CN110187045A - Compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment - Google Patents
Compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment Download PDFInfo
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- CN110187045A CN110187045A CN201910507014.5A CN201910507014A CN110187045A CN 110187045 A CN110187045 A CN 110187045A CN 201910507014 A CN201910507014 A CN 201910507014A CN 110187045 A CN110187045 A CN 110187045A
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- blood stasis
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- 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
Abstract
The present invention relates to effective ingredient technical fields, and in particular to is compound components of panax notoginseng thin-layer identification method in a kind of Moschus blood-circulation and removing blood stasis ointment, including atropine sulfate thin layer identifies measuring method and bagodryl hydrochloride thin layer identifies measuring method.Pass through the characteristic for each drug ingedient in Moschus blood-circulation and removing blood stasis ointment, the thin layer based on compound components of panax notoginseng identifies feature again, adaptable extraction and preparation technique and required preparation are provided, so as to the separation and Extraction ingredient completion thin layer identification measurement to be determined from many active drug ingredients of Moschus blood-circulation and removing blood stasis ointment, it solves during Moschus blood-circulation and removing blood stasis ointment is, Western medicine combination emplastrum, sample coating carries out at high temperature, all active principles are in colloid, it is more difficult when carrying out effective ingredient analysis to identify that measuring method therefrom individually extracts compound components of panax notoginseng by existing thin layer, lead to not the problem of obtaining accurate result.
Description
Technical field
The present invention relates to effective ingredient technical fields, and in particular to is compound components of panax notoginseng in Moschus blood-circulation and removing blood stasis ointment
Thin-layer identification method.
Background technique
Moschus blood-circulation and removing blood stasis ointment be a kind of common Chinese patent drug, wherein containing Moschus, Radix Notoginseng, safflower, Radix Salviae Miltiorrhizae, boric acid, camphor,
Dragon's blood, urea, belladonna liquid extract, bagodryl hydrochloride, procaine hydrochloride composition.With activating microcirculation and removing stasis medicinal, the function of anti-inflammatory analgetic
Effect.For joint sprain, soft tissue bruise, acute lumbar muscle sprain lumbar muscle strain, scapulohumeral periarthritis, pernio of not bursting, nodositas is red.
Due to Moschus blood-circulation and removing blood stasis ointment be in, Western medicine combination emplastrum, sample coating carry out at high temperature, it is all effectively
Substance is more difficult when carrying out effective ingredient analysis to identify that measuring method is therefrom individually extracted by existing thin layer in colloid
Compound components of panax notoginseng out leads to not obtain accurate result.
Summary of the invention
The present invention for Moschus blood-circulation and removing blood stasis ointment be in, Western medicine combination emplastrum, sample be coated with carry out at high temperature, institute
There is active principle in colloid, it is more difficult when carrying out effective ingredient analysis to identify that measuring method is therefrom single by existing thin layer
Compound components of panax notoginseng solely is extracted, leads to not the problem of obtaining accurate result, a kind of Moschus blood-circulation and removing blood stasis ointment is provided
Middle compound components of panax notoginseng thin-layer identification method.
The present invention solves above-mentioned technical problem, the technical solution adopted is that, Radix Notoginseng is effective in a kind of Moschus blood-circulation and removing blood stasis ointment
Ingredient thin-layer identification method, including the preparation of control group reagent, the preparation of measurement group reagent and thin layer identify measurement, compare group reagent system
It is standby the following steps are included:
S1 takes Radix Notoginseng control medicinal material, and reagent is extracted in addition, and dipping solution is made in dipping；
S2 takes dipping solution made from S1, filtering, and filtrate is control group reagent；
Measure group reagent preparation the following steps are included:
S1 takes Moschus blood-circulation and removing blood stasis ointment, adds solubilising reagent, ointment is washed down, and solubilising reagent is made；
S2 takes solubilising reagent made from S1, and slowly reagent is precipitated in addition, until Precipitation, is made mix reagent；
S3 takes mix reagent made from S2 to filter, and filtrate is evaporated, and a residue is made；
S4 takes a residue made from S3 to add water, and stirring is cooled to room temperature, and is filtered, and filtrate is evaporated, and secondary residual is made；
S5 takes secondary residual made from S4, adds solubilising reagent, and measurement group reagent is made；
Thin layer identify measurement the following steps are included:
S1 takes control group reagent and measurement group reagent, is put respectively on same silica gel g thin-layer plate, and by solvent into
Row expansion；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with developing agents, and heat；
S3 after being heated to preference temperature, is inspected under fluorescent light, in control group reagent chromatography and measurement group reagent color
It composes on corresponding position, obtains the fluorescence spot for showing identical color.
Further, it compares in group reagent preparation step, it is ethyl alcohol, additive amount 5mL, Radix Notoginseng control that reagent is extracted in S1
Medicinal material is 0.25g.
Optionally, it compares in group reagent preparation step, dip time is for 24 hours in S2.
Optionally, it measures in group reagent preparation step, solubilising reagent is chloroform, additive amount 20mL, Moschus promoting blood circulation in S1
HUAYU ointment additive amount is 4.
Optionally, it measures in group reagent preparation step, it is ethyl alcohol that reagent is precipitated in S2.
Optionally, it measures in group reagent preparation step, adds 15mL in S4 in a residue, temperature is 40 DEG C~60 DEG C
Hot water.
Optionally, it measures in group reagent preparation step, solubilising reagent is ethyl alcohol, additive amount 2mL in S5.
Optionally, thin layer identifies in measurement preparation step, and control group reagent and measurement each 15 μ L of group reagent, expansion are taken in S1
Agent is the mixed solvent of the n-butanol, ethyl acetate and the water that are 4:1:5 according to volume ratio.
Optionally, thin layer identifies in measurement preparation step, and developing agents are 10% phosphomolybdic acid ethanol solution in S2.
Optionally, thin layer identifies in measurement preparation step, and 105 DEG C are heated in S3 and dries 5min.
Beneficial effects of the present invention include at least following one；
1, the thin layer mirror by the characteristic for each drug ingedient in Moschus blood-circulation and removing blood stasis ointment, then based on compound components of panax notoginseng
Determine feature, adaptable extraction and preparation technique and required preparation are provided, so as to have from many of Moschus blood-circulation and removing blood stasis ointment
It imitates separation and Extraction ingredient to be determined in drug ingedient and completes thin layer identification measurement.
2, solve Moschus blood-circulation and removing blood stasis ointment be in, Western medicine combination emplastrum, sample coating carry out at high temperature, own
Active principle is more difficult when carrying out effective ingredient analysis to identify that measuring method is therefrom independent by existing thin layer in colloid
Compound components of panax notoginseng is extracted, the problem of obtaining accurate result is led to not.
Detailed description of the invention
Fig. 1 is that measurement chart is unfolded in compound components of panax notoginseng specificity；
Fig. 2 is that measurement chart is unfolded in silica G plate under compound components of panax notoginseng durability fluorescent lamp；
Specific embodiment
It is clear in order to enable the objectives, technical solutions, and advantages of the present invention to be more clear, with reference to embodiments to this
Invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting present invention protection content.
Embodiment 1
Compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment, including the preparation of control group reagent, measurement
Group reagent preparation and thin layer identify measurement, control group reagent preparation the following steps are included:
S1 takes Radix Notoginseng control medicinal material, and reagent is extracted in addition, and dipping solution is made in dipping；
S2 takes dipping solution made from S1, filtering, and filtrate is control group reagent；
Measure group reagent preparation the following steps are included:
S1 takes Moschus blood-circulation and removing blood stasis ointment, adds solubilising reagent, ointment is washed down, and solubilising reagent is made；
S2 takes solubilising reagent made from S1, and slowly reagent is precipitated in addition, until Precipitation, is made mix reagent；
S3 takes mix reagent made from S2 to filter, and filtrate is evaporated, and a residue is made；
S4 takes a residue made from S3 to add water, and stirring is cooled to room temperature, and is filtered, and filtrate is evaporated, and secondary residual is made；
S5 takes secondary residual made from S4, adds solubilising reagent, and measurement group reagent is made；
Thin layer identify measurement the following steps are included:
S1 takes control group reagent and measurement group reagent, is put respectively on same silica gel g thin-layer plate, and by solvent into
Row expansion；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with developing agents, and heat；
S3 after being heated to preference temperature, is inspected under fluorescent light, in control group reagent chromatography and measurement group reagent color
It composes on corresponding position, obtains the fluorescence spot for showing identical color.
Thin layer identification by the characteristic for each drug ingedient in Moschus blood-circulation and removing blood stasis ointment, then based on compound components of panax notoginseng
Feature provides adaptable extraction and preparation technique and required preparation, so as to from Moschus blood-circulation and removing blood stasis ointment it is many effectively
Separation and Extraction ingredient to be determined completes thin layer identification measurement in drug ingedient.Solve Moschus blood-circulation and removing blood stasis ointment be in, Western medicine knot
Emplastrum is closed, sample coating carries out at high temperature, and all active principles are carrying out effective ingredient analysis in colloid
When it is more difficult identify that measuring method therefrom individually extracts compound components of panax notoginseng by existing thin layer, lead to not to obtain accurately
As a result the problem of.
Embodiment 2
Compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment, including the preparation of control group reagent, measurement
Group reagent preparation and thin layer identify measurement, control group reagent preparation the following steps are included:
S1 takes Radix Notoginseng control medicinal material 0.25g, adds 5mL ethyl alcohol, and for 24 hours, dipping solution is made in dipping；
S2 takes dipping solution made from S1, filtering, and filtrate is control group reagent；
Measure group reagent preparation the following steps are included:
S1 takes Moschus blood-circulation and removing blood stasis ointment 4, adds 20mL chloroform, ointment is washed down, and solubilising reagent is made；
S2 takes solubilising reagent made from S1, and slowly adds ethyl alcohol, until Precipitation, is made mix reagent；
S3 takes mix reagent made from S2 to filter, and filtrate is evaporated, and a residue is made；
S4, taking a residue heating degree made from S3 is the hot water that 15mL temperature is 40 DEG C~60 DEG C, and stirring is cooled to room
Temperature, filtering, filtrate are evaporated, and secondary residual is made；
S5 takes secondary residual made from S4, adds 2mL ethyl alcohol, and measurement group reagent is made；
Thin layer identify measurement the following steps are included:
S1 takes control group reagent and measurement 15 μ L of group reagent, is put respectively on same silica gel g thin-layer plate, and by for by
It is unfolded according to the mixed solvent of n-butanol, ethyl acetate and water that volume ratio is 4:1:5；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with 10% phosphomolybdic acid ethanol solution, and heat；
S3 is inspected under fluorescent light after being heated to 105 DEG C and drying 5min, in control group reagent chromatography and measurement
On the corresponding position of group reagent chromatography, the fluorescence spot for showing identical color is obtained.
Thin layer identification by the characteristic for each drug ingedient in Moschus blood-circulation and removing blood stasis ointment, then based on compound components of panax notoginseng
Feature provides adaptable extraction and preparation technique and required preparation, so as to from Moschus blood-circulation and removing blood stasis ointment it is many effectively
Separation and Extraction ingredient to be determined completes thin layer identification measurement in drug ingedient.Solve Moschus blood-circulation and removing blood stasis ointment be in, Western medicine knot
Emplastrum is closed, sample coating carries out at high temperature, and all active principles are carrying out effective ingredient analysis in colloid
When it is more difficult identify that measuring method therefrom individually extracts compound components of panax notoginseng by existing thin layer, lead to not to obtain accurately
As a result the problem of.
Embodiment 3
In order to ensure effect of the invention, identification side of the applicant to compound components of panax notoginseng and bagodryl hydrochloride in preparation
Method has carried out corresponding experimental study and demonstration, specific as follows:
Compound components of panax notoginseng thin layer identifies measuring method
(1) reagent and reagent
Moschus blood-circulation and removing blood stasis ointment is provided by Liansheng Pharmaceutical Co., Ltd., Guizhou；Compound components of panax notoginseng control medicinal material is by middle traditional Chinese medicines
Product biological products assay institute provides；Silica gel g thin-layer plate: the silica gel g thin-layer plate of subsidiary factory, Haiyang Chemical Plant, Qingdao production, reagent: chlorine
Imitative, ethyl alcohol, n-butanol and ethyl acetate are that analysis is pure.
(2) specificity
It takes Moschus blood-circulation and removing blood stasis ointment, measurement group reagent and control group reagent is made with 2 method of embodiment, take measurement group respectively
Reagent, control group reagent point sample, expansion, colour developing, are inspected under daylight, in measurement group reagent chromatography, and compare group reagent chromatography
Identical principal spot is shown on corresponding position, spot separation is preferable.
(3) durability
It takes that measurement group reagent is made by above-mentioned 3 batches of samples and compares group reagent and is put respectively in silica G prefabricated board, be unfolded,
After colour developing, as a result spot separator well, noiseless.
The following contents is obtained after measuring according to the technical solution provided in embodiment 2:
Carrier is silica G plate in Fig. 1, solvent be 4:1:5 according to volume ratio n-butanol, ethyl acetate and water it is mixed
Bonding solvent develops the color for 10% phosphomolybdic acid ethanol solution, inspects under fluorescent lamp.
It is followed successively by 1,2,3,4 from left to right, wherein corresponding 151201 sample lots of label 1 measure group reagent, and 2 is corresponding
151202 sample lots measure group reagent, and 3 corresponding 151203 sample lots measure group reagent, 4 corresponding compound components of panax notoginseng controls
Group reagent, wherein 151201,151202,151203 be the test No. of different batches.
Carrier is silica G plate in Fig. 2, solvent be 4:1:5 according to volume ratio n-butanol, ethyl acetate and water it is mixed
Bonding solvent develops the color for 10% phosphomolybdic acid ethanol solution, inspects under fluorescent lamp.
It is followed successively by 1,2,3,4 from left to right, wherein the corresponding compound components of panax notoginseng of label 1 compares group reagent, and 2 correspond to 160801
Sample lots measure group reagent, and 3 corresponding 160901 sample lots measure group reagent, 4 corresponding 160902 sample lots measurement groups examinations
Agent, wherein 160801,160901,160902 be the test No. of different batches.
Claims (10)
1. compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment, it is characterised in that: prepared including control group reagent,
Measure group reagent preparation and thin layer identify measurement, the control group reagent prepare the following steps are included:
S1 takes Radix Notoginseng control medicinal material, and reagent is extracted in addition, and dipping solution is made in dipping；
S2 takes dipping solution made from S1, filtering, and filtrate is control group reagent；
Measurement group reagent preparation the following steps are included:
S1 takes Moschus blood-circulation and removing blood stasis ointment, adds solubilising reagent, ointment is washed down, and solubilising reagent is made；
S2 takes solubilising reagent made from S1, and slowly reagent is precipitated in addition, until Precipitation, is made mix reagent；
S3 takes mix reagent made from S2 to filter, and filtrate is evaporated, and a residue is made；
S4 takes a residue made from S3 to add water, and stirring is cooled to room temperature, and is filtered, and filtrate is evaporated, and secondary residual is made；
S5 takes secondary residual made from S4, adds solubilising reagent, and measurement group reagent is made；
The thin layer identify measurement the following steps are included:
S1 takes control group reagent and measurement group reagent, is put respectively on same silica gel g thin-layer plate, and opened up by solvent
It opens；
Silica gel g thin-layer plate after expansion is taken out, is dried by S2, and is sprayed with developing agents, and heat；
S3 after being heated to preference temperature, is inspected under fluorescent light, in control group reagent chromatography and measurement group reagent chromatography phase
On the position answered, the fluorescence spot for showing identical color is obtained.
2. compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment according to claim 1, it is characterised in that:
It compares in group reagent preparation step, it is ethyl alcohol that reagent is extracted in S1, and additive amount 5mL, Radix Notoginseng control medicinal material is 0.25g.
3. compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment according to claim 2, it is characterised in that:
It compares in group reagent preparation step, dip time is for 24 hours in S2.
4. compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment according to claim 3, it is characterised in that:
It measures in group reagent preparation step, solubilising reagent is chloroform in S1, and additive amount 20mL, Moschus blood-circulation and removing blood stasis ointment additive amount is 4
Piece.
5. compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment according to claim 4, it is characterised in that:
It measures in group reagent preparation step, it is ethyl alcohol that reagent is precipitated in S2.
6. compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment according to claim 5, it is characterised in that:
It measures in group reagent preparation step, adds 15mL, the hot water that temperature is 40 DEG C~60 DEG C in S4 in a residue.
7. compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment according to claim 6, it is characterised in that:
It measures in group reagent preparation step, solubilising reagent is ethyl alcohol, additive amount 2mL in S5.
8. compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment according to claim 7, it is characterised in that:
Thin layer identifies in measurement preparation step, and control group reagent and measurement each 15 μ L of group reagent are taken in S1, and solvent is according to volume ratio
For the mixed solvent of the n-butanol of 4:1:5, ethyl acetate and water.
9. compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment according to claim 8, it is characterised in that:
Thin layer identifies in measurement preparation step, and developing agents are 10% phosphomolybdic acid ethanol solution in S2.
10. compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment according to claim 9, feature exist
In: thin layer identifies in measurement preparation step, and 105 DEG C are heated in S3 and dries 5min.
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| CN201910507014.5A CN110187045A (en) | 2019-06-12 | 2019-06-12 | Compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910507014.5A CN110187045A (en) | 2019-06-12 | 2019-06-12 | Compound components of panax notoginseng thin-layer identification method in Moschus blood-circulation and removing blood stasis ointment |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102091297A (en) * | 2011-01-26 | 2011-06-15 | 湖南康尔佳药业有限公司 | Quality control method for liver health care medicine |
| CN102288708A (en) * | 2011-08-09 | 2011-12-21 | 南京中山制药有限公司 | Method for detecting quality of capsules used for promoting blood circulation and stopping pain |
-
2019
- 2019-06-12 CN CN201910507014.5A patent/CN110187045A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102091297A (en) * | 2011-01-26 | 2011-06-15 | 湖南康尔佳药业有限公司 | Quality control method for liver health care medicine |
| CN102288708A (en) * | 2011-08-09 | 2011-12-21 | 南京中山制药有限公司 | Method for detecting quality of capsules used for promoting blood circulation and stopping pain |
Non-Patent Citations (1)
| Title |
|---|
| 中华人民共和国卫生部药典委员会 编: "《中华人民共和国卫生部 药品标准 中药成方制剂 第八册》", 31 December 1993 * |
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Application publication date: 20190830 |