, causes 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, many
Number patient goes to a doctor in cirrhosis compensatory phase, Decompensated stage, has missed best occasion for the treatment, and prognosis is poor.Hepatitis B be widely current in
Countries in the world, seriously threaten human health, main to invade children and person between twenty and fifty, and 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 that current China is popular the most extensively, harmfulness most serious diseases it
One.Interferon and Ribavirin are usually used in the clinical treatment of hepatitis and hepatitis B, but often cause patient 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 Mingsan of China is instructed；The party by American Ginseng, the Radix Astragali, the fruit of glossy privet, when
Return, the red sage root, the bighead atractylodes rhizome, Chinese yam, the fruit of Chinese magnoliavine, garden burnet, hawthorn, cynomorium songaricum, pilose antler, the tuber of dwarf lilyturf, the 14 taste Chinese medicines such as the fruit of Chinese wolfberry are constituted.Its work(
Can be veins takes off admittedly, tonifying spleen benefit liver, blood-nourishing of promoting the production of body fluid, 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 Neuroleptic Leukocytopenia occurred after person's conventional therapy or tumor patient chemicotherapy, hemoglobin is low and altitude sickness and indigestion
Etc. symptom.14 medicines are shared, collect veins takes off admittedly, tonifying spleen benefit liver, blood-nourishing of promoting the production of body fluid, tranquilize the mind and promote the intelligence invigorating kidney yang, benefiting essence-blood, strengthening the bones and muscles it
Work(is both paid attention to dredging vascular in one, to improve internal organs blood supply, human body allomeric function and metabolism can be improved again, reaches righting and dispels
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 tried out, determined curative effect.
According to the ginseng and pilose antler strengthening the essence tablet quality standard formulated, it is ensured that the stability and curative effect of preparation.Ginseng and the 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 result of preparation shows, in 24 months, the quality of preparation without
Significant change, for the term of validity for formulating preparation provides strong evidence.
The content of the invention
In view of this, the technical problems to be solved by the invention are to provide a kind of method of quality control of ginseng and pilose antler strengthening the essence piece,
The method can fast and accurately differentiate 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 method, Radix Astragali discriminating is carried out using thin-layered chromatography
Differentiate with ginseng；Ginsenoside Rg is carried out using high performance liquid chromatography1With ginsenoside Re's assay.
Further, the Radix Astragali discrimination method is：Ginseng and pilose antler strengthening the essence piece 3g is taken, is removed and is coated, it is finely ground into powder；To described
Powder adds methyl alcohol 20ml, is heated to reflux 1h, filters, and filtrate is evaporated, and residue adds water 30ml dissolvings, then uses n-butanol water saturation
Solution is extracted 2 times, each 20ml, merges n-butanol extracting liquid, washes the n-butanol extracting liquid with water 2 times, and each 20ml is abandoned
Aqueous are gone, the n-butanol liquid after washing is evaporated, residue adds methyl alcohol 0.5ml to dissolve, used as need testing solution；
Astragaloside IV is taken, plus methyl alcohol is made reference substance solutions of every 1ml containing 1mg；
Methyl alcohol is taken as negative control solution；
According to thin-layered chromatography experiment, above-mentioned each 2 μ l of three kinds of solution are drawn, put respectively on same silica gel g thin-layer plate, with body
Product is than being 13:7:2 chloroform-methanol-water is solvent in 10 DEG C of lower floor's solution arranged below, is launched, and is taken out, and is dried in the air
It is dry, spray with 10% ethanol solution of sulfuric acid, it is heated to spot development at 105 DEG C clear；
Observation silica gel g thin-layer plate, inspects under fluorescent lamp, in test sample chromatogram, on position corresponding with reference substance chromatogram,
The sepia spot of aobvious same color.
Further, the ginseng discrimination method is：Ginseng and pilose antler strengthening the essence piece 5g is taken, is removed and is coated, it is finely ground into powder；Will be described
Powder is put in conical flask with cover, adds methyl alcohol 50ml, is heated to reflux 2h, lets cool, and filters, and measures subsequent filtrate 25ml and is evaporated, residue
The 30ml that adds water dissolves, and is extracted 2 times with chloroform, and each 30ml discards chloroform liquid, then shaken with n-butanol water saturation solution
Extraction 5 times is shaken, each 20ml merges n-butanol extracting liquid, washed with ammonia solution 2 times, each 30ml, then use n-butanol water saturation
Solution 30ml is washed, and is taken n-butanol liquid and is evaporated, and residue adds methyl alcohol 1ml to dissolve, used as need testing solution；
Take ginsenoside Rg_1 and Re plus methyl alcohol be made every 1ml respectively mixed reference substance solutions containing 2mg,
Methyl alcohol is taken as negative control solution；
According to thin-layered chromatography experiment, the μ l of need testing solution 10 are drawn, the μ l of the reference substance solution 5, negative control is molten
The μ l of liquid 5, put on same silica gel g thin-layer plate, are 4 with volume ratio:1:5 n-butanol-ethyl acetate-water is arranged below at 10 DEG C
Upper solution be solvent, launch, take out, dry, spray with 10% ethanol solution of sulfuric acid, be heated to spot development at 105 DEG C
Clearly；
Observation silica gel g thin-layer plate, puts and inspect under fluorescent lamp, in test sample chromatogram, in position corresponding with reference substance chromatogram
On, show the spot of same color.
Further, the ginsenoside Rg1It is with ginsenoside Re's content assaying method：
Chromatographic condition and system suitability：With octadecylsilane chemically bonded silica as filler；It is flowing with acetonitrile
Phase A, with water as Mobile phase B, carries out gradient elution；Column temperature is 40 DEG C；Flow velocity 1.0ml/min, Detection wavelength is 203nm, theoretical
The number of plates calculates >=6000 by ginsenoside Rg1 peak；
The gradient is：
| 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 Rgs respectively1Reference substance, ginsenoside Re's reference substance,
Plus 1ml methyl alcohol, shake up and be made mixed solution, obtain final product；
The preparation of need testing solution：Take ginseng and pilose antler strengthening the essence piece 10g, remove and be coated, it is finely ground into powder, in putting conical flask with cover,
Add methyl alcohol 50ml, be heated to reflux 2h, let cool, filter, measure subsequent filtrate 25ml and be evaporated, residue add water 30ml dissolving, use positive fourth
The shaking of alcohol water saturation solution is extracted 5 times, and each 20ml merges n-butanol extracting liquid, is washed with ammonia solution 2 times, each 30ml, then
Washed with n-butanol water saturation solution 30ml, take n-butanol liquid and be evaporated, residue adds methyl alcohol to dissolve and be transferred in 10ml measuring bottles, plus
Methanol dilution shakes up to scale, filtration, takes subsequent filtrate, obtains final product；
Assay method：It is accurate respectively to draw reference substance solution and each 10 μ l of need testing 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 is containing 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 technique effect：
1) ginseng and pilose antler strengthening the essence tablet quality control method of the invention, there is provided the method for differentiating ginseng and the Radix Astragali in medicine, and
Main flavour of a drug ginseng is with ginsenoside Rg in using high-efficient liquid phase technique other side1(C42H72O14) and ginsenoside Re (C48H82O18) be
Index carries out assay.
2) method of quality control of the invention can better control over the quality of medicine, with stronger specificity and good
Reappearance, real embodiment drug safety is effective, quality controllable.
Certainly, implementing any product of the invention must be not necessarily required to while reaching all the above technique effect.
Brief description of the drawings
Accompanying drawing described herein is used for providing a further understanding of the present invention, constitutes a part of the invention, this hair
Bright schematic description and description does not constitute inappropriate limitation of the present invention for explaining the present invention.In the accompanying drawings：
The Radix Astragali differentiates thin-layer chromatogram (fluorescent lamp) during Fig. 1 show the embodiment of the present invention 1；
Ginseng differentiates thin-layer chromatogram (fluorescent lamp) during Fig. 2 show the embodiment of the present invention 2；
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 ginsenoside Re's efficient liquid of assay negative control
Phase chromatogram.
Specific embodiment
Describe embodiments of the present invention in detail below in conjunction with drawings and Examples, thereby how the present invention is applied
Technological means can fully understand and implement according to this to solve technical problem and reach the implementation process of technology effect.
Embodiment 1, the discriminating of the Radix Astragali
Ginseng and pilose antler strengthening the essence piece 3g is taken, is conventionally removed and is coated, it is finely ground into powder, to addition methyl alcohol 20ml in powder,
1h is heated to reflux, is filtered, filtrate is evaporated, residue adds water 30ml dissolvings, then extract 2 times with n-butanol water saturation solution, every time
20ml, merge n-butanol extracting liquid, wash n-butanol extracting liquid with water 2 times, each 20ml discards aqueous, by after washing just
Butanol liquid is evaporated, and residue adds methyl alcohol 0.5ml to dissolve, used as need testing solution.
Astragaloside IV is taken, plus methyl alcohol is made reference substance solutions of every 1ml containing 1mg.
Methyl alcohol is taken as negative control solution.
According to thin-layered chromatography experiment, above-mentioned each 2 μ l of three kinds of solution are drawn, put respectively on same silica gel g thin-layer plate, with three
(volume ratio is 13 to chloromethanes-methanol-water:7:2) it is solvent in 10 DEG C of lower floor's solution arranged below, launches, take out, dries in the air
It is dry, spray with 10% ethanol solution of sulfuric acid, spot development is heated at 105 DEG C clearly, silica gel g thin-layer plate is inspected 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 test sample chromatogram, on position corresponding with Astragaloside IV reference substance chromatogram, show the spot of same color
Point.In negative control sample chromatogram, with Astragaloside IV reference substance chromatogram relevant position on, have no corresponding spot.Show ginseng
Contain the Radix Astragali in fine and soft strengthening the essence piece.
Embodiment 2, the discriminating of ginseng
Ginseng and pilose antler strengthening the essence piece 5g is taken, is conventionally removed and is coated, it is finely ground into powder, put in conical flask with cover, add first
Alcohol 50ml, is heated to reflux 2h, lets cool, filtration, measures subsequent filtrate 25ml and is evaporated, and residue adds water 30ml dissolvings, is transferred to point liquid and leaks
In bucket, shaken with chloroform and extracted 2 times, each 30ml discards chloroform liquid, then carried with the shaking of n-butanol water saturation solution
Take 5 times, each 20ml, merge n-butanol extracting liquid, washed with ammonia solution 2 times, each 30ml, then with n-butanol water saturation solution
30ml is washed, and is taken n-butanol liquid and is evaporated, and residue adds methyl alcohol 1ml to dissolve, used as need testing solution.
Take ginsenoside Rg_1 and Re plus methyl alcohol is made every 1ml respectively mixed reference substance solutions containing 2mg.
Methyl alcohol is taken as negative control solution.
According to thin-layered chromatography experiment, the μ l of need testing solution 10 are drawn, the μ l points of reference substance solution 5 are in same silica gel g thin-layer plate
On, with n-butanol-ethyl acetate-water, (volume ratio is 4:1:5) it is solvent in 10 DEG C of upper solutions arranged below, launches,
Take out, dry, spray with 10% ethanol solution of sulfuric acid, spot development is heated at 105 DEG C clearly, inspect under fluorescent light.Solvent
As negative control.
Result as shown in Fig. 2 in figure 1 be ginsenoside Rg1, Re mixing reference substances, 2,3,4 is test sample, and 5 is negative right
Product in the same old way.In figure in test sample chromatogram, with ginsenoside Rg1, on the corresponding position of Re mixing reference substance chromatograms, show identical face
The spot of color.In negative control sample chromatogram, with ginsenoside Rg1, on Re reference substance chromatograms relevant 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, this law use high-efficient liquid phase technique other side in ginseng with ginsenoside Rg1
With ginsenoside Re for index carries out assay.
Chromatographic condition and system suitability：With octadecylsilane chemically bonded silica as filler；It is flowing with acetonitrile
Phase A, with water as Mobile phase B, carries out gradient elution；Column temperature is 40 DEG C；Flow velocity 1.0ml/min, Detection wavelength is 203nm, theoretical
The number of plates calculates >=6000 by ginsenoside Rg1 peak.
The gradient is：
The preparation of reference substance solution：Precision weighs 0.2mg ginsenoside Rgs respectively1Reference substance, ginsenoside Re's reference substance,
Plus 1ml methyl alcohol, shake up and be made mixed solution, obtain final product.
The preparation of need testing solution：Ginseng and pilose antler strengthening the essence piece 10g is taken, is conventionally removed and is coated, it is finely ground into powder, put tool
In plug conical flask, methyl alcohol 50ml is added, be heated to reflux 2h, let cool, filtered, measured subsequent filtrate 25ml and be evaporated, residue adds water 30ml
Dissolving, is transferred in separatory funnel, is shaken with n-butanol water saturation solution and extracted 5 times, each 20ml, 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, is taken n-butanol liquid and is evaporated, residue
Plus methyl alcohol dissolves and is transferred in 10ml measuring bottles, plus methanol dilution is to scale, shakes up, filtration, takes subsequent filtrate, obtains final product.
Assay method：Accurate absorption need testing solution and each 10 μ l of reference substance solution are injected separately into liquid chromatograph respectively,
Determine, record chromatogram, ginsenoside Rg in test sample is gone out with calculated by peak area by external standard method1With the total amount of ginsenoside Re.
This product every is 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 in the range of 200-400nm, there are absorption, the selected detection of bibliography in end
Wavelength is 203nm.
2.2 system suitabilities
Under above-mentioned chromatographic condition, reference substance solution, need testing solution and negative control solution (solvent) are taken respectively, respectively enter
The μ l of sample 10, record chromatogram, and measurement result is as in Figure 3-5.Ginsenoside Rg in sample1Theoretical cam curve is calculated：N=
16450 (＞ 6000)；Main peak is 1.455 with the separating degree of impurity peaks；Negative control solution is at reference substance absworption peak without absorption；
Show that auxiliary material and various catabolites disturb smaller to main peak, meet the requirement of system suitability.
2.3 linear relationships are tested
The accurately weighed ginsenoside Rg of difference1Reference substance and ginsenoside Re's reference substance, are placed in same measuring bottle, prepare adult
Ginseng saponin(e Rg1, ginsenoside Re mixed reference substance solution (contain ginsenoside Rg1For 0.53mg/ml, ginsenoside Re are
0.37mg/ml), respectively precision measure 1,2,3,4,5ml, be placed in 10ml measuring bottles, plus dilution in acetonitrile is to scale, shakes up.It is accurate
Each 10 μ l of above-mentioned solution are measured, liquid chromatograph is injected separately into according to above-mentioned chromatographic condition, determine 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, coefficient correlation
R=0.9999；Ginsenoside Re's regression equation is Y=891838x-1660, and coefficient R=0.9999. results show, ginseng
Saponin(e Rg1 concentration in the range of 0.053-0.265mg/ml, ginsenoside Re's concentration in the range of 0.037-0.185mg/ml, peak
Area is good with concentration linear relationship, the results are shown in Table 1.
The ginsenoside Rg of table 11With ginsenoside Re's linear relationship result of the test
2.4 minimum detectable activities
No. 1 solution under line taking sexual intercourse experiment item, precision measures 2ml, and in putting 10ml measuring bottles, plus mobile phase is diluted to quarter
Degree, shakes up, and precision measures 10 μ l, is injected separately into liquid chromatograph, determines, in chromatogram, signal to noise ratio ＞ 10:1, so minimum inspection
Output<0.2μg/ml.
2.5 precision tests
No. 3 solution under line taking sexual intercourse experiment item, precision measures 10 μ l, and METHOD FOR CONTINUOUS DETERMINATION 6 times the results are shown in Table 2, show this
Method precision is good.
The Precision test result of table 2
2.6 stability tests
Ginseng and pilose antler strengthening the essence piece is taken, need testing solution is prepared into by assay lower section method；Precision draw need testing solution with
Reference substance solution, sample introduction is distinguished in 0h, 1h, 2h, 4h, 8h and 24h, and the μ l of each sample size 10 record peak area value.The results are shown in Table
3, reference substance and sample test liquid are good in 24h internal stabilities.
The stability test result of table 3
| Determine number of times | 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 tests
Ginseng and pilose antler strengthening the essence piece is taken, 6 parts of need testing solutions is prepared by assay lower section method, respectively by assay lower section
Method is determined, and calculates content.4 are the results are shown in Table, sample average content is 0.293mg/ml, RSD=0.89%, investigate method repetition
Property is good.
The reproducible test results of table 4
| Determine number of times | 1 | 2 | 3 | 4 | 5 | 6 |
| Total content (mg/ pieces) | 0.291 | 0.294 | 0.296 | 0.295 | 0.293 | 0.289 |
2.8 recovery tests
The sample of known content is taken, it is finely ground, 1g is taken, it is accurately weighed, plus ginsenoside Rg1Reference substance solution (0.53mg/
Ml) 1ml and ginsenoside Re's reference substance solution (0.37mg/ml) 1ml, is prepared by need testing solution preparation method, determines peak face
Product, calculates measured amount, the results are shown in Table 5, and the sample average rate of recovery is 1.04% for 99.30%, RSD.
The recovery test result of table 5
Ginseng and pilose antler strengthening the essence tablet quality control method of the invention, there is provided differentiate the method for ginseng and the Radix Astragali in medicine, and adopt
With main flavour of a drug ginseng in high-efficient liquid phase technique other side with ginsenoside Rg1(C42H72O14) and ginsenoside Re (C48H82O18) it is finger
Mark carries out assay.Method of quality control of the invention can better control over the quality of medicine, with stronger specificity and
Good reappearance, real embodiment drug safety is effective, quality controllable.
Some vocabulary have such as been used to censure special component or method in the middle of specification and claim.Art technology
Personnel are, it is to be appreciated that different regions may call same composition with different nouns.This specification and claims are not
In the way of the difference of title is used as distinguishing composition.As the "comprising" of the specification in the whole text and claim mentioned in is
One open language, therefore " include but be not limited to " should be construed to." substantially " refer to this area in receivable error range
Technical staff can solve the technical problem in the range of certain error, basically reach the technique effect.Specification is follow-up
It is described as implementing better embodiment of the invention, so the description is for the purpose of illustrating rule of the invention, not
It is used to limit the scope of the present invention.Protection scope of the present invention ought be defined depending on the appended claims person of defining.
Also, it should be noted that term " including ", "comprising" or its any other variant be intended to nonexcludability
Comprising, so that commodity or system including a series of key elements not only include those key elements, but also including without clear and definite
Other key elements listed, or it is this commodity or the intrinsic key element of system also to include.In the feelings without more limitations
Under condition, the key element limited by sentence "including a ...", it is not excluded that in the commodity or system including the key element also
There is other identical element.
Described above has shown and described some preferred embodiments of the invention, but as previously described, it should be understood that the present invention
Be not limited to form disclosed herein, be not to be taken as the exclusion to other embodiment, and can be used for various other combinations,
Modification and environment, and can be in invention contemplated scope described herein, by above-mentioned teaching or the technology or knowledge of association area
It is modified.And the change and change that those skilled in the art are carried out do not depart from the spirit and scope of the present invention, then all should be in this hair
In the protection domain of bright appended claims.
Claims (4)
1. ginseng and pilose antler strengthening the essence tablet quality control method, it is characterised in that carry out Radix Astragali discriminating and ginseng using thin-layered chromatography
Differentiate；Ginsenoside Rg is carried out using high performance liquid chromatography1With ginsenoside Re's assay.
2. ginseng and pilose antler strengthening the essence tablet quality control method as claimed in claim 1, it is characterised in that the Radix Astragali discrimination method is：
Ginseng and pilose antler strengthening the essence piece 3g is taken, is removed and is coated, it is finely ground into powder；Methyl alcohol 20ml is added to the powder, 1h is heated to reflux, filtered, filter
Liquid is evaporated, and residue adds water 30ml dissolvings, is then extracted 2 times with n-butanol water saturation solution, each 20ml, merges n-butanol and extracts
Liquid, washes the n-butanol extracting liquid with water 2 times, and each 20ml discards aqueous, the n-butanol liquid after washing is evaporated, residue
Plus methyl alcohol 0.5ml dissolvings, as need testing solution；
Astragaloside IV is taken, plus methyl alcohol is made reference substance solutions of every 1ml containing 1mg；
Methyl alcohol is taken as negative control solution；
According to thin-layered chromatography experiment, above-mentioned each 2 μ l of three kinds of solution are drawn, put respectively on same silica gel g thin-layer plate, with volume ratio
It is 13:7:2 chloroform-methanol-water is solvent in 10 DEG C of lower floor's solution arranged below, is launched, and is taken out, and is dried, and is sprayed
With 10% ethanol solution of sulfuric acid, spot development is heated at 105 DEG C clear；
Observation silica gel g thin-layer plate, inspects under fluorescent lamp, in test sample chromatogram, on position corresponding with reference substance chromatogram, shows phase
With the sepia spot of color.
3. ginseng and pilose antler strengthening the essence tablet quality control method as claimed in claim 1, it is characterised in that the ginseng discrimination method is：
Ginseng and pilose antler strengthening the essence piece 5g is taken, is removed and is coated, it is finely ground into powder；During the powder put into conical flask with cover, methyl alcohol 50ml, heating are added
Backflow 2h, let cool, filter, measure subsequent filtrate 25ml and be evaporated, residue add water 30ml dissolving, with chloroform extract 2 times, every time
30ml, discards chloroform liquid, then shakes extraction 5 times with n-butanol water saturation solution, and each 20ml 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, is taken n-butanol liquid and is evaporated, residue
Plus methyl alcohol 1ml dissolvings, as need testing solution；
Take ginsenoside Rg_1 and Re plus methyl alcohol is made every 1ml respectively mixed reference substance solutions containing 2mg；
Methyl alcohol is taken as negative control solution；
According to thin-layered chromatography experiment, the μ l of need testing solution 10, the reference substance solution 5 μ l, the μ of negative control solution 5 are drawn
L, puts on same silica gel g thin-layer plate, is 4 with volume ratio:1:5 n-butanol-ethyl acetate-water is arranged below upper at 10 DEG C
Layer solution is solvent, is launched, and is taken out, and is dried, and is sprayed with 10% ethanol solution of sulfuric acid, is heated to spot development at 105 DEG C clear；
Observation silica gel g thin-layer plate, puts and inspect under fluorescent lamp, in test sample chromatogram, on position corresponding with reference substance chromatogram, shows
The spot of same color.
4. ginseng and pilose antler strengthening the essence tablet quality control method as claimed in claim 1, it is characterised in that the ginsenoside Rg1And ginseng
Saponin(e Re content assaying methods are：
Chromatographic condition and system suitability：With octadecylsilane chemically bonded silica as filler；With acetonitrile as mobile phase A,
With water as Mobile phase B, gradient elution is carried out；Column temperature is 40 DEG C；Flow velocity 1.0ml/min, Detection wavelength is 203nm, theoretical tray
Number calculates >=6000 by ginsenoside Rg1 peak；
The gradient is：
The preparation of reference substance solution：Precision weighs 0.2mg ginsenoside Rgs respectively1Reference substance, ginsenoside Re's reference substance, plus 1ml
Methyl alcohol, shakes up and is made mixed solution, obtains final product；
The preparation of need testing solution：Ginseng and pilose antler strengthening the essence piece 10g is taken, is removed and is coated, it is finely ground into powder, put in conical flask with cover, add
Methyl alcohol 50ml, is heated to reflux 2h, lets cool, filtration, measure subsequent filtrate 25ml and be evaporated, residue add water 30ml dissolving, use n-butanol water
Saturated solution shaking is extracted 5 times, and each 20ml merges n-butanol extracting liquid, is washed with ammonia solution 2 times, each 30ml, then with just
Butanol water saturation solution 30ml is washed, and is taken n-butanol liquid and is evaporated, and residue adds methyl alcohol to dissolve and be transferred in 10ml measuring bottles, plus methyl alcohol
Scale is diluted to, is shaken up, filtered, take subsequent filtrate, obtained final product；
Assay method：It is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, liquid chromatograph is injected, record chromatogram
Figure, by external standard method with ginsenoside Rg in calculated by peak area test sample1With the total amount of ginsenoside Re, this product every containing ginseng with
Ginsenoside Rg1Total amount meter with ginsenoside Re is no less than 0.20mg.
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Citations (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 |
| 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 |
| EP2906233A1 (en) * | 2012-10-12 | 2015-08-19 | Indena S.p.A. | Formulations for the treatment and prevention of obesity |
| 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 |
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| 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 |
| EP2906233A1 (en) * | 2012-10-12 | 2015-08-19 | Indena S.p.A. | Formulations for the 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 |
Non-Patent Citations (1)
| Title |
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| 国家药典委员会: "《中华人民共和国药典2010年版一部》", 31 January 2010 * |
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