CN109540896A - A kind of pair of hepatic injury has the method for quality control of defencive function Chinese medicinal capsule - Google Patents
A kind of pair of hepatic injury has the method for quality control of defencive function Chinese medicinal capsule Download PDFInfo
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
- G01N30/94—Development
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- G—PHYSICS
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- 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
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- G01N2030/062—Preparation extracting sample from raw material
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
Abstract
The invention discloses the method for quality control that a kind of pair of hepatic injury has defencive function Chinese medicinal capsule; quality controls are carried out using three kinds of methods are quantitative determined using microscopical characters, thin layer identification and functional component: 1) microscopical characters: taking this product content; microscopically observation is set after processing; elongated light brown mycelia is scattered distribution; in bending; and minority has bifurcated, diameter is about 3 to 7 microns.2) thin layer identifies: in sample chromatogram, on position corresponding with Radix Astragali reference substance chromatography, identical sepia spot is shown under daylight；Identical orange-yellow fluorescence spot is shown under ultraviolet lamp (365nm)；3) functional component quantitative determines: effective component schizandrin in high effective liquid chromatography for measuring capsule, and every gram of capsule 's content contains Schisandra chinensis in terms of schizandrin, no less than 0.5mg.Stability of the present invention is good, reproducible, and the rate of recovery is high, has stronger specificity.The present invention improves the quality standard that a kind of pair of hepatic injury has assistant protection function Chinese medicinal capsule.
Description
Technical field
The present invention relates to the field of Chinese medicines, have the quality of defencive function Chinese medicinal capsule to control more particularly to a kind of pair of hepatic injury
Method.
Background technique
It is pure Chinese medicine oral preparation that a kind of pair of hepatic injury, which has assistant protection function Chinese medicinal capsule, and verifying has by clinic application
Good protect liver effect has specific prevention and protective effect to Alcoholic, chemical damage, by pueraria lobata, hoveniae semoveniae semen, Huang
The Six-elements pure Chinese medicine medicinal material such as stilbene, ganoderma lucidum, Schisandra chinensis, galangal, a kind of Chinese medicine compound prescription glue being processed into through modern pharmaceutical technique
Capsule preparation.Due to chemical composition of Chinese materia medica complexity, the qualitative and quantitative control process of severe jamming Chinese materia medica preparation functional component, to protect
Demonstrate,proving a kind of pair of hepatic injury has the quality controllable of assistant protection function Chinese medicinal capsule and stablizes, and the present invention uses microscopical characters, thin layer
Identify and three kinds of methods of functional component assay carry out qualitative, quantitative quality control, is that a kind of specificity is strong, effective and accurate
Method of quality control.
The present invention uses microscopic identification method to have the ganoderma lucidum in assistant protection function Chinese medicinal capsule to a kind of pair of hepatic injury for the first time
Fructification is identified.Ganoderma lucidum fruitbody in addition to containing the basic nutritions such as polysaccharide and vegetable protein, also containing triterpenes, adenosine,
A variety of secondary metabolites such as alkaloids have concentrated the Major Nutrient and functional component of ganoderma lucidum, but ganoderma lucidum fruitbody has solid-state
Culture and two kinds of inoculation methods of liquid fermentation, since the solid state rheology time is longer than liquid fermentation, nutrition and functional component difference
Obviously, especially triterpenes functional component, solid state rheology is significantly higher than liquid fermentation, thus the present invention is established and trained for solid-state
The microscopical characters project of ganoderma lucidum fruitbody is supported, to control the quality of Chinese medicinal capsule of the present invention.
The present invention use thin layer differential method, in capsule Radix Astragali and its functional component Astragaloside IV carry out Qualitive test,
Due to the volatile oil oil compounds in prescription containing galangal, for eliminate liposoluble constituent in Chinese medicine capsule and other
Interference of the impurity to discrimination process, using ether grease removal, methanol extraction, extracting n-butyl alcohol, alkalization removal of impurities, macroporous resin purification etc.
Polishing purification step establishes thin layer and identifies pre-treating method, finally molten with the lower layer of methylene chloride-methanol-water (12:8:3)
Liquid is that solvent carries out thin-layer developing, selects environmental-friendly methylene chloride to substitute highly toxic chloroform, establishes thin layer
Development system, the thin-layer identification method specificity established are strong, effective and accurate.
The present invention uses high performance liquid chromatography, carries out quantitative survey to the Schisandra chinensis functional component schizandrin in capsule
It is fixed.In order to eliminate the influence in Chinese medicine capsule by volatile oil liposoluble constituent to quantitative determination, functional component is mentioned
It takes and diatomite is added in enrichment process, for adsorbing volatile oil liposoluble constituent, sample is measured with to reduce such components
Interference, can improve the specificity of quantitative determination well.
Summary of the invention
The purpose of the present invention is to provide the method for quality control that a kind of pair of hepatic injury has defencive function Chinese medicinal capsule, make to produce
Quality is controlled better.To achieve the above object, the invention adopts the following technical scheme: a kind of pair of hepatic injury has protection
The method of quality control of function Chinese medicinal capsule, which is characterized in that using microscopical characters, thin layer identifies and three kinds of methods of assay
Carry out quality control.
1) microscopical characters: taking capsule 's content, and No. 5 sieves are crossed after grinding, appropriate powder is selected to set on coverslip, hydration is added dropwise
Chloral test solution, covered, microscopically observation: elongated light brown mycelia is scattered distribution, is in bending, and minority has point
Fork, diameter is about 3 to 7 microns.
2) thin layer identifies: taking capsule 's content, powder 12g is taken after grinding, add diethyl ether 60ml, shakes 1 hour, filtration discards
Filtrate, dregs of a decoction methanol 60ml are heated to reflux 1 hour, filtration, and for filtrate recycling design to doing, residue adds water 30ml to make to dissolve, and are used
4 times (20ml, 20ml, 15ml, 15ml) is extracted in water saturated n-butanol shaking, merges n-butanol liquid, after being washed with ammonia solution, just
For butanol liquid recycling design to dry, residue adds water 20ml to make to dissolve, and lets cool, and by D101 type large pore resin absorption column, (column internal diameter is
1.5cm, pillar height 15cm), eluted with water 40ml, discard eluent, then with 40% ethyl alcohol 50ml elution, discard eluent, after with
Eluent is collected in 70% ethyl alcohol 50ml elution, and recycling design is to doing, and residue adds methanol 1ml to make to dissolve, as test solution.Separately
Milkvetch Root 3g is taken, control medicinal material solution is made in the same way of.Astragaloside IV reference substance is taken again, adds methanol that every 1ml is made containing the molten of 1mg
Liquid, as reference substance solution.According to thin-layered chromatography, above-mentioned three kinds of solution 5-10 μ l is drawn, is put respectively in same silica gel g thin-layer plate
On, using lower layer's solution of methylene chloride-methanol-water (12:8:3) as solvent, it is unfolded, takes out, dry, sprays with 10% sulfuric acid second
It is clear to be heated to spot development at 105 DEG C for alcoholic solution.Sample chromatogram should be with reference substance chromatography on a corresponding position, daylight
Under show identical sepia spot；Identical orange-yellow fluorescence spot is shown under ultraviolet lamp (365nm).
3) the effective component schizandrin in high effective liquid chromatography for measuring capsule:
The preparation method of reference substance solution: it is appropriate that precision weighs schizandrin reference substance, and methanol is added and is made containing schisandrol
The solution of first 0.15mg/mL, as reference substance solution.
The preparation method of test solution: taking this product content about 4g, accurately weighed, and 5g diatomite is added, and is uniformly mixed
In postposition Soxhlet extractor, add methanol 50mL, be heated to reflux 4 hours, extracting solution recycling design is simultaneously concentrated to dryness, and residue adds methanol
Dissolution, is transferred in 25ml measuring bottle, adds methanol to scale, shake up, with the organic membrane filtration of 0.45um, take subsequent filtrate to get sample
Product solution.
Measuring method is, accurate respectively to draw reference substance solution and each 10uL of test solution, injects liquid chromatograph, surveys
Determine to get chromatographic condition are as follows: using octadecylsilane chemically bonded silica as filler；[acetonitrile (A)-water is eluted using gradient
(B) gradient elution (0min:45%A → 25min:68%A → 40min:68%A → 60min:45%A) is carried out for mobile phase], detection
Wavelength is 250nm；Theoretical cam curve is calculated by schizandrin peak, should be not less than 3000；Every g capsule 's content is containing Schisandra chinensis with five
Taste alcohol first meter, no less than 0.5mg.
Advantages of the present invention is as follows: the present invention has defencive function Chinese medicinal capsule for a kind of pair of hepatic injury, has carried out Radix Astragali
Thin layer identify, the liquid phase of the schizandrin of Schisandra chinensis identifies and the liquid phase of the Astragaloside IV of Radix Astragali identifies.The present invention stablizes
Property it is good, reproducible, the rate of recovery is high, has stronger specificity.There is protection function to a kind of pair of hepatic injury by the method for the invention
Can Chinese medicinal capsule detected, improving a kind of pair of hepatic injury has the stability of quality of defencive function Chinese medicinal capsule and controllable
Property.
Detailed description of the invention
Fig. 1 is microscopical characters figure.
Fig. 2 is thin-layer chromatogram under daylight.
Fig. 3 is thin-layer chromatogram under ultraviolet lamp (365nm): 1 a kind of pair of hepatic injury has defencive function Chinese medicinal capsule
00DJD01；2 Radix Astragali control medicinal materials；3 Astragaloside IV reference substances；4 a kind of pairs of hepatic injuries have defencive function Chinese medicinal capsule 00DJD02.
Fig. 4 is that a kind of pair of hepatic injury has defencive function Chinese medicinal capsule schizandrin reference substance map.
Fig. 5 is that a kind of pair of hepatic injury has defencive function Chinese medicinal capsule sample schizandrin map.
Specific embodiment
1 microscopical characters of embodiment
Capsule 's content is taken, No. 5 sieves are crossed after grinding, appropriate powder is selected to set on coverslip, chloraldurate test solution is added dropwise, closes the lid
Slide, it is in bending, and minority has bifurcated, diameter is about 3 to 7 micro- that microscopically observation: elongated light brown mycelia, which is scattered distribution,
Rice, the microscopic features are more apparent, and (see figure 1) complies with standard.
2 thin layer of embodiment identifies
Capsule 's content is taken, powder 12g is taken after grinding, add diethyl ether 60ml, shakes 1 hour, and filtration discards filtrate, dregs of a decoction methanol
60ml is heated to reflux 1 hour, filtration, and for filtrate recycling design to doing, residue adds water 30ml to make the n-butanol for dissolving, being saturated with water
4 times (20ml, 20ml, 15ml, 15ml) is extracted in shaking, merges n-butanol liquid, after being washed with ammonia solution, n-butanol liquid recycling design
To doing, residue adds water 20ml to make to dissolve, and lets cool, and by D101 type large pore resin absorption column, (column internal diameter 1.5cm, pillar height are
15cm), it is eluted with water 40ml, discards eluent, then with 40% ethyl alcohol 50ml elution, discard eluent, after with 70% ethyl alcohol 50ml
Eluent is collected in elution, and recycling design is to doing, and residue adds methanol 1ml to make to dissolve, as test solution.Separately take Milkvetch Root
3g is made in the same way of control medicinal material solution.Astragaloside IV reference substance is taken again, adds methanol that solution of every 1ml containing 1mg is made, as right
According to product solution.According to thin-layered chromatography, above-mentioned three kinds of solution 5-10 μ l is drawn, is put respectively on same silica gel g thin-layer plate, with dichloro
Lower layer's solution of methane-methanol-water (12:8:3) is solvent, is unfolded, and takes out, dries, spray with 10% ethanol solution of sulfuric acid,
105 DEG C to be heated to spot development clear.
The thin layer identifies sample chromatogram and reference substance chromatography on a corresponding position, and identical brown color spot is shown under daylight
Point；Identical orange-yellow fluorescence spot is shown at ultraviolet lamp (365nm), through three batches of sample detections, is complied with standard.(see figure
2,3)
The quantitative determination of 3 functional component of embodiment
1, instrument and reagent:
Agilent Agilent1200 high performance liquid chromatograph.
Supersonic wave cleaning machine (power 200w, frequency 40KHz)
Electronic balance XS105 type
Acetonitrile is chromatographically pure, and water is ultrapure water, remaining reagent is that analysis is pure.
Schizandrin reference substance lot number is 110857-201211,110857-201714, is purchased from Chinese food drug
Research institute is examined and determine, for assay.
2, liquid phase chromatogram condition and system suitability:
Month rising sun Welch Ultimate XB- C18 (4.6 × 250mm × 5 μm) chromatographic column.
Mobile phase: use gradient eluted [acetonitrile (A)-water (B) for mobile phase carry out gradient elution (0min:45%A →
25min:68%A → 40min:68%A → 60min:45%A)]
Flow velocity: 1.0mL/min
Detection wavelength: 250nm
Column temperature: 35 DEG C
Sampling volume: 10uL
Theoretical cam curve is calculated by schizandrin peak, is 5500.The separating degree of impurity peaks is 2.84 on schizandrin and side,
Greater than 1.5.
The preparation of 4 reference substance solutions: it is appropriate that precision weighs schizandrin reference substance, and methanol is added and is made containing Schisandra chinensis
The solution of alcohol first 0.15mg/mL, as reference substance solution.
The preparation of 5 test solutions:
This product content about 4g is taken, it is accurately weighed, 5g diatomite is added, is uniformly mixed in postposition Soxhlet extractor, adds methanol
50mL is heated to reflux 4 hours, and extracting solution recycling design is simultaneously concentrated to dryness, and residue adds methanol to dissolve, and is transferred in 25ml measuring bottle,
Add methanol to scale, shakes up, with the organic membrane filtration of 0.45um, take subsequent filtrate to get sample solution.
6 blank tests:
The preparation of 6.1 negative sample solution:
The negative sample for taking scarce schizandrin, the negative sample solution prepared by the preparation method of test solution.
6.2 blank tests:
Schizandrin reference substance solution, Chinese medicinal capsule test solution and negative sample solution is taken to be injected separately into high-efficient liquid phase color
Spectrometer measurement, experimental result: lack schisandra chinensis medicinal material negative sample solution at retention time corresponding with reference substance solution without
Peak occurs, other ingredientss do not interfere the measurement of schizandrin in the side of showing.
The investigation of 7 linear relationships:
Precision weighs schizandrin reference substance 12.79mg, is placed in 25mL measuring bottle, adds methanol to dissolve and is diluted to scale, shakes
It is even；Again it is accurate measure reference substance solution 1,2,3,4,5mL set in 10mL measuring bottle respectively, add methanol dilution to scale, shake up to get
Concentration be 0.05116mg/mL, 0.10232mg/mL, 0.15348mg/mL, 0.20464mg/mL, 0.25580mg/mL,
The schizandrin reference substance of 0.5116mg/mL draws reference substance solution 10uL and injects high performance liquid chromatograph, measures peak in accordance with the law
Area is drawn standard curve, as a result be see the table below.
The result shows that schizandrin is in good linear relationship within the scope of 0. 51~5.12ug, regression equation is
Linear equation is -209.1(r=0.9991 y=22579x)
8 stability experiments
Test solution (00DJD01) is taken, respectively after preparation after 0 hour, 4 hours, 10 hours, 17 hours, 24 hours, by upper
Chromatographic condition measurement content is stated, as a result see the table below.
The result shows that the RSD < 2.0% of schizandrin peak area in 0~24 hour, illustrates test solution 24
Stablize in hour.
9 Precision Experiments
Text method is pressed, takes same sample (00DJD01) solution under above-mentioned chromatographic condition, is repeated sample introduction 6 times, opposite mark is acquired
Quasi- deviation RSD < 2.0%, as a result see the table below.
The experimental results showed that instrument precision is good.
10 repeated experiments
Text method is pressed, 6 parts are taken to sample (00DJD01), 6 parallel extractions is carried out and measures, as a result see the table below.
The result shows that the equal < 2.0% of schizandrin relative standard deviation RSD, illustrates that this law has good reproducibility.
The experiment of 11 rate of recovery
Precision weighs same crowd of sample (00DJD01) 2.00g of known content, and totally 9 parts (calculate sample according to finished product measurement result
Schizandrin content is 1.54mg/g), every part of sample is separately added into a certain amount of schizandrin reference substance, by text method
Its content is measured, the rate of recovery is calculated, as a result see the table below.
As a result: the average recovery rate of sample is 100.2%, and relative standard deviation value is respectively less than 2.0%, the results showed that this law tool
There is the good rate of recovery, method is feasible.
The investigation of 12 ranges
The method for pressing text, taking each two parts of sample (00DJD01) 2.0g, 4.0g, 6.0g, (low concentration is the 50% of limit, high concentration
It is the 150% of limit), it is tested by the preparation method of test solution, as a result see the table below.
The result shows that schizandrin relative standard deviation RSD less than 2.0%, illustrates that this law has good reproducibility.
13 durabilities
Moon rising sun Welch Ultimate XB- C18 (4.6 × 250mm × 5 μm), water generation Waters RP18 were tried in an experiment
(4.6 × 250mm × 5 μm), C18(4.6 × 250mm × 5 μm YMC-Triart).The result shows that the separation of three root chromatogram columns is imitated
Fruit is good.The result shows that the experimental method reproducibility is good.
The measurement of 14 sample sizes
The assay that text method carries out schizandrin is pressed to three batches of samples respectively, every batch of takes two parts (see Fig. 4,5) in parallel,
As a result it see the table below.
By States Pharmacopoeia specifications, (the C containing schizandrin in schisandra chinensis medicinal material24H32O7) 0.40% must not be less than.According in formula five
The accounting of taste provides that every g capsule 's content in terms of Astragaloside IV, must not be less than 0. 5mg containing Schisandra chinensis.
Claims (10)
1. the method for quality control that a kind of pair of hepatic injury has defencive function Chinese medicinal capsule, which is characterized in that using microscopical characters, thin
Layer identifies and functional component quantitative determination.
2. a kind of pair of hepatic injury as described in claim 1 has defencive function Chinese medicinal capsule, it is characterised in that by pueraria lobata, trifoliate orange Dulcis
The Six-elements such as son, Radix Astragali, ganoderma lucidum, Schisandra chinensis, galangal medicinal material is prepared through modern production process processing.
3. quality control method as described in claim 1, it is characterised in that microscopical characters method are as follows: take capsule contents
Object crosses No. 5 sieves, appropriate powder is selected to set on coverslip after grinding, dropwise addition chloraldurate test solution, covered, under microscope
Observation: elongated light brown mycelia is scattered distribution, and in bending, and minority has bifurcated, and diameter is about 3 to 7 microns.
4. quality control method as described in claim 1, it is characterised in that thin-layer identification method are as follows: take capsule contents
Object takes powder 12g after grinding, add diethyl ether 60ml, shakes 1 hour, and filtration discards filtrate, and dregs of a decoction methanol 60ml is heated to reflux 1
Hour, filtration, for filtrate recycling design to doing, residue adds water 30ml to make to dissolve, and the n-butanol shaking being saturated with water is extracted 4 times
(20ml, 20ml, 15ml, 15ml) merges n-butanol liquid, and after being washed with ammonia solution, to doing, residue adds n-butanol liquid recycling design
Water 20ml makes to dissolve, and lets cool, by D101 type large pore resin absorption column (column internal diameter 1.5cm, pillar height 15cm), with water 40ml
Elution discards eluent, then is eluted with 40% ethyl alcohol 50ml, discards eluent, elutes after with 70% ethyl alcohol 50ml, collects elution
Liquid, recycling design is to doing, and residue adds methanol 1ml to make to dissolve, as test solution.
5. separately taking Milkvetch Root 3g, it is made in the same way of control medicinal material solution.
6. taking Astragaloside IV reference substance again, add methanol that solution of every 1ml containing 1mg is made, as reference substance solution.
7. shining thin-layered chromatography, above-mentioned three kinds of solution 5-10 μ l is drawn, is put respectively on same silica gel g thin-layer plate, with dichloromethane
Lower layer's solution of alkane-methanol-water (12:8:3) is solvent, is unfolded, and takes out, dries, and is sprayed with 10% ethanol solution of sulfuric acid, 105
It is clear DEG C to be heated to spot development.
8. sample chromatogram should show identical sepia spot with reference substance chromatography on a corresponding position under daylight；Ultraviolet light
Identical orange-yellow fluorescence spot is shown under lamp (365nm)；
Quality control method as described in claim 1, which is characterized in that functional component method for quantitatively determining is using high
Effect liquid phase chromatogram method measures functional component schizandrin.
9. quality control method as claimed in claim 5, it is characterised in that the preparation method of test solution: take this product
Content about 4g, accurately weighed, addition 5g diatomite is uniformly mixed in postposition Soxhlet extractor, adds methanol 50mL, be heated to reflux
4 hours, extracting solution recycling design was simultaneously concentrated to dryness, and residue adds methanol to dissolve, and is transferred in 25ml measuring bottle, added methanol to scale,
It shakes up, with the organic membrane filtration of 0.45um, takes subsequent filtrate to get sample solution.
10. quality control method as claimed in claim 5, which is characterized in that measuring method is accurate absorption pair respectively
According to product solution and each 10uL of test solution, liquid chromatograph is injected, is measured to get chromatographic condition are as follows: with octadecylsilane
Bonded silica gel is filler；Using gradient to be eluted, [acetonitrile (A)-water (B) carries out gradient elution (0min:45%A for mobile phase
→ 25min:68%A → 40min:68%A → 60min:45%A)], Detection wavelength 250nm；Theoretical cam curve presses schizandrin
Peak is calculated, and should be not less than 3000；Every g capsule 's content contains Schisandra chinensis in terms of schizandrin, no less than 0.5mg.
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