CN108226370B - A kind of identification of traditional Chinese medicine gel and content assaying method - Google Patents
A kind of identification of traditional Chinese medicine gel and content assaying method Download PDFInfo
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- CN108226370B CN108226370B CN201810178147.8A CN201810178147A CN108226370B CN 108226370 B CN108226370 B CN 108226370B CN 201810178147 A CN201810178147 A CN 201810178147A CN 108226370 B CN108226370 B CN 108226370B
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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 field, it is related to identification and the content assaying method of a kind of traditional Chinese medicine gel, and in particular to camphor, the identification 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.Identification provided by the invention and content assaying method, chaff interferent is few in test solution, effective component is complete, can increase the sensitivity of detector, protects chromatographic column, with the good advantage of simple and feasible, accurate quick, stability.
Description
Technical field
The invention belongs to Chinese medicine quality standard field, it is related to identification 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 technique
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, are used for the new and old soft tissue injury of closed and muscular fatigue
Ache and rheumatic arthralgia.Compound Chinese patent medicine complicated component establishes more comprehensive Product Quality Evaluation method, improves quality mark
Standard is one of the main method for guaranteeing 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 of single preparation either prescription；
2) UV-VIS spectrophotometry mainly has dual-wavelength spectrophotometry, thin layer-spectrophotometry and column chromatography-spectrophotometric
Method is suitable for the analysis of micro and trace components；3) gas chromatography has high-effect, highly selective, highly sensitive and speed fast
Advantage can only measure the sample in Chinese patent drug containing volatile component at present but due to being limited by sample vapor pressure；4) thin layer
Scanning method, this method is meant to be radiated on lamellae with the light of certain wavelength, is had to thin-layer chromatography and is absorbed ultraviolet light or visible light
Spot or can excite the spot of generation fluorescence to be scanned to through irradiating, obtained map will be scanned and integration data is used for medicine
The identification of product analysis, determination of foreign matter and assay；5) high performance liquid chromatography, have efficiently, it is high speed, highly sensitive, applicable
Range is wide, the wide advantage of mobile phase range of choice, to analysis of amino acid, protein, alkaloid, nucleic acid, the volatilization such as stay 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, there are also cores
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 agent such as Lu Peng
The 7th Analysis of Chinese Traditional Medicine seminar proceeding of China Association of Traditional Chinese Medicine, content [A] China Association of Traditional Chinese Medicine of brain
[C] China Association of Traditional Chinese Medicine, 2014:4.) use gas chromatography to measure camphor, peppermint in MUSK SHUHUOLING gelling agent simultaneously
The content of brain and borneol, wherein test solution the preparation method comprises the following steps: take MUSK SHUHUOLING gelling agent sample about 1g, precision claims
It is fixed, set in stuffed conical flask, add dehydrated alcohol 50mL, precision measures, and shaking makes to be completely dissolved, filtering to get.Zeng Decheng was (once
Moral at Quality Standard of Shexiangshuhuoling Tincture research [J] Chinese patent drug, 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 directly uses sample itself as test sample, without any place
Reason；Camphor high performance liquid chromatography measurement when test sample the preparation method comprises the following steps: precision pipettes this product 2ml
It sets in 10ml measuring bottle, is diluted to scale with ethyl alcohol, shakes up.It is being not less than 1.0 × 105R/min is centrifuged 10min, takes
Supernatant is as test solution.
Chinese medicine has the characteristics that multicomponent, weak effect, coordinates integration, ingredient complicated composition, and the interaction between ingredient is made
With then increasingly complex.Although the identification for effective component in Chinese patent drug and content detection have more research at present, when pair
Camphor, borneol, the identification of menthol and detection research are less in anti-MUSK SHUHUOLING gelling agent, and these researchs mostly collect
In chromatographic conditions such as the mobile phase of liquid chromatogram, column temperature, elution flow rate, the dosage of solvent and concentration in the detection process adjustment
Optimization, and it is less for other step researchs of detection, and preparation process, that is, sample Study on pretreatment of especially sample is less,
The prior art mostly uses simple alcohol molten or ultrasonic MUSK SHUHUOLING gelling agent, but compound Chinese patent medicine complicated component,
Tens even several hundred kinds of components 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 broadens, divides
Do not open, miscellaneous peak mostly etc..Therefore, the separation and Extraction of Chinese patent drug effective component is cumbersome, is always the difficult point of drug inspection.And conventional
The crude extract complicated composition that preparation method of test article obtains, 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 effective component discrimination process is commonly present in sample chromatogram and comparison medicine wood color
Spectrum is compared, the unconspicuous problem of spot, examines menthol, camphor tree in MUSK SHUHUOLING gelling agent 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 identify
Method itself has certain problems, and especially pre-treating method is improper.
Summary of the invention
The technical problem to be solved by the present invention is in view of the foregoing drawbacks, provide the identification and content of a kind of traditional Chinese medicine gel
Measuring method.This method test solution chaff interferent is few, can increase the sensitivity of detector, protects chromatographic column, simple and feasible, quasi-
It is really quick, stability is good.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of identification 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: it takes MUSK SHUHUOLING gelling agent 3-5g to add 70% ethyl alcohol 30-50mL, seals, dipping
20-30min, ultrasonic 3-5min；It is heated to reflux 1-2h, is cooled to room temperature, is extracted 3 times with chloroform shaking, filtrate is evaporated, and residue adds
1mL dehydrated alcohol dissolution, shake up to get；
Contrast solution preparation: take menthol reference substance and borneol reference substance add dehydrated alcohol be made every 1mL contain 5mg and
The solution of 10mg；
Thin-layered chromatography experiment: each 5 μ L of test solution and control solution is drawn, is put respectively in same silica G thin layer
On plate, with benzene-ethyl acetate (18:2) for solvent, expansion, exhibition is taken out, is dried away from 12-14cm, sprays with 2% vanillin-sulfuric acid
It is clear to be heated to spot development at 105 DEG C for solution；In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, show identical
The spot of color；
(b) prepared by test solution: it takes MUSK SHUHUOLING gelling agent 3-5g to add 70% ethyl alcohol 30-50mL, seals, dipping
20-30min, ultrasonic 3-5min；It is heated to reflux 1-2h, 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 dehydrated alcohol dissolve, shake up to get；
Contrast solution preparation: camphor reference substance is taken to add methanol that solution of every 1mL containing 10mg is made；
Thin-layered chromatography experiment: each 10 μ L of test solution and control solution is drawn, is put respectively in same silica G thin layer
On plate, with petroleum ether-ethyl acetate (10: 0.5) for solvent, expansion, exhibition is taken out, is dried away from 11-13cm, smoked with iodine vapor
It is clear to spot development；In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown；
(2) content of Headspace Gas Chromatography camphor, borneol, menthol:
Chromatographic condition: DB-WAX quartz capillary chromatographic column；Carrier gas is high pure nitrogen, flow velocity 1.0-2.0mL/min；Hydrogen fire
Flame ionization detector；Temperature programming, keeps 5-8min, rises to 180- with 10-15 DEG C/min by 130-140 DEG C of initial temperature
190 DEG C of holding 4-6min；Split ratio 25-35:1；240-250 DEG C of injector temperature；Detector temperature: 250-270 DEG C.
Test solution preparation:
A. it takes MUSK SHUHUOLING gelling agent 3-5g to add methanol 30mL, seals, impregnate 20-30min；
B. flow back 1-2h, is cooled to room temperature, and takes filtrate 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: taking borneol, Camphorae and menthue reference substance appropriate, accurately weighed, adds methanol to be made molten
Liquid；
The preparation of negative control sample solution: remaining medicinal material outside borneol, remaining in addition to camphor are removed 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
Be free of 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；
Measurement: 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 bottle, cover close
Envelope, sets in 90 DEG C of insulating boxs and balances 30min, takes upper layer 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 even several hundred kinds of components 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 effective component
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
Identify and the preparation method of the test solution of assay, this method is simple, quickly, efficiently, collection extracts, 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 being taken to add 70% ethyl alcohol
30mL, sealing impregnate 30min, ultrasonic 4min；It is heated to reflux 1.5h, is cooled to room temperature, is extracted 3 times with chloroform shaking, filtrate is steamed
Dry, residue adds 1mL dehydrated alcohol to dissolve, shake up to get.
Further, chloroform used in the 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 being taken to add 70% second
Alcohol 50mL, sealing impregnate 25min, ultrasonic 5min；It is heated to reflux 1h, is cooled to room temperature, takes filtrate 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 dehydrated alcohol dissolve, shake up to get.
Further, the solid-phase extraction column using it is preceding using 8mL methanol activate, then plus 10mL washing go first in column
Alcohol crosses the flow control of solid-phase extraction column in 2-3s/ drop.
The perfect condition of chromatographic condition is to obtain higher separating degree in a relatively short period of time, and have column appropriate
Capacity.Select to consider when chromatographic column the physicochemical property of analyte, by the clastotype of use and separated object and solid
Determine the interaction of phase surface.
Further, the content of the Headspace Gas Chromatography camphor, borneol, menthol, chromatographic condition: DB-WAX stone
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, 6min is kept, 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 DEG C.
Further, the content of the Headspace Gas Chromatography camphor, borneol, menthol, test solution preparation: A.
It takes MUSK SHUHUOLING gelling agent 3g to add methanol 30mL, seals, impregnate 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 column.
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 beneficial effect of the invention jointly
Fruit.
The application passes through to improve and supplies in view of the above-mentioned problems, provide identification and the content assaying method of a kind of traditional Chinese medicine gel
The preparation method of test sample solution can increase the sensitive of detector so that chaff interferent is few in test solution, effective component is complete
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
Every other embodiment obtained under the premise of the property made labour, belongs to protection scope of the present invention.
Main test instrument: gas chromatograph (GC, Agilent Technologies 7890A, fid detector),
CPA225D electronic balance, DirectQ3System pure water meter, DS-7510DTH ultrasonic cleaner；
Reagent: agents useful for same is that analysis is pure；
Sample: MUSK SHUHUOLING gelling agent provides (lot number: 20170916) by Sichuan Guangda Pharmaceutical Co., Ltd.
Negative control sample: not mentholated negative control sample, not camphorated negative control sample and be free of 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 column (30m × 0.320mm × 0.5 μm)；Solid-phase extraction column: HLB column.
Embodiment 1
Thin-layer identification method:
(a) prepared by test solution: it takes MUSK SHUHUOLING gelling agent 3g to add 70% ethyl alcohol 30mL, seals, impregnate 30min,
Ultrasonic 4min；It is heated to reflux 1.5h, is cooled to room temperature, is extracted 3 times with chloroform shaking, chloroform used in 3 times is respectively 30mL, 20mL
And 20mL, filtrate are evaporated, residue add 1mL dehydrated alcohol dissolve, shake up to get；
Contrast solution preparation: take menthol reference substance and borneol reference substance add dehydrated alcohol be made every 1mL contain 5mg and
The solution of 10mg；
Thin-layered chromatography experiment: each 5 μ L of test solution and control solution is drawn, is put respectively in same silica G thin layer
On plate, with benzene-ethyl acetate (18:2) for solvent, expansion, exhibition is taken out, is dried away from 13cm, sprays molten with 2% vanillin-sulfuric acid
It is clear to be heated to spot development at 105 DEG C for liquid；In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, identical face is shown
The spot of color；
(b) test solution prepare: solid-phase extraction column using it is preceding using 8mL methanol activate, then plus 10mL washing go in column
Methanol；It takes MUSK SHUHUOLING gelling agent 5g to add 70% ethyl alcohol 50mL, seals, impregnate 25min, ultrasonic 5min；It is heated to reflux 1h, it is cold
But to room temperature, filtrate is taken after crossing 0.22 μm of filter membrane, filtrate crosses solid-phase extraction column, cross the flow control of solid-phase extraction column in 3s/ drop,
Eluted with chloroform, eluent is evaporated, residue add 1mL dehydrated alcohol dissolve, shake up to get；
Contrast solution preparation: camphor reference substance is taken to add methanol that solution of every 1mL containing 10mg is made；
Thin-layered chromatography experiment: each 10 μ L of test solution and control solution is drawn, is put respectively in same silica G thin layer
On plate, with petroleum ether-ethyl acetate (10: 0.5) for solvent, expansion, exhibition takes out away from 12cm, dries, smoked with iodine vapor to spot
Point colour developing is clear；In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown；
Clear spot obviously without hangover, boundless edge effect, can it is corresponding with reference substance on.
Embodiment 2
Thin-layer identification method:
(a) prepared by test solution: it takes MUSK SHUHUOLING gelling agent 4g to add 70% ethyl alcohol 50mL, seals, impregnate 30min,
Ultrasonic 3min；Be heated to reflux 1h, be cooled to room temperature, with chloroform shaking extract 3 times, chloroform used in 3 times be respectively 30mL, 20mL and
20mL, filtrate are evaporated, residue add 1mL dehydrated alcohol dissolve, shake up to get；
Contrast solution preparation: take menthol reference substance and borneol reference substance add dehydrated alcohol be made every 1mL contain 5mg and
The solution of 10mg；
Thin-layered chromatography experiment: each 5 μ L of test solution and control solution is drawn, is put respectively in same silica G thin layer
On plate, with benzene-ethyl acetate (18:2) for solvent, expansion, exhibition is taken out, is dried away from 14cm, sprays molten with 2% vanillin-sulfuric acid
It is clear to be heated to spot development at 105 DEG C for liquid；In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, identical face is shown
The spot of color；
(b) test solution prepare: solid-phase extraction column using it is preceding using 8mL methanol activate, then plus 10mL washing go in column
Methanol；It takes MUSK SHUHUOLING gelling agent 5g to add 70% ethyl alcohol 50mL, seals, impregnate 30min, ultrasonic 4min；1.5h is heated to reflux,
It is cooled to room temperature, takes filtrate 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 dehydrated alcohol dissolve, shake up to get；
Contrast solution preparation: camphor reference substance is taken to add methanol that solution of every 1mL containing 10mg is made；
Thin-layered chromatography experiment: each 10 μ L of test solution and control solution is drawn, is put respectively in same silica G thin layer
On plate, with petroleum ether-ethyl acetate (10: 0.5) for solvent, expansion, exhibition takes out away from 13cm, dries, smoked with iodine vapor to spot
Point colour developing is clear；In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown；
Clear spot obviously without hangover, boundless edge effect, can it is corresponding with reference substance on.
Comparative example 1
Thin-layer identification method:
(a) test solution prepare: take MUSK SHUHUOLING gelling agent 3g add 1mL dehydrated alcohol dissolve, shake up to get；
Contrast solution preparation: take menthol reference substance and borneol reference substance add dehydrated alcohol be made every 1mL contain 5mg and
The solution of 10mg；
Thin-layered chromatography experiment: each 5 μ L of test solution and control solution is drawn, is put respectively in same silica G thin layer
On plate, with benzene-ethyl acetate (18:2) for solvent, expansion, exhibition is taken out, is dried away from 13cm, sprays molten with 2% vanillin-sulfuric acid
It is clear to be heated to spot development at 105 DEG C for liquid；In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, identical face is shown
The spot of color；
(b) test solution prepare: take MUSK SHUHUOLING gelling agent 5g add 1mL dehydrated alcohol dissolve, shake up to get；
Contrast solution preparation: camphor reference substance is taken to add methanol that solution of every 1mL containing 10mg is made；
Thin-layered chromatography experiment: each 10 μ L of test solution and control solution is drawn, is put respectively in same silica G thin layer
On plate, with petroleum ether-ethyl acetate (10: 0.5) for solvent, expansion, exhibition takes out away from 12cm, dries, smoked with iodine vapor to spot
Point colour developing is clear；In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown；
Although spot can it is corresponding with reference substance on, spot is fuzzy without hangover, but edge effect is more obvious.
Embodiment 3
The content of Headspace Gas Chromatography camphor, borneol, menthol:
1.1 chromatographic conditions: DB-WAX quartz capillary chromatographic column (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 DEG C.
The preparation of 1.2 test solutions:
A. it takes MUSK SHUHUOLING gelling agent 3g to add methanol 30mL, seals, impregnate 20min；
B. flow back 1h, is cooled to room temperature, and takes filtrate 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: taking borneol, Camphorae and menthue reference substance appropriate, accurately weighed, and methanol is added to be made
Solution；
The preparation of 1.4 negative control sample solution: remaining medicinal material outside borneol, its in addition to camphor are removed respectively by prescription
Remaining medicinal material and remaining medicinal material in addition to menthol, be made without borneol negative control sample, without camphor negative control sample it is molten
Liquid and be free of menthol negative control sample, it is molten that scarce borneol negative control sample is made according to the preparation method of test solution
Liquid lacks camphor negative control sample solution and scarce menthol negative control sample solution；
1.5 measurements: 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 bottle, is covered close
Envelope, sets in 90 DEG C of insulating boxs and balances 30min, takes upper layer 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, add methanol to dissolve, be made camphor, menthol,
Borneol concentration is respectively the reference substance solution A of 4.8296,1.0475,1.9071mg/ml；Precision pipette reference substance solution A5ml in
In 10ml measuring bottle, with methanol constant volume to scale, reference substance solution B is obtained；Precision pipettes reference substance solution B5ml in 10ml measuring bottle,
With methanol constant volume to scale, reference substance solution C is obtained；Precision pipettes reference substance solution C5ml in 10ml measuring bottle, uses methanol constant volume
To scale, reference substance solution D is obtained；Precision pipettes reference substance solution D5ml in 10ml measuring bottle, 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 bottle, is sealed, set 90 DEG C of constant temperature
30min is balanced in case, takes upper layer saturated gas 1mL, is injected gas chromatograph, 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.
Each ingredient standard working curve regression equation of table 1 and linear relationship
2.2 precision test
Precision draws mixing reference substance 1mL, injects in 10mL ml headspace bottle, seals, set in 90 DEG C of insulating boxs and balance
30min takes upper layer saturated gas 1mL, injects gas chromatograph, continuous sample introduction 6 times, measures camphor, menthol, borneol peak face
Product, as a result the RSD value of peak area is respectively 0.52%, 0.61%, 0.63%, shows that instrument precision is good.
2.3 repetitive test
It takes with a collection of 6 parts of sample of MUSK SHUHUOLING gelling agent, 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 bottle, is sealed, set in 90 DEG C of insulating boxs and balance 30min, take upper layer 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%, 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 value of peak area is respectively 0.55%, 0.87%, 0.66%, shows that test solution is interior for 24 hours and stablizes.
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 stuffed conical flask, mixed reference substance solution A5ml are added, 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
It is accurate respectively to measure above-mentioned test solution, reference substance solution, lack borneol negative control sample solution, lack camphor yin
Property control sample solution and scarce each 1mL of menthol negative control sample solution, inject in 10mL ml headspace bottle, seal, set 90
30min is balanced in DEG C insulating box, takes upper layer saturated gas 1mL, gas chromatograph is injected, is detected.
Sample is measured in parallel 3 times, is averaged.The chromatographic peak of reference substance and sample is good, and negative control is to measurement without dry
It disturbs.Camphor, menthol and borneol content are calculated by external standard method；MUSK SHUHUOLING gelling agent is mentioned 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
The content of Headspace Gas Chromatography camphor, borneol, menthol:
Chromatographic condition: DB-WAX quartz capillary chromatographic column (30m × 0.320mm × 0.5 μm)；Carrier gas is high pure nitrogen,
Flow velocity 1.5mL/min；Flame ionization ditector；Temperature programming, keeps 6min, on 12 DEG C/min by 130 DEG C of initial temperature
Rise to 180 DEG C of holding 4min；Split ratio 25:1；250 DEG C of injector temperature；Detector temperature: 260 DEG C.
Test solution preparation:
It takes MUSK SHUHUOLING gelling agent 3g to add methanol 30mL, seals, impregnate 20min, maceration extract is evaporated, and residue adds methanol fixed
Hold to 10mL, shake up to get.
The preparation of reference substance solution: taking borneol, Camphorae and menthue reference substance appropriate, accurately weighed, adds methanol to be made molten
Liquid；
The preparation of negative control sample solution: remaining medicinal material outside borneol, remaining in addition to camphor are removed 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
Be free of 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；
Measurement: 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 bottle, cover close
Envelope, sets in 90 DEG C of insulating boxs and balances 30min, takes upper layer saturated gas 1mL, injects gas chromatograph, is detected.
Sample is measured in parallel 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
The content of Headspace Gas Chromatography camphor, borneol, menthol:
Chromatographic condition: DB-WAX quartz capillary chromatographic column (30m × 0.320mm × 0.5 μm)；Carrier gas is high pure nitrogen,
Flow velocity 1.5mL/min；Flame ionization ditector；Temperature programming, keeps 6min, on 12 DEG C/min by 130 DEG C of initial temperature
Rise to 180 DEG C of holding 4min；Split ratio 25:1；250 DEG C of injector temperature；Detector temperature: 260 DEG C.
Test solution preparation:
MUSK SHUHUOLING gelling agent 3g is taken to add methanol 30mL, flow back 1h, is cooled to room temperature, and takes filter 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: taking borneol, Camphorae and menthue reference substance appropriate, accurately weighed, adds methanol to be made molten
Liquid；
The preparation of negative control sample solution: remaining medicinal material outside borneol, remaining in addition to camphor are removed 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
Be free of 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；
Measurement: 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 bottle, cover close
Envelope, sets in 90 DEG C of insulating boxs and balances 30min, takes upper layer saturated gas 1mL, injects gas chromatograph, is detected.
Sample is measured in parallel 3 times, is averaged.The chromatographic peak of reference substance is good, and negative control is to noiseless, the sample of measurement
Chromatographic peak separating degree is lower, and stability and precision are low.Camphor, menthol and borneol content are calculated by external standard method；Moschus, which relaxes, lives
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
The content of Headspace Gas Chromatography camphor, borneol, menthol:
Chromatographic condition: DB-WAX quartz capillary chromatographic column (30m × 0.320mm × 0.5 μm)；Carrier gas is high pure nitrogen,
Flow velocity 1.5mL/min；Flame ionization ditector；Temperature programming, keeps 6min, on 12 DEG C/min by 130 DEG C of initial temperature
Rise to 180 DEG C of holding 4min；Split ratio 25:1；250 DEG C of injector temperature；Detector temperature: 260 DEG C.
Test solution preparation:
It takes MUSK SHUHUOLING gelling agent 3g to add methanol 30mL, takes filtrate after crossing 0.22 μm of filter membrane；Solid-phase extraction column is taken, water is used
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: taking borneol, Camphorae and menthue reference substance appropriate, accurately weighed, adds methanol to be made molten
Liquid；
The preparation of negative control sample solution: remaining medicinal material outside borneol, remaining in addition to camphor are removed 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
Be free of 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；
Measurement: 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 bottle, cover close
Envelope, sets in 90 DEG C of insulating boxs and balances 30min, takes upper layer saturated gas 1mL, injects gas chromatograph, is detected.
Sample is measured in parallel 3 times, is averaged.The chromatographic peak of reference substance and sample is good, and negative control is to measurement without dry
It disturbs.Camphor, menthol and borneol content are calculated by external standard method；MUSK SHUHUOLING gelling agent is mentioned 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
According to a kind of identification of traditional Chinese medicine gel and content assaying method disclosed in Chinese patent CN104807896A, as a result
Show that each chromatographic peak and reference substance and reference medicine chromatography peak correspond in sample chromatogram figure, 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
The content of Headspace Gas Chromatography camphor, borneol, menthol:
Chromatographic condition: DB-WAX quartz capillary chromatographic column (30m × 0.320mm × 0.5 μm)；Carrier gas is high pure nitrogen,
Flow velocity 2mL/min；Flame ionization ditector；Temperature programming, keeps 5min by 140 DEG C of initial temperature, with 15 DEG C/min rising
To 190 DEG C of holding 6min；Split ratio 35:1；250 DEG C of injector temperature；Detector temperature: 250 DEG C.
Test solution preparation:
A. it takes MUSK SHUHUOLING gelling agent 4g to add methanol 30mL, seals, impregnate 25min；
B. flow back 1.5h, is cooled to room temperature, and takes filtrate 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: taking borneol, Camphorae and menthue reference substance appropriate, accurately weighed, adds methanol to be made molten
Liquid；
The preparation of negative control sample solution: remaining medicinal material outside borneol, remaining in addition to camphor are removed 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
Be free of 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；
Measurement: 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 bottle, cover close
Envelope, sets in 90 DEG C of insulating boxs and balances 30min, takes upper layer saturated gas 1mL, injects gas chromatograph, is detected.
Sample is measured in parallel 3 times, is averaged.The chromatographic peak of reference substance and sample is good, and negative control is to measurement without dry
It disturbs.Camphor, menthol and borneol content are calculated by external standard method；MUSK SHUHUOLING gelling agent is mentioned 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
The content of Headspace Gas Chromatography camphor, borneol, menthol:
Chromatographic condition: DB-WAX quartz capillary chromatographic column (30m × 0.320mm × 0.5 μm)；Carrier gas is high pure nitrogen,
Flow velocity 1mL/min；Flame ionization ditector；Temperature programming, keeps 5min by 135 DEG C of initial temperature, with 10 DEG C/min rising
To 190 DEG C of holding 5min；Split ratio 30:1；240 DEG C of injector temperature；Detector temperature: 270 DEG C.
Test solution preparation:
A. it takes MUSK SHUHUOLING gelling agent 5g to add methanol 30mL, seals, impregnate 30min；
B. flow back 2h, is cooled to room temperature, and takes filtrate 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: taking borneol, Camphorae and menthue reference substance appropriate, accurately weighed, adds methanol to be made molten
Liquid；
The preparation of negative control sample solution: remaining medicinal material outside borneol, remaining in addition to camphor are removed 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
Be free of 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；
Measurement: 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 bottle, cover close
Envelope, sets in 90 DEG C of insulating boxs and balances 30min, takes upper layer saturated gas 1mL, injects gas chromatograph, is detected.
Sample is measured in parallel 3 times, is averaged.The chromatographic peak of reference substance and sample is good, and negative control is to measurement without dry
It disturbs.Camphor, menthol and borneol content are calculated by external standard method；MUSK SHUHUOLING gelling agent is mentioned 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
The content of Headspace Gas Chromatography camphor, borneol, menthol:
Chromatographic condition: DB-WAX quartz capillary chromatographic column (30m × 0.320mm × 0.5 μm)；Carrier gas is high pure nitrogen,
Flow velocity 1.5mL/min；Flame ionization ditector；Temperature programming, keeps 8min, on 15 DEG C/min by 130 DEG C of initial temperature
Rise to 185 DEG C of holding 5min；Split ratio 30:1；250 DEG C of injector temperature；Detector temperature: 260 DEG C.
Test solution preparation:
A. it takes MUSK SHUHUOLING gelling agent 3g to add methanol 30mL, seals, impregnate 30min；
B. flow back 1.5h, is cooled to room temperature, and takes filtrate 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: taking borneol, Camphorae and menthue reference substance appropriate, accurately weighed, adds methanol to be made molten
Liquid；
The preparation of negative control sample solution: remaining medicinal material outside borneol, remaining in addition to camphor are removed 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
Be free of 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；
Measurement: 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 bottle, cover close
Envelope, sets in 90 DEG C of insulating boxs and balances 30min, takes upper layer saturated gas 1mL, injects gas chromatograph, is detected.
Sample is measured in parallel 3 times, is averaged.The chromatographic peak of reference substance and sample is good, and negative control is to measurement without dry
It disturbs.Camphor, menthol and borneol content are calculated by external standard method；MUSK SHUHUOLING gelling agent is mentioned 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.
Detection method of the invention, hence it is evident that be 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 constituted, produces apparent synergistic function.
The above description is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, all utilizations
Equivalent structure or equivalent flow shift made by description of the invention is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (10)
1. identification 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: taking MUSK SHUHUOLING gelling agent 3-5g to add 70% ethyl alcohol 30-50mL, seals, impregnates 20-
30min, ultrasonic 3-5min；It is heated to reflux 1-2h, is cooled to room temperature, is extracted 3 times with chloroform shaking, filtrate is evaporated, and residue adds 1mL
Dehydrated alcohol dissolution, shake up to get；
Contrast solution preparation: menthol reference substance and borneol reference substance is taken to add dehydrated alcohol that every 1mL is made respectively containing 5mg's and 10mg
Mixed solution；
Thin-layered chromatography experiment: drawing each 5 μ L of test solution and control solution, is put respectively on same silica gel g thin-layer plate,
Using benzene-ethyl acetate=18:2 as solvent, expansion, exhibition is taken out, is dried away from 12-14cm, spray with 2% vanillin-sulfuric acid solution,
105 DEG C to be heated to spot development clear；In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, same color is shown
Spot；
(b) prepared by test solution: taking MUSK SHUHUOLING gelling agent 3-5g to add 70% ethyl alcohol 30-50mL, seals, impregnates 20-
30min, ultrasonic 3-5min；It is heated to reflux 1-2h, 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 dehydrated alcohol dissolve, shake up to get；
Contrast solution preparation: camphor reference substance is taken to add methanol that solution of every 1mL containing 10mg is made；
Thin-layered chromatography experiment: each 10 μ L of test solution and control solution is drawn, is put respectively in same silica gel g thin-layer plate
On, using petroleum ether-ethyl acetate=10:0.5 as solvent, expansion, exhibition is taken out away from 11-13cm, is dried, is smoked with iodine vapor to spot
Point colour developing is clear；In sample chromatogram, at the position corresponding to the chromatogram of the reference substance, the spot of same color is shown；
(2) content of Headspace Gas Chromatography camphor, borneol, menthol:
Chromatographic condition: DB-WAX quartz capillary chromatographic column；Carrier gas is high pure nitrogen, flow velocity 1.0-2.0mL/min；Hydrogen flame from
Sonization detector；Temperature programming, keeps 5-8min, rises to 180-190 DEG C with 10-15 DEG C/min by 130-140 DEG C of initial temperature
Keep 4-6min；Split ratio 25-35:1；240-250 DEG C of injector temperature；Detector temperature: 250-270 DEG C；
Test solution preparation:
A. it takes MUSK SHUHUOLING gelling agent 3-5g to add methanol 30mL, seals, impregnate 20-30min；
B. flow back 1-2h, is cooled to room temperature, and takes filtrate 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: taking borneol, Camphorae and menthue reference substance appropriate, accurately weighed, adds methanol that solution is made；
The preparation of negative control sample solution: remaining medicinal material outside borneol, remaining medicinal material in addition to camphor are removed respectively by prescription
With remaining medicinal material in addition to menthol, it is 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；
Measurement: 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 bottle, seal, set
30min is balanced in 90 DEG C of insulating boxs, takes upper layer saturated gas 1mL, gas chromatograph is injected, is detected.
2. identification 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. identification 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. identification 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: it takes MUSK SHUHUOLING gelling agent 3g to add 70% ethyl alcohol 30mL, seals, dipping
30min, ultrasonic 4min；Be heated to reflux 1.5h, be cooled to room temperature, with chloroform shaking extract 3 times, filtrate is evaporated, residue add 1mL without
Water-ethanol dissolution, shake up to get.
5. identification and the content assaying method of a kind of traditional Chinese medicine gel according to claim 4, which is characterized in that described
Chloroform used in chloroform shaking extraction 3 times is respectively 30mL, 20mL and 20mL.
6. identification 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: it takes MUSK SHUHUOLING gelling agent 5g to add 70% ethyl alcohol 50mL, seals, dipping
25min, ultrasonic 5min；It is heated to reflux 1h, is cooled to room temperature, takes filtrate after crossing 0.22 μm of filter membrane, filtrate crosses solid-phase extraction column, uses
Chloroform elution, eluent is evaporated, and residue adds 1mL dehydrated alcohol to dissolve, shake up to get.
7. identification 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 plus 10mL washing remove methanol in column, cross the flow control of solid-phase extraction column
In 2-3s/ drop.
8. identification 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 column；Carrier gas is
High pure nitrogen, flow velocity 1.5mL/min；Flame ionization ditector；Temperature programming, keeps 6min by 130 DEG C of initial temperature, 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 DEG C.
9. identification 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, and test solution preparation: A. takes MUSK SHUHUOLING gelling agent 3g
Add methanol 30mL, seal, impregnates 20min；B. flow back 1h, is cooled to room temperature, and takes filtrate 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 10mL, shakes up, i.e.,
?.
10. identification 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 column.
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