CN108226370A - A kind of discriminating of traditional Chinese medicine gel and content assaying method - Google Patents
A kind of discriminating of traditional Chinese medicine gel and content assaying method Download PDFInfo
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- CN108226370A CN108226370A CN201810178147.8A CN201810178147A CN108226370A CN 108226370 A CN108226370 A CN 108226370A CN 201810178147 A CN201810178147 A CN 201810178147A CN 108226370 A CN108226370 A CN 108226370A
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- borneol
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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
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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
- G01N30/02—Column chromatography
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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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The invention belongs to Chinese medicine quality standard fields, are related to discriminating and the content assaying method of a kind of traditional Chinese medicine gel, and in particular to camphor, the discriminating of borneol and menthol and assay in MUSK SHUHUOLING gelling agent.MUSK SHUHUOLING gelling agent is mainly made of camphor, borneol, menthol, safflower, Radix Notoginseng, muscone, dragon's blood and the extract of glutinous rehmannia and auxiliary material carbomer, triethanolamine.Discriminating provided by the invention and content assaying method, chaff interferent is few in test solution, active ingredient is complete, can increase the sensitivity of detector, protect chromatographic column, the advantage for having simple and feasible, accurate quick, stability good.
Description
Technical field
The invention belongs to Chinese medicine quality standard fields, are related to discriminating and the assay side of a kind of traditional Chinese medicine gel
Method, and in particular to compound Chinese medicinal preparation MUSK SHUHUOLING gelling agent method of quality control.
Background technology
MUSK SHUHUOLING gelling agent be compound preparation, mainly by camphor, borneol, menthol, safflower, Radix Notoginseng, muscone,
Dragon's blood and glutinous rehmannia composition, have the effect of invigorating circulation of blood to dissipate blood stasis and reducing swelling and relieving pain, for the new and old soft tissue injury of closed and muscular fatigue
Acid pains and arthralgia pain due to rheumatism.Compound Chinese patent medicine complicated component establishes more comprehensive Product Quality Evaluation method, improves quality mark
Standard is one of main method for ensureing product curative effect.Chinese patent drug content assaying method mainly has at present：1) quantitative chemical analysis,
Mainly there are analysis by titration and gravimetry, the inorganic constituents suitable for the assay either prescription of single preparation；
2) UV-VIS spectrophotometry mainly has dual-wavelength spectrophotometry, thin layer-spectrophotometry and column chromatography-spectrophotometric
Method is analyzed suitable for micro and trace components；3) gas chromatography, it is fast with high-effect, highly selective, highly sensitive and speed
Advantage, but due to being limited by sample vapor pressure, the sample containing volatile ingredient in Chinese patent drug can only be measured at present；4) thin layer
Scanning method, this method mean that the light with certain wavelength is radiated on lamellae, have to thin-layer chromatography and absorb ultraviolet light or visible ray
Spot or to that the spot for generating fluorescence can excite to be scanned through irradiation, will the obtained collection of illustrative plates of scanning and integration data for medicine
The discriminating of product analysis, determination of foreign matter and assay；5) high performance liquid chromatography, have efficiently, at a high speed, it is highly sensitive, applicable
Range is wide, the wide advantage of mobile phase range of choice, to analysis of amino acid, protein, alkaloid, nucleic acid, stays the volatilizations such as body, lipoid
Property is low, and thermal stability is poor, and the big high-molecular compound of molecular weight and ionic compound are particularly advantageous.In addition to this, also core
Magnetic resonance, mass spectrum and its joint technology, atomic absorption spectrum, X-ray diffraction method etc..
(camphor, menthol and the dragon in Lu Peng Capillary Gas Chromatography MUSK SHUHUOLING gelling agents such as Lu Peng
The 7th Analysis of Chinese Traditional Medicine seminar proceeding of China Association of Traditional Chinese Medicine of content [A] China Association of Traditional Chinese Medicine of brain
[C] China Association of Traditional Chinese Medicine, 2014:4.) camphor, peppermint in MUSK SHUHUOLING gelling agent are measured simultaneously using gas chromatography
The preparation method of the content of brain and borneol, wherein test solution is：MUSK SHUHUOLING gelling agent sample about 1g is taken, precision claims
It is fixed, put in conical flask with cover, add absolute ethyl alcohol 50mL, precision measures, and shaking makes to be completely dissolved, filter to get.Zeng Decheng was (once
Moral into Quality Standard of Shexiangshuhuoling Tincture research [J] Chinese patent drugs, 2000, (09):15-18.) to Radix Notoginseng in MUSK SHUHUOLING,
Dragon's blood, glutinous rehmannia, menthol, borneol, camphor have carried out indentification by TLC, with containing for high effective liquid chromatography for measuring camphor
Amount, wherein the indentification by TLC of menthol, borneol and camphor is directly by the use of sample itself as test sample, without any place
Reason；The preparation method of test sample when the high performance liquid chromatography of camphor measures is：Precision pipettes this product 2ml
It puts in 10ml measuring bottles, is diluted to scale with ethyl alcohol, shakes up.Not less than 1.0 × 105R/min centrifuges 10min, takes
Supernatant is as test solution.
Chinese medicine has the characteristics that multicomponent, weak effect, coordinates integration, and into complexity is grouped as, the interaction between ingredient is made
With then increasingly complex.Although the discriminating for active ingredient in Chinese patent drug and content detection have more research at present, when pair
Camphor, borneol, the discriminating of menthol and detection research are less in anti-MUSK SHUHUOLING gelling agent, and these researchs mostly collect
In in detection process the chromatographic conditions such as the mobile phase of liquid chromatogram, column temperature, elution flow rate, the dosage of solvent and concentration adjustment
Optimization, and it is less for other step researchs of detection, and the Study on pretreatment of especially preparation process, that is, sample of sample is less,
The prior art is molten or ultrasonic mostly using simple alcohol for MUSK SHUHUOLING gelling agent, but compound Chinese patent medicine complicated component,
Tens or even hundreds of kind of component are contained in a usual sample, and the content difference between each component is very big, other components can
The detection of target components can be caused greatly to interfere；Instrument failure, chromatographic column damage are resulted even in, chromatographic peak is broadened, divided
It does not open, more than miscellaneous peak etc..Therefore, the separation and Extraction of Chinese patent drug active ingredient is cumbersome, is always the difficult point of drug inspection.And conventional
The crude extract composition that test sample preparation method obtains is complicated, and often target substance content is low, and interference is big, the selection to analysis method
There is very high requirement；In addition to this, Chinese patent drug active ingredient discrimination process is commonly present in test sample chromatography and comparison medicine wood color
Spectrum is compared, the unconspicuous problem of spot, and menthol, camphor tree in MUSK SHUHUOLING gelling agent are examined using the thin layer method that standard is recorded
These volatile polar components of brain, borneol, it may occur that can not detect, phenomena such as spot is abnormal, trace it to its cause and mainly differentiate
Method in itself there are it is certain the problem of, especially pre-treating method is improper.
Invention content
The technical problems to be solved by the invention are to provide discriminating and the content of a kind of traditional Chinese medicine gel in view of the foregoing drawbacks
Assay method.This method test solution chaff interferent is few, can increase the sensitivity of detector, protects chromatographic column, simple and feasible, accurate
It is really quick, stability is good.
To achieve these goals, the present invention adopts the following technical scheme that：
A kind of discriminating of traditional Chinese medicine gel and content assaying method, which is characterized in that comprise the steps of：
(1) thin-layer identification method：
(a) prepared by test solution：MUSK SHUHUOLING gelling agent 3-5g is taken to add 70% ethyl alcohol 30-50mL, is sealed, dipping
20-30min, ultrasonic 3-5min；1-2h is heated to reflux, is cooled to room temperature, with chloroform shaking extraction 3 times, filtrate is evaporated, and residue adds
1mL absolute ethyl alcohols dissolve, shake up to get；
It is prepared by contrast solution：Take menthol reference substance and borneol reference substance add absolute ethyl alcohol be made every 1mL respectively containing 5mg and
The solution of 10mg；
Thin-layered chromatography is tested：Test solution and each 5 μ L of reference substance solution are drawn, is put respectively in same silica G thin layer
On plate, with benzene-ethyl acetate (18:2) it is solvent, expansion opens up away from 12-14cm, takes out, dry, spray with 2% vanillin-sulfuric acid
It is clear to be heated to spot development at 105 DEG C for solution；In test sample chromatography, on position corresponding with reference substance chromatography, show identical
The spot of color；
(b) prepared by test solution：MUSK SHUHUOLING gelling agent 3-5g is taken to add 70% ethyl alcohol 30-50mL, is sealed, dipping
20-30min, ultrasonic 3-5min；1-2h is heated to reflux, is cooled to room temperature, takes filtrate after crossing 0.22 μm of filter membrane, filtrate crosses solid phase extraction
Take column, eluted with chloroform, eluent is evaporated, residue add 1mL absolute ethyl alcohols dissolve, shake up to get；
It is prepared by contrast solution：Camphor reference substance is taken to add methanol that solution of every 1mL containing 10mg is made；
Thin-layered chromatography is tested：Test solution and each 10 μ L of reference substance solution are drawn, is put respectively in same silica G thin layer
On plate, with petroleum ether-ethyl acetate (10: 0.5) for solvent, expansion opens up away from 11-13cm, takes out, dry, smoked with iodine vapor
It is clear to spot development；In test sample chromatography, on position corresponding with reference substance chromatography, the spot of same color is shown；
(2) content of Headspace Gas Chromatography camphor, borneol, menthol：
Chromatographic condition：DB-WAX quartz capillary chromatographic columns；Carrier gas is high pure nitrogen, flow velocity 1.0-2.0mL/min；Hydrogen fire
Flame ionization detector；Temperature programming, 130-140 DEG C of initial temperature keep 5-8min, 180- are risen to 10-15 DEG C/min
190 DEG C of holding 4-6min；Split ratio 25-35:1；240-250 DEG C of injector temperature；Detector temperature：250-270℃.
It is prepared by test solution：
A. MUSK SHUHUOLING gelling agent 3-5g is taken to add methanol 30mL, is sealed, impregnates 20-30min；
B. flow back 1-2h, is cooled to room temperature, and filtrate is taken after crossing 0.22 μm of filter membrane；
C. solid-phase extraction column is taken, is activated with water, filtrate crosses column in B, is eluted with chloroform, and eluent is evaporated, and residue adds methanol
Be settled to 10mL, shake up to get；
The preparation of reference substance solution：Take borneol, Camphorae and menthue reference substance appropriate, it is accurately weighed, methanol is added to be made molten
Liquid；
The preparation of negative control sample solution：Remove remaining medicinal material outside borneol, remaining in addition to camphor respectively by prescription
Medicinal material and remaining medicinal material in addition to menthol are made without borneol negative control sample, without camphor negative control sample solution
With without menthol negative control sample, according to the preparation method of test solution be made scarce borneol negative control sample solution,
Lack camphor negative control sample solution and scarce menthol negative control sample solution；
It measures：It is accurate respectively to measure above-mentioned test solution, reference substance solution, lack borneol negative control sample solution, lack
Camphor negative control sample solution and scarce each 1mL of menthol negative control sample solution are injected in 10mL ml headspace bottles, and capping is close
Envelope, puts in 90 DEG C of insulating boxs and balances 30min, takes upper strata saturated gas 1mL, injects gas chromatograph, is detected.
Further, the traditional Chinese medicine gel is MUSK SHUHUOLING gelling agent.
Further, the MUSK SHUHUOLING gelling agent by camphor, borneol, menthol, safflower, Radix Notoginseng, muscone,
Dragon's blood and the extract of glutinous rehmannia are made with auxiliary material carbomer, triethanolamine.
Compound Chinese patent medicine complicated component, contains tens or even hundreds of kind of component in a usual sample, and each group point it
Between content difference it is very big, other components cause great interference to the detection of target components.Therefore, Chinese patent drug active ingredient
Separation and Extraction it is extremely important, be related to the reliability of measurement result and the service life of instrument.The present invention is for tested
The physicochemical property of quantity of material, long-term in-depth study are obtained for borneol in MUSK SHUHUOLING gelling agent, Camphorae and menthue
Differentiate and the preparation method of the test solution of assay, this method is simple, quick, efficiently, collection extraction, purification, concentration and
Pre-separation is integrated, and will not reduce the pollution of chromatographic column.
Further, in thin-layer identification method (a) prepared by test solution：MUSK SHUHUOLING gelling agent 3g is taken to add 70% ethyl alcohol
30mL, sealing impregnate 30min, ultrasonic 4min；1.5h is heated to reflux, is cooled to room temperature, with chloroform shaking extraction 3 times, filtrate is steamed
Dry, residue adds 1mL absolute ethyl alcohols to dissolve, shake up to get.
Further, chloroform used in chloroform shaking extraction 3 times is respectively 30mL, 20mL and 20mL.
Further, in (b) prepared by test solution in thin-layer identification method：MUSK SHUHUOLING gelling agent 5g is taken to add 70% second
Alcohol 50mL, sealing impregnate 25min, ultrasonic 5min；1h is heated to reflux, is cooled to room temperature, filtrate is taken after crossing 0.22 μm of filter membrane, is filtered
Liquid crosses solid-phase extraction column, is eluted with chloroform, and eluent is evaporated, residue add 1mL absolute ethyl alcohols dissolve, shake up to get.
Further, the solid-phase extraction column is activated using preceding using 8mL methanol, then 10mL washings is added to go first in column
Alcohol crosses the flow control of solid-phase extraction column in 2-3s/ drops.
The perfect condition of chromatographic condition is to obtain higher separating degree in a relatively short period of time, and with appropriate column
Capacity.Select to consider during chromatographic column analyte physicochemical property, by the clastotype of use and separated object with it is solid
Determine the interaction of phase surface.
Further, the content of the Headspace Gas Chromatography camphor, borneol, menthol, chromatographic condition：DB-WAX stones
English capillary chromatographic column；Carrier gas is high pure nitrogen, flow velocity 1.5mL/min；Flame ionization ditector；Temperature programming, starting
130 DEG C of temperature keeps 6min, and 180 DEG C of holding 4min are risen to 12 DEG C/min；Split ratio 25:1；250 DEG C of injector temperature；
Detector temperature：260℃.
Further, it is prepared by the content of the Headspace Gas Chromatography camphor, borneol, menthol, test solution：A.
MUSK SHUHUOLING gelling agent 3g is taken to add methanol 30mL, is sealed, impregnates 20min；B. flow back 1h, is cooled to room temperature, and crosses 0.22 μm of filter
Filtrate is taken after film；C. solid-phase extraction column is taken, is activated with water, filtrate crosses column in B, is eluted with chloroform, and eluent is evaporated, and residue adds first
Alcohol is settled to 10mL, shake up to get.
Further, solid-phase extraction column used in the content of the Headspace Gas Chromatography camphor, borneol, menthol
For HLB columns.
Above-mentioned detecting step, chromatographic parameter, reagent type, reagent dosage, in particular for the preparation method of test sample solution, all
It is to be obtained by long-term complicated experiment, is that the synergistic effect of above-mentioned many factors supports the beneficial effect of the present invention jointly
Fruit.
The application is in view of the above-mentioned problems, provide discriminating and the content assaying method of a kind of traditional Chinese medicine gel, by improving confession
The preparation method of test sample solution so that chaff interferent is few in test solution, active ingredient is complete, can increase the sensitive of detector
Degree protects chromatographic column.With the good advantage of simple and feasible, accurate quick, stability.
Specific embodiment
The present invention is further elaborated with reference to embodiments.These embodiments be only for illustrative purposes,
And do not limit the scope of the invention and essence.Based on the embodiment of the present invention, those of ordinary skill in the art are not making wound
All other embodiments obtained under the premise of the property made labour, belong to protection scope of the present invention.
Main test instrument：Gas chromatograph (GC, Agilent Technologies 7890A, fid detector),
CPA225D electronic balances, DirectQ3System pure water meters, DS-7510DTH ultrasonic cleaners；
Reagent：Agents useful for same is that analysis is pure；
Sample：MUSK SHUHUOLING gelling agent provides (lot number by Sichuan Guangda Pharmaceutical Co., Ltd：20170916).
Negative control sample：Not mentholated negative control sample, not camphorated negative control sample and without ice
The negative control sample of piece is provided by Sichuan Guangda Pharmaceutical Co., Ltd.
Reference substance：Menthol (lot number：110728-200506), camphor (lot number 110747-201409), borneol (lot number：
110881-201107) it is purchased from Chinese food drug identification research institute；
Chromatographic column：DB-WAX quartz capillary chromatographic columns (30m × 0.320mm × 0.5 μm)；Solid-phase extraction column：HLB columns.
Embodiment 1
Thin-layer identification method：
(a) prepared by test solution：MUSK SHUHUOLING gelling agent 3g is taken to add 70% ethyl alcohol 30mL, is sealed, impregnates 30min,
Ultrasonic 4min；1.5h is heated to reflux, is cooled to room temperature, with chloroform shaking extraction 3 times, chloroform used in 3 times is respectively 30mL, 20mL
And 20mL, filtrate are evaporated, residue add 1mL absolute ethyl alcohols dissolve, shake up to get；
It is prepared by contrast solution：Take menthol reference substance and borneol reference substance add absolute ethyl alcohol be made every 1mL respectively containing 5mg and
The solution of 10mg；
Thin-layered chromatography is tested：Test solution and each 5 μ L of reference substance solution are drawn, is put respectively in same silica G thin layer
On plate, with benzene-ethyl acetate (18:2) it is solvent, expansion opens up away from 13cm, takes out, dry, spray molten with 2% vanillin-sulfuric acid
It is clear to be heated to spot development at 105 DEG C for liquid；In test sample chromatography, on position corresponding with reference substance chromatography, identical face is shown
The spot of color；
(b) prepared by test solution：Solid-phase extraction column is activated using preceding using 8mL methanol, then 10mL washings is added to go in column
Methanol；MUSK SHUHUOLING gelling agent 5g is taken to add 70% ethyl alcohol 50mL, is sealed, impregnates 25min, ultrasonic 5min；1h is heated to reflux, it is cold
But to room temperature, filtrate is taken after crossing 0.22 μm of filter membrane, filtrate crosses solid-phase extraction column, crosses the flow control of solid-phase extraction column in 3s/ drops,
Eluted with chloroform, eluent is evaporated, residue add 1mL absolute ethyl alcohols dissolve, shake up to get；
It is prepared by contrast solution：Camphor reference substance is taken to add methanol that solution of every 1mL containing 10mg is made；
Thin-layered chromatography is tested：Test solution and each 10 μ L of reference substance solution are drawn, is put respectively in same silica G thin layer
On plate, with petroleum ether-ethyl acetate (10: 0.5) for solvent, expansion opens up away from 12cm, takes out, dry, smoked with iodine vapor to spot
Point colour developing is clear；In test sample chromatography, on position corresponding with reference substance chromatography, the spot of same color is shown；
Clear spot significantly without hangover, boundless edge effect, can it is corresponding with reference substance on.
Embodiment 2
Thin-layer identification method：
(a) prepared by test solution：MUSK SHUHUOLING gelling agent 4g is taken to add 70% ethyl alcohol 50mL, is sealed, impregnates 30min,
Ultrasonic 3min；Be heated to reflux 1h, be cooled to room temperature, with chloroform shaking extraction 3 times, chloroform used in 3 times be respectively 30mL, 20mL and
20mL, filtrate are evaporated, residue add 1mL absolute ethyl alcohols dissolve, shake up to get；
It is prepared by contrast solution：Take menthol reference substance and borneol reference substance add absolute ethyl alcohol be made every 1mL respectively containing 5mg and
The solution of 10mg；
Thin-layered chromatography is tested：Test solution and each 5 μ L of reference substance solution are drawn, is put respectively in same silica G thin layer
On plate, with benzene-ethyl acetate (18:2) it is solvent, expansion opens up away from 14cm, takes out, dry, spray molten with 2% vanillin-sulfuric acid
It is clear to be heated to spot development at 105 DEG C for liquid；In test sample chromatography, on position corresponding with reference substance chromatography, identical face is shown
The spot of color；
(b) prepared by test solution：Solid-phase extraction column is activated using preceding using 8mL methanol, then 10mL washings is added to go in column
Methanol；MUSK SHUHUOLING gelling agent 5g is taken to add 70% ethyl alcohol 50mL, is sealed, impregnates 30min, ultrasonic 4min；It is heated to reflux 1.5h,
It is cooled to room temperature, filtrate is taken after crossing 0.22 μm of filter membrane, filtrate crosses solid-phase extraction column, crosses the flow control of solid-phase extraction column in 2s/
Drop, eluted with chloroform, eluent is evaporated, residue add 1mL absolute ethyl alcohols dissolve, shake up to get；
It is prepared by contrast solution：Camphor reference substance is taken to add methanol that solution of every 1mL containing 10mg is made；
Thin-layered chromatography is tested：Test solution and each 10 μ L of reference substance solution are drawn, is put respectively in same silica G thin layer
On plate, with petroleum ether-ethyl acetate (10: 0.5) for solvent, expansion opens up away from 13cm, takes out, dry, smoked with iodine vapor to spot
Point colour developing is clear；In test sample chromatography, on position corresponding with reference substance chromatography, the spot of same color is shown；
Clear spot significantly without hangover, boundless edge effect, can it is corresponding with reference substance on.
Comparative example 1
Thin-layer identification method：
(a) prepared by test solution：Take MUSK SHUHUOLING gelling agent 3g add 1mL absolute ethyl alcohols dissolve, shake up to get；
It is prepared by contrast solution：Take menthol reference substance and borneol reference substance add absolute ethyl alcohol be made every 1mL respectively containing 5mg and
The solution of 10mg；
Thin-layered chromatography is tested：Test solution and each 5 μ L of reference substance solution are drawn, is put respectively in same silica G thin layer
On plate, with benzene-ethyl acetate (18:2) it is solvent, expansion opens up away from 13cm, takes out, dry, spray molten with 2% vanillin-sulfuric acid
It is clear to be heated to spot development at 105 DEG C for liquid；In test sample chromatography, on position corresponding with reference substance chromatography, identical face is shown
The spot of color；
(b) prepared by test solution：Take MUSK SHUHUOLING gelling agent 5g add 1mL absolute ethyl alcohols dissolve, shake up to get；
It is prepared by contrast solution：Camphor reference substance is taken to add methanol that solution of every 1mL containing 10mg is made；
Thin-layered chromatography is tested：Test solution and each 10 μ L of reference substance solution are drawn, is put respectively in same silica G thin layer
On plate, with petroleum ether-ethyl acetate (10: 0.5) for solvent, expansion opens up away from 12cm, takes out, dry, smoked with iodine vapor to spot
Point colour developing is clear；In test sample chromatography, on position corresponding with reference substance chromatography, the spot of same color is shown；
Although spot can it is corresponding with reference substance on, spot obscures no hangover, but edge effect is more apparent.
Embodiment 3
Headspace Gas Chromatography camphor, borneol, menthol content：
1.1 chromatographic condition：DB-WAX quartz capillary chromatographic columns (30m × 0.320mm × 0.5 μm)；Carrier gas is High Purity Nitrogen
Gas, flow velocity 1.5mL/min；Flame ionization ditector；Temperature programming, 130 DEG C of initial temperature, keep 6min, with 12 DEG C/
Min rises to 180 DEG C of holding 4min；Split ratio 25:1；250 DEG C of injector temperature；Detector temperature：260℃.
It is prepared by 1.2 test solutions：
A. MUSK SHUHUOLING gelling agent 3g is taken to add methanol 30mL, is sealed, impregnates 20min；
B. flow back 1h, is cooled to room temperature, and filtrate is taken after crossing 0.22 μm of filter membrane；
C. solid-phase extraction column is taken, is activated with water, filtrate crosses column in B, is eluted with chloroform, and eluent is evaporated, and residue adds methanol
Be settled to 10mL, shake up to get.
The preparation of 1.3 reference substance solutions：Take borneol, Camphorae and menthue reference substance appropriate, it is accurately weighed, methanol is added to be made
Solution；
The preparation of 1.4 negative control sample solution：Remove remaining medicinal material outside borneol, its in addition to camphor respectively by prescription
Remaining medicinal material and remaining medicinal material in addition to menthol are made without borneol negative control sample, are molten without camphor negative control sample
Liquid and without menthol negative control sample, it is molten to be made scarce borneol negative control sample according to the preparation method of test solution
Liquid lacks camphor negative control sample solution and scarce menthol negative control sample solution；
1.5 it measures：Respectively it is accurate measure above-mentioned test solution, reference substance solution, lack borneol negative control sample solution,
Camphor negative control sample solution and scarce each 1mL of menthol negative control sample solution are lacked, is injected in 10mL ml headspace bottles, capping is close
Envelope, puts in 90 DEG C of insulating boxs and balances 30min, takes upper strata saturated gas 1mL, injects gas chromatograph, is detected.
The drafting of 2.1 standard curves
Take camphor, menthol, borneol reference substance appropriate respectively, it is accurately weighed, methanol is added to dissolve, be made camphor, menthol,
Borneol concentration is respectively 4.8296,1.0475, the reference substance solution A of 1.9071mg/ml；Precision pipette reference substance solution A5ml in
In 10ml measuring bottles, with methanol constant volume to scale, reference substance solution B is obtained；Precision pipettes reference substance solution B5ml in 10ml measuring bottles,
With methanol constant volume to scale, reference substance solution C is obtained；Precision pipettes reference substance solution C5ml in 10ml measuring bottles, uses methanol constant volume
To scale, reference substance solution D is obtained；Precision pipettes reference substance solution D5ml in 10ml measuring bottles, with methanol constant volume to scale, obtains pair
According to product solution E.Above-mentioned each 1mL of various concentration reference substance solution is taken, is injected in 10mL ml headspace bottles, is sealed, put 90 DEG C of constant temperature
30min is balanced in case, takes upper strata saturated gas 1mL, gas chromatograph is injected, is detected.Using each constituent concentration as abscissa,
Peak area is ordinate,
Standard curve is drawn, correlation is good in a certain range for each ingredient.Each components regression equation and the range of linearity are shown in
Table 1.
1 each ingredient standard working curve regression equation of table and linear relationship
2.2 precision test
Precision draws mixing reference substance 1mL, injects in 10mL ml headspace bottles, seals, put in 90 DEG C of insulating boxs and balance
30min takes upper strata saturated gas 1mL, injects gas chromatograph, and continuous sample introduction 6 times measures camphor, menthol, borneol peak face
Product, as a result the RSD values of peak area are respectively 0.52%, 0.61%, 0.63%, show that instrument precision is good.
2.3 repetitive test
It takes with a collection of 6 parts of MUSK SHUHUOLING gelling agent sample, by legal system available test sample solution below " 1.2 " item, precision is inhaled
Each test liquid 1mL is taken, is injected in 10mL ml headspace bottles, is sealed, put in 90 DEG C of insulating boxs and balance 30min, take upper strata saturated air
Body 1mL injects gas chromatograph, and the RSD for calculating the chromatographic peak peak area of camphor, menthol and borneol in sample is respectively
0.71%th, 0.68%, 0.61%.
2.4 stability test
Precision is drawn with a traditional Chinese medicine gel sample solution, after preparation 0h, 1h, 6h, 9h, 12h, measure for 24 hours
Peak area, as a result the RSD values of peak area are respectively 0.55%, 0.87%, 0.66%, show test solution interior stabilization for 24 hours.
2.5 recovery test
Precision weigh MUSK SHUHUOLING gelling agent sample 3.00251g, 3.01200g, 3.00010g, 3.01099g,
3.01152g, 3.08219g are respectively placed in conical flask with cover, add in mixed reference substance solution A5ml, precision measures, by 1.2
Prepared by the preparation method of middle test solution, carry out sample-adding recovery experiment, calculates the rate of recovery.The result shows that camphor, menthol and
Borneol average recovery rate is respectively 99.27%, 100.53% and 101.10%；RSD is respectively 0.47%, 0.70% and
0.56%.
2.6 sample size
The above-mentioned test solution of accurate measurement, reference substance solution, scarce borneol negative control sample solution, scarce camphor are cloudy respectively
Property control sample solution and scarce each 1mL of menthol negative control sample solution, inject in 10mL ml headspace bottles, seal, put 90
30min is balanced in DEG C insulating box, takes upper strata saturated gas 1mL, gas chromatograph is injected, is detected.
Sample parallel determination 3 times, is averaged.The chromatographic peak of reference substance and sample is good, and negative control is to measuring without dry
It disturbs.Camphor, menthol and borneol content are calculated by external standard method；MUSK SHUHUOLING gelling agent is carried by Sichuan Guangda Pharmaceutical Co., Ltd
For camphor, menthol and borneol content detection result are respectively 0.055mg/g, 0.015mg/g and 0.020mg/g.
Comparative example 2
Headspace Gas Chromatography camphor, borneol, menthol content：
Chromatographic condition：DB-WAX quartz capillary chromatographic columns (30m × 0.320mm × 0.5 μm)；Carrier gas is high pure nitrogen,
Flow velocity 1.5mL/min；Flame ionization ditector；Temperature programming, 130 DEG C of initial temperature keep 6min, on 12 DEG C/min
Rise to 180 DEG C of holding 4min；Split ratio 25:1；250 DEG C of injector temperature；Detector temperature：260℃.
It is prepared by test solution：
MUSK SHUHUOLING gelling agent 3g is taken to add methanol 30mL, is sealed, impregnates 20min, maceration extract is evaporated, and residue adds methanol to determine
Hold to 10mL, shake up to get.
The preparation of reference substance solution：Take borneol, Camphorae and menthue reference substance appropriate, it is accurately weighed, methanol is added to be made molten
Liquid；
The preparation of negative control sample solution：Remove remaining medicinal material outside borneol, remaining in addition to camphor respectively by prescription
Medicinal material and remaining medicinal material in addition to menthol are made without borneol negative control sample, without camphor negative control sample solution
With without menthol negative control sample, according to the preparation method of test solution be made scarce borneol negative control sample solution,
Lack camphor negative control sample solution and scarce menthol negative control sample solution；
It measures：It is accurate respectively to measure above-mentioned test solution, reference substance solution, lack borneol negative control sample solution, lack
Camphor negative control sample solution and scarce each 1mL of menthol negative control sample solution are injected in 10mL ml headspace bottles, and capping is close
Envelope, puts in 90 DEG C of insulating boxs and balances 30min, takes upper strata saturated gas 1mL, injects gas chromatograph, is detected.
Sample parallel determination 3 times, is averaged.The chromatographic peak of reference substance is good, and negative control is noiseless to measuring, still
The chromatographic peak of sample goes out ghost peak, and separating degree is low, and peak type has hangover.Method is unstable, can not draw a conclusion.
Comparative example 3
Headspace Gas Chromatography camphor, borneol, menthol content：
Chromatographic condition：DB-WAX quartz capillary chromatographic columns (30m × 0.320mm × 0.5 μm)；Carrier gas is high pure nitrogen,
Flow velocity 1.5mL/min；Flame ionization ditector；Temperature programming, 130 DEG C of initial temperature keep 6min, on 12 DEG C/min
Rise to 180 DEG C of holding 4min；Split ratio 25:1；250 DEG C of injector temperature；Detector temperature：260℃.
It is prepared by test solution：
MUSK SHUHUOLING gelling agent 3g is taken to add methanol 30mL, flow back 1h, is cooled to room temperature, and filter is taken after crossing 0.22 μm of filter membrane
Liquid；Filtrate is evaporated, and residue adds methanol constant volume to 10mL, shake up to get.
The preparation of reference substance solution：Take borneol, Camphorae and menthue reference substance appropriate, it is accurately weighed, methanol is added to be made molten
Liquid；
The preparation of negative control sample solution：Remove remaining medicinal material outside borneol, remaining in addition to camphor respectively by prescription
Medicinal material and remaining medicinal material in addition to menthol are made without borneol negative control sample, without camphor negative control sample solution
With without menthol negative control sample, according to the preparation method of test solution be made scarce borneol negative control sample solution,
Lack camphor negative control sample solution and scarce menthol negative control sample solution；
It measures：It is accurate respectively to measure above-mentioned test solution, reference substance solution, lack borneol negative control sample solution, lack
Camphor negative control sample solution and scarce each 1mL of menthol negative control sample solution are injected in 10mL ml headspace bottles, and capping is close
Envelope, puts in 90 DEG C of insulating boxs and balances 30min, takes upper strata saturated gas 1mL, injects gas chromatograph, is detected.
Sample parallel determination 3 times, is averaged.The chromatographic peak of reference substance is good, and negative control is to measuring noiseless, sample
Chromatographic peak separating degree is relatively low, and stability and precision are low.Camphor, menthol and borneol content are calculated by external standard method；Moschus relaxes work
Clever gelling agent is provided by Sichuan Guangda Pharmaceutical Co., Ltd, and camphor, menthol and borneol content detection result are respectively
0.049mg/g, 0.013mg/g and 0.016mg/g.
Comparative example 4
Headspace Gas Chromatography camphor, borneol, menthol content：
Chromatographic condition：DB-WAX quartz capillary chromatographic columns (30m × 0.320mm × 0.5 μm)；Carrier gas is high pure nitrogen,
Flow velocity 1.5mL/min；Flame ionization ditector；Temperature programming, 130 DEG C of initial temperature keep 6min, on 12 DEG C/min
Rise to 180 DEG C of holding 4min；Split ratio 25:1；250 DEG C of injector temperature；Detector temperature：260℃.
It is prepared by test solution：
MUSK SHUHUOLING gelling agent 3g is taken to add methanol 30mL, filtrate is taken after crossing 0.22 μm of filter membrane；Solid-phase extraction column is taken, uses water
Activation, filtrate crosses column, eluted with chloroform, and eluent is evaporated, and residue adds methanol constant volume to 10mL, shake up to get.
The preparation of reference substance solution：Take borneol, Camphorae and menthue reference substance appropriate, it is accurately weighed, methanol is added to be made molten
Liquid；
The preparation of negative control sample solution：Remove remaining medicinal material outside borneol, remaining in addition to camphor respectively by prescription
Medicinal material and remaining medicinal material in addition to menthol are made without borneol negative control sample, without camphor negative control sample solution
With without menthol negative control sample, according to the preparation method of test solution be made scarce borneol negative control sample solution,
Lack camphor negative control sample solution and scarce menthol negative control sample solution；
It measures：It is accurate respectively to measure above-mentioned test solution, reference substance solution, lack borneol negative control sample solution, lack
Camphor negative control sample solution and scarce each 1mL of menthol negative control sample solution are injected in 10mL ml headspace bottles, and capping is close
Envelope, puts in 90 DEG C of insulating boxs and balances 30min, takes upper strata saturated gas 1mL, injects gas chromatograph, is detected.
Sample parallel determination 3 times, is averaged.The chromatographic peak of reference substance and sample is good, and negative control is to measuring without dry
It disturbs.Camphor, menthol and borneol content are calculated by external standard method；MUSK SHUHUOLING gelling agent is carried by Sichuan Guangda Pharmaceutical Co., Ltd
For camphor, menthol and borneol content detection result are respectively 0.047mg/g, 0.013mg/g and 0.017mg/g.
Comparative example 5
Discriminating and content assaying method according to traditional Chinese medicine gel a kind of disclosed in Chinese patent CN104807896A, as a result
Show that each chromatographic peak is corresponded with reference substance and control medicinal material chromatographic peak in test sample chromatogram, but chromatographic peak miscellaneous peak is more,
Separating degree is low, and ingredient is miscellaneous to injure greatly pillar.Camphor, menthol and borneol content detection result be respectively 0.050mg/g,
0.013mg/g and 0.018mg/g.
Embodiment 4
Headspace Gas Chromatography camphor, borneol, menthol content：
Chromatographic condition：DB-WAX quartz capillary chromatographic columns (30m × 0.320mm × 0.5 μm)；Carrier gas is high pure nitrogen,
Flow velocity 2mL/min；Flame ionization ditector；Temperature programming, 140 DEG C of initial temperature keep 5min, are risen with 15 DEG C/min
To 190 DEG C of holding 6min；Split ratio 35:1；250 DEG C of injector temperature；Detector temperature：250℃.
It is prepared by test solution：
A. MUSK SHUHUOLING gelling agent 4g is taken to add methanol 30mL, is sealed, impregnates 25min；
B. flow back 1.5h, is cooled to room temperature, and filtrate is taken after crossing 0.22 μm of filter membrane；
C. solid-phase extraction column is taken, is activated with water, filtrate crosses column in B, is eluted with chloroform, and eluent is evaporated, and residue adds methanol
Be settled to 10mL, shake up to get.
The preparation of reference substance solution：Take borneol, Camphorae and menthue reference substance appropriate, it is accurately weighed, methanol is added to be made molten
Liquid；
The preparation of negative control sample solution：Remove remaining medicinal material outside borneol, remaining in addition to camphor respectively by prescription
Medicinal material and remaining medicinal material in addition to menthol are made without borneol negative control sample, without camphor negative control sample solution
With without menthol negative control sample, according to the preparation method of test solution be made scarce borneol negative control sample solution,
Lack camphor negative control sample solution and scarce menthol negative control sample solution；
It measures：It is accurate respectively to measure above-mentioned test solution, reference substance solution, lack borneol negative control sample solution, lack
Camphor negative control sample solution and scarce each 1mL of menthol negative control sample solution are injected in 10mL ml headspace bottles, and capping is close
Envelope, puts in 90 DEG C of insulating boxs and balances 30min, takes upper strata saturated gas 1mL, injects gas chromatograph, is detected.
Sample parallel determination 3 times, is averaged.The chromatographic peak of reference substance and sample is good, and negative control is to measuring without dry
It disturbs.Camphor, menthol and borneol content are calculated by external standard method；MUSK SHUHUOLING gelling agent is carried by Sichuan Guangda Pharmaceutical Co., Ltd
For camphor, menthol and borneol content detection result are respectively 0.054mg/g, 0.016mg/g and 0.020mg/g.
Embodiment 5
Headspace Gas Chromatography camphor, borneol, menthol content：
Chromatographic condition：DB-WAX quartz capillary chromatographic columns (30m × 0.320mm × 0.5 μm)；Carrier gas is high pure nitrogen,
Flow velocity 1mL/min；Flame ionization ditector；Temperature programming, 135 DEG C of initial temperature keep 5min, are risen with 10 DEG C/min
To 190 DEG C of holding 5min；Split ratio 30:1；240 DEG C of injector temperature；Detector temperature：270℃.
It is prepared by test solution：
A. MUSK SHUHUOLING gelling agent 5g is taken to add methanol 30mL, is sealed, impregnates 30min；
B. flow back 2h, is cooled to room temperature, and filtrate is taken after crossing 0.22 μm of filter membrane；
C. solid-phase extraction column is taken, is activated with water, filtrate crosses column in B, is eluted with chloroform, and eluent is evaporated, and residue adds methanol
Be settled to 10mL, shake up to get.
The preparation of reference substance solution：Take borneol, Camphorae and menthue reference substance appropriate, it is accurately weighed, methanol is added to be made molten
Liquid；
The preparation of negative control sample solution：Remove remaining medicinal material outside borneol, remaining in addition to camphor respectively by prescription
Medicinal material and remaining medicinal material in addition to menthol are made without borneol negative control sample, without camphor negative control sample solution
With without menthol negative control sample, according to the preparation method of test solution be made scarce borneol negative control sample solution,
Lack camphor negative control sample solution and scarce menthol negative control sample solution；
It measures：It is accurate respectively to measure above-mentioned test solution, reference substance solution, lack borneol negative control sample solution, lack
Camphor negative control sample solution and scarce each 1mL of menthol negative control sample solution are injected in 10mL ml headspace bottles, and capping is close
Envelope, puts in 90 DEG C of insulating boxs and balances 30min, takes upper strata saturated gas 1mL, injects gas chromatograph, is detected.
Sample parallel determination 3 times, is averaged.The chromatographic peak of reference substance and sample is good, and negative control is to measuring without dry
It disturbs.Camphor, menthol and borneol content are calculated by external standard method；MUSK SHUHUOLING gelling agent is carried by Sichuan Guangda Pharmaceutical Co., Ltd
For camphor, menthol and borneol content detection result are respectively 0.055mg/g, 0.016mg/g and 0.020mg/g.
Embodiment 6
Headspace Gas Chromatography camphor, borneol, menthol content：
Chromatographic condition：DB-WAX quartz capillary chromatographic columns (30m × 0.320mm × 0.5 μm)；Carrier gas is high pure nitrogen,
Flow velocity 1.5mL/min；Flame ionization ditector；Temperature programming, 130 DEG C of initial temperature keep 8min, on 15 DEG C/min
Rise to 185 DEG C of holding 5min；Split ratio 30:1；250 DEG C of injector temperature；Detector temperature：260℃.
It is prepared by test solution：
A. MUSK SHUHUOLING gelling agent 3g is taken to add methanol 30mL, is sealed, impregnates 30min；
B. flow back 1.5h, is cooled to room temperature, and filtrate is taken after crossing 0.22 μm of filter membrane；
C. solid-phase extraction column is taken, is activated with water, filtrate crosses column in B, is eluted with chloroform, and eluent is evaporated, and residue adds methanol
Be settled to 10mL, shake up to get.
The preparation of reference substance solution：Take borneol, Camphorae and menthue reference substance appropriate, it is accurately weighed, methanol is added to be made molten
Liquid；
The preparation of negative control sample solution：Remove remaining medicinal material outside borneol, remaining in addition to camphor respectively by prescription
Medicinal material and remaining medicinal material in addition to menthol are made without borneol negative control sample, without camphor negative control sample solution
With without menthol negative control sample, according to the preparation method of test solution be made scarce borneol negative control sample solution,
Lack camphor negative control sample solution and scarce menthol negative control sample solution；
It measures：It is accurate respectively to measure above-mentioned test solution, reference substance solution, lack borneol negative control sample solution, lack
Camphor negative control sample solution and scarce each 1mL of menthol negative control sample solution are injected in 10mL ml headspace bottles, and capping is close
Envelope, puts in 90 DEG C of insulating boxs and balances 30min, takes upper strata saturated gas 1mL, injects gas chromatograph, is detected.
Sample parallel determination 3 times, is averaged.The chromatographic peak of reference substance and sample is good, and negative control is to measuring without dry
It disturbs.Camphor, menthol and borneol content are calculated by external standard method；MUSK SHUHUOLING gelling agent is carried by Sichuan Guangda Pharmaceutical Co., Ltd
For camphor, menthol and borneol content detection result are respectively 0.054mg/g, 0.017mg/g and 0.019mg/g.
The detection method of the present invention, hence it is evident that better than comparative example, illustrate that the linking of detection method links is close, take
Detection method indispensable with reasonable, that this specific combination is formed, produces apparent synergistic function.
The foregoing is merely the preferred embodiment of the present invention, are not intended to limit the scope of the invention, every utilization
The equivalent structure or equivalent flow shift that description of the invention is made directly or indirectly is used in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (10)
1. discriminating and the content assaying method of a kind of traditional Chinese medicine gel, which is characterized in that comprise the steps of：
(1) thin-layer identification method：
(a) prepared by test solution：MUSK SHUHUOLING gelling agent 3-5g is taken to add 70% ethyl alcohol 30-50mL, is sealed, impregnates 20-
30min, ultrasonic 3-5min；1-2h is heated to reflux, is cooled to room temperature, with chloroform shaking extraction 3 times, filtrate is evaporated, and residue adds 1mL
Absolute ethyl alcohol dissolve, shake up to get；
It is prepared by contrast solution：Menthol reference substance and borneol reference substance is taken to add absolute ethyl alcohol that every 1mL is made respectively containing 5mg's and 10mg
Solution；
Thin-layered chromatography is tested：Test solution and each 5 μ L of reference substance solution are drawn, is put respectively on same silica gel g thin-layer plate,
With benzene-ethyl acetate (18:2) it is solvent, expansion opens up away from 12-14cm, takes out, dry, spray with 2% vanillin-sulfuric acid solution,
It is clear that spot development is heated at 105 DEG C；In test sample chromatography, on position corresponding with reference substance chromatography, same color is shown
Spot；
(b) prepared by test solution：MUSK SHUHUOLING gelling agent 3-5g is taken to add 70% ethyl alcohol 30-50mL, is sealed, impregnates 20-
30min, ultrasonic 3-5min；1-2h is heated to reflux, is cooled to room temperature, takes filtrate after crossing 0.22 μm of filter membrane, filtrate crosses Solid Phase Extraction
Column is eluted with chloroform, and eluent is evaporated, residue add 1mL absolute ethyl alcohols dissolve, shake up to get；
It is prepared by contrast solution：Camphor reference substance is taken to add methanol that solution of every 1mL containing 10mg is made；
Thin-layered chromatography is tested：Test solution and each 10 μ L of reference substance solution are drawn, is put respectively in same silica gel g thin-layer plate
On, with petroleum ether-ethyl acetate (10: 0.5) for solvent, expansion is opened up and is taken out away from 11-13cm, dries, smoked with iodine vapor to spot
Point colour developing is clear；In test sample chromatography, on position corresponding with reference substance chromatography, the spot of same color is shown；
(2) content of Headspace Gas Chromatography camphor, borneol, menthol：
Chromatographic condition：DB-WAX quartz capillary chromatographic columns；Carrier gas is high pure nitrogen, flow velocity 1.0-2.0mL/min；Hydrogen flame from
Sonization detector；Temperature programming, 130-140 DEG C of initial temperature keep 5-8min, 180-190 DEG C are risen to 10-15 DEG C/min
Keep 4-6min；Split ratio 25-35:1；240-250 DEG C of injector temperature；Detector temperature：250-270℃.
It is prepared by test solution：
A. MUSK SHUHUOLING gelling agent 3-5g is taken to add methanol 30mL, is sealed, impregnates 20-30min；
B. flow back 1-2h, is cooled to room temperature, and filtrate is taken after crossing 0.22 μm of filter membrane；
C. solid-phase extraction column is taken, is activated with water, filtrate crosses column in B, is eluted with chloroform, and eluent is evaporated, and residue adds methanol constant volume
To 10mL, shake up to get；
The preparation of reference substance solution：Take borneol, Camphorae and menthue reference substance appropriate, it is accurately weighed, add methanol that solution is made；
The preparation of negative control sample solution：Remove remaining medicinal material outside borneol, remaining medicinal material in addition to camphor respectively by prescription
With remaining medicinal material in addition to menthol, it is not made without borneol negative control sample, without camphor negative control sample solution and not
Negative control sample containing menthol is made scarce borneol negative control sample solution according to the preparation method of test solution, lacks camphor tree
Brain negative control sample solution and scarce menthol negative control sample solution；
It measures：It is accurate respectively to measure above-mentioned test solution, reference substance solution, lack borneol negative control sample solution, lack camphor
Negative control sample solution and scarce each 1mL of menthol negative control sample solution inject in 10mL ml headspace bottles, seal, put
30min is balanced in 90 DEG C of insulating boxs, takes upper strata saturated gas 1mL, gas chromatograph is injected, is detected.
2. discriminating and the content assaying method of a kind of traditional Chinese medicine gel according to claim 1, which is characterized in that described
Traditional Chinese medicine gel is MUSK SHUHUOLING gelling agent.
3. discriminating and the content assaying method of a kind of traditional Chinese medicine gel according to claim 2, which is characterized in that described
MUSK SHUHUOLING gelling agent by camphor, borneol, menthol, safflower, Radix Notoginseng, muscone, dragon's blood and the extract of glutinous rehmannia with it is auxiliary
Material carbomer, triethanolamine are made.
4. discriminating and the content assaying method of a kind of traditional Chinese medicine gel according to claim 1, which is characterized in that described
In thin-layer identification method (a) prepared by test solution：MUSK SHUHUOLING gelling agent 3g is taken to add 70% ethyl alcohol 30mL, is sealed, dipping
30min, ultrasonic 4min；Be heated to reflux 1.5h, be cooled to room temperature, with chloroform shaking extraction 3 times, filtrate is evaporated, residue add 1mL without
Water-ethanol dissolve, shake up to get.
5. discriminating and the content assaying method of a kind of traditional Chinese medicine gel according to claim 4, which is characterized in that described
Chloroform shaking extraction 3 times used in chloroform be respectively 30mL, 20mL and 20mL.
6. discriminating and the content assaying method of a kind of traditional Chinese medicine gel according to claim 1, which is characterized in that described
In (b) prepared by test solution in thin-layer identification method：MUSK SHUHUOLING gelling agent 5g is taken to add 70% ethyl alcohol 50mL, is sealed, leaching
Stain 25min, ultrasonic 5min；1h is heated to reflux, is cooled to room temperature, filtrate is taken after crossing 0.22 μm of filter membrane, filtrate crosses solid-phase extraction column,
Eluted with chloroform, eluent is evaporated, residue add 1mL absolute ethyl alcohols dissolve, shake up to get.
7. discriminating and the content assaying method of a kind of traditional Chinese medicine gel according to claim 6, which is characterized in that described
Solid-phase extraction column is activated using preceding using 8mL methanol, then 10mL washings is added to remove methanol in column, crosses the flow control of solid-phase extraction column
In 2-3s/ drops.
8. discriminating and the content assaying method of a kind of traditional Chinese medicine gel according to claim 1, which is characterized in that the top
Gas chromatography measures the content of camphor, borneol, menthol, chromatographic condition：DB-WAX quartz capillary chromatographic columns；Carrier gas is
High pure nitrogen, flow velocity 1.5mL/min；Flame ionization ditector；Temperature programming, 130 DEG C of initial temperature keep 6min, with
12 DEG C/min rises to 180 DEG C of holding 4min；Split ratio 25:1；250 DEG C of injector temperature；Detector temperature：260℃.
9. discriminating and the content assaying method of a kind of traditional Chinese medicine gel according to claim 1, which is characterized in that the top
Gas chromatography measures the content of camphor, borneol, menthol, prepared by test solution：A. MUSK SHUHUOLING gelling agent 3g is taken
Add methanol 30mL, seal, impregnate 20min；B. flow back 1h, is cooled to room temperature, and filtrate is taken after crossing 0.22 μm of filter membrane；C. solid phase is taken to extract
Column is taken, is activated with water, filtrate crosses column in B, is eluted with chloroform, and eluent is evaporated, and residue adds methanol constant volume to be shaken up, i.e., to 10mL
.
10. discriminating and the content assaying method of a kind of traditional Chinese medicine gel according to claim 9, which is characterized in that described
Solid-phase extraction column is HLB columns.
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| CN110658276A (en) * | 2019-10-09 | 2020-01-07 | 广州暨南生物医药研究开发基地有限公司 | Folium artemisiae argyi quality assessment method |
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