CN109541045B - The active components content assaying method such as a kind of halimasch and its product Asclerol - Google Patents
The active components content assaying method such as a kind of halimasch and its product Asclerol Download PDFInfo
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- CN109541045B CN109541045B CN201811054880.5A CN201811054880A CN109541045B CN 109541045 B CN109541045 B CN 109541045B CN 201811054880 A CN201811054880 A CN 201811054880A CN 109541045 B CN109541045 B CN 109541045B
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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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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Abstract
It is the content assaying method of the benzoic acid Protoilludane sesquiterpenoid ester derivant active component of intermediate, the manufactured goods such as halimasch powder, Asclerol, armillaria mellea accreting with Rhizoma Gastrodiae piece of main or secondary raw material etc. the present invention relates to a kind of halimasch, halimasch liquid or solid fermentation object and with the above substance.The present invention is by ultraviolet-visible spectrophotometry, using benzoic acid derivative as reference substance, measures the molar content of benzoic acid Protoilludane sesquiterpenoid ester derivant active component.This method is with strong points, and easy to operate quickly testing cost is low, and the quality control and activity suitable for halimasch and products thereof ensure.
Description
Technical field
The present invention relates to the field of Chinese medicines, in particular to a kind of halimasch, halimasch liquid or solid fermentation object and with above
Substance is that the benzoic acid of intermediate, manufactured goods such as halimasch powder, Asclerol, armillaria mellea accreting with Rhizoma Gastrodiae piece of main or secondary raw material etc. is former
The content assaying method of Yi Lu alkane type Sesquiterpene Polyesterss derivative active component.
Background technique
HalimaschArmillaria MelleaFor Basidiomycotina fungi, belong to Agaricales, Tricholomataceae, Armillaria, not
Name: Armillariella mellea attains mushroom, sweet mushroom, sweet ring gill fungus, oak gill fungus, is a kind of common edible and medicinal fungi.Research has shown that halimasch and its fermentation produce
Object contains a variety of active ingredients such as polysaccharide, Protoilludane sesquiterpenoid, diterpene, triterpene and purine compound, especially with benzene first
Sour Protoilludane sesquiterpenoid ester derivant is most representative.It is proved through functional experiment, halimasch and its tunning have
Hypoglycemic, nervous centralis adjusts, improves the functions such as immunity of organisms.
Asclerol oral solution is made of halimasch Fermented Condensed liquid, two taste medicine of royal jelly, has strengthening by means of tonics, calm peace
The effect of refreshing, it to be used in poor health, confused and worried, insomnia and dreamful sleep, neurasthenia, headache and dizziness belongs to above-mentioned patient.Asclerol
Oral solution is common Chinese patent drug, and manufacturing enterprise shares 110 at present, is related to authentication code 110.Asclerol oral solution matter
Amount standard is recorded in the 20th " national standard for traditional Chinese medicines compilation channels and collaterals limbs brain of " the Sanitation Ministry medicine standard " Traditional Chinese medicine historical preparation
It is fascicle ", the National Drug Administration national drug standards WS3-B-3975-98-2002 and WS-11356(ZD-
1356) -2002.Prescription preparation method is consistent, but each standard is not quite similar.Each standard has the thin layer of 10-HAD
Identify item, but the national drug standards WS3-B-3975-98-2002 that most of enterprise executes measures item without component content, no
It can guarantee product quality, more lack identification and quantitative analysis to important component halimasch in Asclerol oral solution.With sweet ring
Bacterium be raw material Chinese patent medicine preparation there are also armillaria mellea accreting with Rhizoma Gastrodiae piece, armillaria mellea accreting with Rhizoma Gastrodiae capsule, compound armillaria mellea piece, compound uncarias
Piece etc., though thin-layer chromatography identification is devised by reference substance of halimasch control medicinal material in a standard, and using titration measuring honey
Ring bacterium converts into the content of mannitol, but for assay angle, standard is still short of specific aim, detected substance mannitol by
In exist in various plants and and be not belonging to the main active substances of halimasch so as to execute meaning poor for the quantitative approach.
In addition, being the healthcare food product of raw material there are also clear rhythm granule using halimasch, primary raw material is armillaria mycelium, sieve
Cloth fiber crops, pueraria lobata, xylitol, the quality regulation content of Puerarin and halimasch element；And kind gracilistylus capsule, primary raw material are
The rhizome of davallia, Cortex Eucommiae, Herba Epimedii, Poria cocos, halimasch, black fungus, quality only define the content of Thick many candies and general flavone.
To sum up, halimasch and still too low as the quality control method of the product of raw material using halimasch at present, and specific aim is poor,
It is difficult to meet the control of halimasch and products thereof quality of production, the requirements of support of drug effect and clinical effect effect.
Summary of the invention
Based on the above reasons, the present invention provides a kind of halimasch, halimasch liquid or solid fermentation object and with the above object
Matter be the benzoic acid of main or secondary raw material intermediate, manufactured goods such as halimasch powder, Asclerol, armillaria mellea accreting with Rhizoma Gastrodiae piece etc. it is former she
The content assaying method and this method of Shandong alkane type Sesquiterpene Polyesterss derivative active component are in halimasch and products thereof quality of production
Purposes in control and drug effect guarantee.
To achieve the goals above, technical solution of the present invention comprises the steps of:
(1) preparation of test solution: solvent extraction method is used if solid sample, if fluid sample using extraction
Method is further purified using chromatography, is configured to the test solution of suitable concentration；
(2) it the preparation of reference substance solution: selects benzoic acid derivative as reference substance, is configured to the reference substance of suitable concentration
Solution；
(3) it content assaying method: uses ultraviolet-visible spectrophotometry (colorimetric method), ultraviolet specrophotometer, enzyme mark
Instrument reads absorbance A, OD value in 200-220 nm, 250-270 nm, 290-310 nm range optimal wavelength, using standard curve
Method, external standard method calculate benzoic acid Protoilludane sesquiterpenoid ester derivant active component content.
Term explanation: 1. terms used hereins " solid sample " refer to halimasch, halimasch fructification, halimasch mycelia
Body, halimasch solid fermentation object, Armillaria mellea fermented solution dry product, with halimasch or halimasch object (liquid fermentation and solid fermentation)
For the extract of raw material, the product (food, health food, drug) of solid forms.2. terms used herein " solvent extraction method "
Refer to organic solvent, water etc. for solvent dipping, decoct, be heated to reflux, ultrasonic wave added, microwave-assisted isoreactivity substance extract
Use method.3. terms used herein " fluid sample " refers to Armillaria mellea fermented solution and its concentrate, fermented with halimasch, halimasch
Object (liquid fermentation and solid fermentation) is the product (food, health food, drug) of the extracting solution of raw material, liquid form.4.
Term used in text " chromatography " refers to large pore resin absorption column chromatography, silica gel chromatograph, polyamide chromatography, gel chromatography, active carbon
The method that chromatography, chromatography on alumina etc. are enriched with for active constituent, isolate and purify.5. terms used herein " benzoic acid derivative "
It is preferred that 2,4- dihydroxy-benzoic acid and its ester series compound, 2- methyl -4,6- dihydroxy-benzoic acid and its ester series compound,
2- methyl -6- hydroxyl -4- methoxy benzoic acid and its ester series compound, 2- methyl -6- hydroxyl -4- methoxyl group -5- chlorobenzene first
Acid and its ester series compound, further preferred 2,4- methyl dihydroxy benzoate, 2- methyl -4,6- dihydroxy-benzoic acid first
Ester, 2- methyl -6- hydroxyl -4- methoxyl methyl benzoate, 2- methyl -6- hydroxyl -4- methoxy-5-chlorobenzoic acid methyl esters, honey
Ring fungus beetle element-Kui prime, halimasch element-fourth of the twelve Earthly Branches element, halimasch acid, halimasch occasion element-oneself element, melleolide A-M,
Melledonal A-E etc..
Benzoic acid Protoilludane sesquiterpenoid ester derivant is effective in the preferred samples such as halimasch and Asclerol oral solution
Position assay solution are as follows:
(1) preparation of test solution: the liquid sample taken water as a solvent such as Asclerol oral solution is extracted with ethyl acetate
Take, ethyl acetate layer constant volume at suitable concentration test solution；It using alcohol as the liquid sample of solvent, is evaporated, residue acetic acid
Ethyl ester extracts, and with ethyl acetate constant volume at the test solution of suitable concentration；Solid sample is extracted with ethyl acetate, and with second
Acetoacetic ester constant volume at suitable concentration test solution；
(2) preparation of reference substance solution: with 2- methyl -4,6- methyl dihydroxy benzoate or 2,4- dihydroxy-benzoic acid first
Ester is reference substance, is configured to the reference substance solution of suitable concentration；
(3) content assaying method: ultraviolet-visible spectrophotometry is used, ultraviolet specrophotometer is in 260 nm -265
Test solution and control solution absorbance A value is measured at nm respectively, benzoic acid Protoilludanes type times is calculated using external standard method
Hemiterpene ester derivant active component content, and provided with molar concentration.
Compared with prior art, present invention has an advantage that
(1) method has stronger specific aim: benzoic acid Protoilludane sesquiterpenoid class compound is halimasch and its hair
Characteristic activities in ferment object become.Spread out in halimasch and its fermentation material containing polysaccharide, benzoic acid Protoilludane sesquiterpenoid ester
A variety of active ingredients such as biology, diterpene, triterpene and purine compound, in these active constituents, with benzoic acid Protoilludanes
Type Sesquiterpene Polyesterss derivative is most representative, separated at present to identify nearly 50 kinds of benzoic acid Protoilludane sesquiterpenoid ester derivative
Object, these compounds there's almost no in other biologies.
(2) method novelty is innovated: there is presently no benzoic acid in any document report halimasch and its Related product it is former she
The content assaying method of Shandong alkane type Sesquiterpene Polyesterss derivative active component, the invention select benzoic acid derivative simple and easy to get simultaneously
It is preferred that 2,4- methyl dihydroxy benzoates or 2- methyl -4,6- methyl dihydroxy benzoate are reference substance, using it is easy, applicable,
Benzoic acid Protoilludanes type sesquialter in universal ultraviolet-visible spectrophotometry (colorimetric method) measurement halimasch and its Related product
The molar concentration of terpene ester derivant active component, the innovation of method novelty.
(3) enforceability easy to operate is strong: active component assay involved in the invention, and test sample preparation is using molten
One or more of conventional methods such as agent extraction method, extraction, chromatography, the test sample for being then configured to suitable concentration are molten
Liquid；The benzoic acid derivative for preparing suitable concentration simultaneously is reference substance solution；Two kinds of solution are used into colorimetric method for determining A value,
The content of benzoic acid Protoilludane sesquiterpenoid ester derivant active component in test sample is calculated by external standard method, or using mark
Directrix curve method calculates content, and method is easy to operate, and experimental result intuitively expresses benzoic acid Protoilludane sesquiterpenoid ester in sample
The amount content of derivative active component substance, enforceability are strong.
(4) testing cost is low: active component assay involved in the invention, does not need expensive chemical reagent, right
Conventional chemical reagent benzoate derivatives, preferably 2,4- methyl dihydroxy benzoate or 2- methyl -4,6- dihydroxy are used according to product
Yl benzoic acid methyl esters is easy to obtain, and cheap relative to the micro rare secondary metabolite in biology, therefore
This method cost is extremely low.
Specific embodiment
For the more detailed description present invention, following assay examples are provided.But the scope of the present invention is simultaneously not only limited to
In this.
Embodiment 1: containing for benzoic acid Protoilludane sesquiterpenoid ester derivant active component measures in halimasch concentrate
It is fixed
1.1 instruments and reagent
Reagent: halimasch concentrate, ethyl acetate, 2,4- methyl dihydroxy benzoates (MW168.15, purity > 98%).
Instrument and equipment: UV6100 dual-beam ultraviolet-uisible spectrophotometer (U.S. spectrum in Shanghai reaches Instrument Ltd.), quartz
Cuvette.
Benzoic acid Protoilludane sesquiterpenoid ester derivant active component content assaying method in 1.2 samples
1.2.1 the preparation of test solution
Precision measures 1 mL of halimasch concentrate, adds distilled water 9mL, and ethyl acetate extracts 3 times, and 10 mL, merges second every time
Ethyl acetate layer adds ethyl acetate to be settled in 100 mL volumetric flasks, as test solution.
1.2.2 the preparation of reference substance solution
Precision weighs that 2,4- methyl dihydroxy benzoate is appropriate, and ethyl acetate is added to be prepared into the solution of series of concentrations:
0.001mg/mL(5.947 μm of ol/L), 0.002mg/mL(11.894 μm of ol/L), 0.004mg/mL(23.788 μm of ol/L),
0.008mg/mL(47.577 μm of ol/L), 0.010mg/mL(59.471 μm of ol/L), 0.020mg/mL(118.941 μm of ol/L).
1.2.3 the preparation of standard curve
The reference substance solution of series of concentrations is measured into absorbance A value at ultraviolet specrophotometer 260nm wavelength, is inhaled
Luminosity A(reference substance concentration) data pair, standard curve is drawn, equation of linear regression is calculated.
1.2.4 sample size measures
Test solution is measured into absorbance A value at ultraviolet-uisible spectrophotometer 260nm wavelength, brings standard curve into
Equation of linear regression calculates benzoic acid Protoilludane sesquiterpenoid ester derivant active component content.
1.3 methodological study
1.3.1 the preparation of standard curve and the range of linearity are investigated
The reference substance solution of series of concentrations is measured into absorbance A value at ultraviolet specrophotometer 260nm wavelength, is inhaled
Luminosity A(reference substance concentration) data pair: 0.09408(5.947 μm of ol/L), 0.18858(11.894 μm of ol/L), 0.37464
(23.788 μm of ol/L), 0.64776(47.577 μm of ol/L), 0.82428(59.471 μm of ol/L), 1.55844(118.941 μ
Mol/L), the linear equation of calculating is A=12.844C+0.0417, coefficient R2=0.998, illustrate this method in 5.947 μ
Linear relationship is good within the scope of mol/L-118.941 μm of ol/L.
1.3.2 precision is investigated
It takes test solution that quartz colorimetric utensil is added in right amount, is placed in ultraviolet-uisible spectrophotometer, A is measured at 260 nm
Value, METHOD FOR CONTINUOUS DETERMINATION 6 times.As a result 6 measurement A value average values are 0.48049, RSD=0.37%, illustrate that this method precision is good.
1.3.3 study on the stability
Test solution is taken, measures A value at 260 nm, it is primary every 2 h measurement, it measures 6 times.As a result 6 measurement A values are flat
Mean value is 0.47596, RSD=1.12%, illustrates to keep stablizing in 12 h of test solution.
1.3.4 reproducibility is investigated
It is independent to measure by 6 parts of the independently prepared test solution of test solution preparation method with a batch halimasch concentrate
A value, and bring the content that standard curve calculates benzoic acid Protoilludane sesquiterpenoid ester derivant active component in sample into.As a result
Active component average content is 3.44 μm of ol/mL in 6 independent measurement samples, and RSD=1.93% illustrates that this method reproducibility is good
It is good.
1.3.5 the rate of recovery is investigated
Precision measures 9 parts of 0.5 mL of halimasch concentrate, and it is appropriate to be separately added into 2,4- methyl dihydroxy benzoate, by supplying
Test sample solution preparation method prepares test solution, measures A value, brings standard curve into and calculates active component content, and calculates back
Yield.As a result the rate of recovery is between 97.3%-102.1%, average recovery rate 99.8%, RSD=1.98%, illustrates that this method is loaded
The rate of recovery is preferable.
The measurement of 1.4 sample sizes
Take 3 batches, halimasch concentrate sample, prepare test solution according to sample solution preparation method, and in it is ultraviolet can
See at spectrophotometer 260nm wavelength measurement absorbance A value, bring standard curve equation of linear regression into, calculate benzoic acid it is former she
Shandong alkane type Sesquiterpene Polyesterss derivative active component content.As a result benzoic acid Protoilludane sesquiterpenoid in 3 batches of halimasch concentrates
Ester derivant active component content is respectively 3.47 μm of ol/mL, 3.65 μm of ol/mL, 3.58 μm of ol/mL.
Embodiment 2: the assay of benzoic acid Protoilludane sesquiterpenoid ester derivant active component in Armillariella mellea
1.1 instruments and reagent
Reagent: Armillariella mellea, ethyl acetate, 2- methyl -4,6- methyl dihydroxy benzoate (WM182.17, purity > 98%).
Instrument and equipment: UV6100 dual-beam ultraviolet-uisible spectrophotometer (U.S. spectrum in Shanghai reaches Instrument Ltd.), quartz
Cuvette.
The preparation of 1.2 reference substance solutions
It is appropriate that precision weighs 2- methyl -4,6- methyl dihydroxy benzoate, adds ethyl acetate to be prepared into concentration and is
0.010mg/mL(54.894 μm of ol/L) solution.
The preparation of 1.3 test solutions
Armillariella mellea crushes, and takes 1g, accurately weighed, adds 100 mL of ethyl acetate, is ultrasonically treated 30 min, supplies volume, filters,
Take subsequent filtrate as test solution.
The measurement of 1.4 sample sizes
Test solution and control solution are taken, is respectively placed in measure at 265 nm wavelength of ultraviolet-uisible spectrophotometer and inhale
Luminosity A value calculates benzoic acid Protoilludane sesquiterpenoid ester derivant active component content in sample using one point external standard method.Knot
In 3 batches of Armillariella mellea samples of fruit benzoic acid Protoilludane sesquiterpenoid ester derivant active component content be respectively 6.87 μm of ol/g,
5.69μmol/g、4.82μmol/g。
Embodiment 3: containing for benzoic acid Protoilludane sesquiterpenoid ester derivant active component measures in Asclerol oral solution
It is fixed
1.1 instruments and reagent
Reagent: Asclerol oral solution, ethyl acetate, 2,4- methyl dihydroxy benzoates (MW168.15, purity > 98%).
Instrument and equipment: UV6100 dual-beam ultraviolet-uisible spectrophotometer (U.S. spectrum in Shanghai reaches Instrument Ltd.), quartz
Cuvette.
The preparation of 1.2 reference substance solutions
It is appropriate that precision weighs 2,4- methyl dihydroxy benzoate, and adding ethyl acetate to be prepared into concentration is 0.010mg/mL
The solution of (59.471 μm of ol/L).
The preparation of 1.3 test solutions
Precision measures Asclerol oral solution 1mL, adds distilled water 9mL, and ethyl acetate extracts 3 times, and 10 mL, merges second every time
Ethyl acetate layer adds ethyl acetate to be settled in 100 mL volumetric flasks, as test solution.
The measurement of 1.4 sample sizes
Test solution and control solution are taken, is respectively placed in measure at ultraviolet-uisible spectrophotometer 260nm wavelength and inhale
Luminosity A value calculates benzoic acid Protoilludane sesquiterpenoid ester derivant active component content in sample using one point external standard method.Knot
Benzoic acid Protoilludane sesquiterpenoid ester derivant active component content is respectively 2.13 μ in 3 batches of Asclerol oral solution samples of fruit
mol/mL、2.08μmol/mL、2.25μmol/mL。
Embodiment 4: the assay of benzoic acid Protoilludane sesquiterpenoid ester derivant active component in halimasch powder
1.1 instruments and reagent
Reagent: halimasch powder, ethyl acetate, 2,4- methyl dihydroxy benzoates (MW168.15, purity > 98%).
Instrument and equipment: UV6100 dual-beam ultraviolet-uisible spectrophotometer (U.S. spectrum in Shanghai reaches Instrument Ltd.), quartz
Cuvette.
The preparation of 1.2 reference substance solutions
It is appropriate that precision weighs 2,4- methyl dihydroxy benzoate, and adding ethyl acetate to be prepared into concentration is 0.010mg/mL
The solution of (59.471 μm of ol/L).
The preparation of 1.3 test solutions
Halimasch powder 0.5g is taken, it is accurately weighed, add 100 mL of ethyl acetate, is ultrasonically treated 30 min, supplies volume, mistake
Filter, takes subsequent filtrate as test solution.
The measurement of 1.4 sample sizes
Test solution and control solution are taken, is respectively placed in measure at ultraviolet-uisible spectrophotometer 260nm wavelength and inhale
Luminosity A value calculates benzoic acid Protoilludane sesquiterpenoid ester derivant active component content in sample using one point external standard method.Knot
Benzoic acid Protoilludane sesquiterpenoid ester derivant active component content is respectively 7.05 μm of ol/ in 3 batches of halimasch powder samples of fruit
g、7.39μmol/g、6.98μmol/g。
Embodiment 5: containing for benzoic acid Protoilludane sesquiterpenoid ester derivant active component measures in armillaria mellea accreting with Rhizoma Gastrodiae piece
It is fixed
1.1 instruments and reagent
Reagent: armillaria mellea accreting with Rhizoma Gastrodiae piece (0.33g/ piece), ethyl acetate, 2,4- methyl dihydroxy benzoates (MW168.15, it is pure
Degree > 98%).
Instrument and equipment: UV6100 dual-beam ultraviolet-uisible spectrophotometer (U.S. spectrum in Shanghai reaches Instrument Ltd.), quartz
Cuvette.
The preparation of 1.2 reference substance solutions
It is appropriate that precision weighs 2,4- methyl dihydroxy benzoate, and adding ethyl acetate to be prepared into concentration is 0.010mg/mL
The solution of (59.471 μm of ol/L).
The preparation of 1.3 test solutions
Armillaria mellea accreting with Rhizoma Gastrodiae piece 10 are taken, finely ground mixing takes 0.5g, and it is accurately weighed, add 100 mL of ethyl acetate, is ultrasonically treated
30 min supply volume, and filtering takes subsequent filtrate as test solution.
The measurement of 1.4 sample sizes
Test solution and control solution are taken, is respectively placed in measure at ultraviolet-uisible spectrophotometer 260nm wavelength and inhale
Luminosity A value calculates benzoic acid Protoilludane sesquiterpenoid ester derivant active component content in sample using one point external standard method.Knot
Benzoic acid Protoilludane sesquiterpenoid ester derivant active component content is respectively 1.68 μ in 3 batches of armillaria mellea accreting with Rhizoma Gastrodiae piece samples of fruit
Mol/ piece, 1.86 μm of ol/ pieces, 1.74 μm of ol/ pieces.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Made any modifications, equivalent replacements, and improvements etc., is all included in the scope of protection of the present invention within principle.
Claims (2)
1. a kind of halimasch, halimasch liquid fermentation material, halimasch solid fermentation object and with the above substance be main, secondary raw material
The content assaying method of benzoic acid Protoilludane sesquiterpenoid ester derivant active component in manufactured intermediate, finished product, it is special
Sign is, comprises the steps of:
(1) preparation of test solution: the liquid sample taken water as a solvent is extracted with ethyl acetate, ethyl acetate layer constant volume at
The test solution of suitable concentration；It using alcohol as the liquid sample of solvent, is evaporated, residue with ethyl acetate extracts, and with acetic acid second
Ester constant volume at suitable concentration test solution；Solid sample is extracted with ethyl acetate, and with ethyl acetate constant volume at being suitable for dense
The test solution of degree；
(2) preparation of reference substance solution: with 2- methyl -4,6- methyl dihydroxy benzoate and/or 2,4- dihydroxy-benzoic acid first
Ester is reference substance, is configured to the reference substance solution of suitable concentration；
(3) content assaying method: using ultraviolet-visible spectrophotometry, and ultraviolet specrophotometer is distinguished at 260nm-265nm
Test solution and control solution absorbance is measured, benzoic acid Protoilludane sesquiterpenoid ester in sample is calculated using external standard method
Derivative active component content, and provided with molar concentration.
2. the content assaying method of benzoic acid Protoilludane sesquiterpenoid ester derivant active component as described in claim 1 exists
Purposes in the control of halimasch and products thereof quality and activity guarantee.
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