CN110412199A - A kind of quality determining method of Rhizoma Chuanxiong toothpaste - Google Patents
A kind of quality determining method of Rhizoma Chuanxiong toothpaste Download PDFInfo
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- CN110412199A CN110412199A CN201910651022.7A CN201910651022A CN110412199A CN 110412199 A CN110412199 A CN 110412199A CN 201910651022 A CN201910651022 A CN 201910651022A CN 110412199 A CN110412199 A CN 110412199A
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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
- G01N30/90—Plate chromatography, e.g. thin layer or paper chromatography
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Abstract
The present invention provides a kind of quality determining methods of Rhizoma Chuanxiong toothpaste, it is the toothpaste active ingredient by sodium chloride solution and extracted by ether, are dissolved in ethyl acetate as test solution, identify Rhizoma Chuanxiong toothpaste using thin-layered chromatography；The toothpaste active ingredient extracted with sodium chloride solution and water-saturated n-butanol, is dissolved in 70% methanol as test solution, using ferulaic acid content in high effective liquid chromatography for measuring toothpaste.Quality determining method of the invention, with specific toothpaste sample processing method, the active constituent in toothpaste has effectively been extracted, while having eliminated interference component when detection, realize the accurate identification of Rhizoma Chuanxiong toothpaste, and the quantitative detection of effective component, the method for the present invention is easy, reproducible, as a result reliable, practical method is provided for the quality control of Rhizoma Chuanxiong toothpaste, guarantee is provided for Product Safety and validity, has a good application prospect.
Description
Technical field
Present invention relates particularly to a kind of quality determining methods of Rhizoma Chuanxiong toothpaste.
Background technique
Bleeding gums are common one of the symptoms of the department of stomatology, and " bleeding gums " are medically divided into passivity bleeding and active
Property two class of bleeding, bleeding gums are more common in periodontitis and gingivitis patients；It may be decrease of platelet, but be sometimes also likely to be certain
The oral appearance of a little systemic diseases.And gingivitis, periodontitis morbidity in, local factor especially bacterium, plaque have
Important function.Therefore, oral hygiene is carried out, inhibiting oral bacteria to breed is the important means for preventing bleeding gums and periodontitis.
Rhizoma Chuanxiong Chuanxiong Rhizoma is the dry of umbelliferae Rhizoma Chuanxiong Ligusticum chuanxiong Hort.
Dry rhizome, main product is saved in China Sichuan, Yunnan, Guizhou, Guangxi etc., wherein the most famous with Sichuan Pengzhou producing region[4].Rhizoma Chuanxiong
It is pungent, warm, there is the effect of blood-activating and qi-promoting, wind-expelling pain-stopping[5].Shennong's Herbal records Rhizoma Chuanxiong, and " main apoplexy enters brain, has a headache, and trembles with fear
Numbness, muscle contraction emergency, metal-inflicted wound, married woman's blood close s.m.p ", therefore it is the gas medicine in blood that former times people, which calls Rhizoma Chuanxiong,.Rhizoma imperatae is that gramineae plant is white
The dry rhizome of thatch Imperata cylindrica Beauv.var.major (Nees) C.E.Hubb., property is sweet, cold, has cool
The effect of blood hemostasis, clearing heat and promoting fluid, inducing diuresis for treating strangurtia.
Traditional Chinese medicine is the health resources that China shows unique characteristics, and the economic resources having a high potential, with the modernization of Chinese medicine
The propulsion of process, the big health industry of Chinese medicine are quietly formed, and Chinese medicine class cosmetics are exactly one of to represent, and utilize road native drug
The utility strategies of advantage and full industrial chain apply to Rhizoma Chuanxiong in toothpaste research and development, and developing effectively to prevent and inhibit
Bleeding gums, the Rhizoma Chuanxiong toothpaste for mitigating gingivitis, improving swelling and aching of gum, but its quality control standard lags, and cannot be product
Safety and validity provide safeguard.
Summary of the invention
To solve the above problems, the present invention provides a kind of for identifying the configuration method of the sample solution of Rhizoma Chuanxiong toothpaste,
It includes the following steps:
Toothpaste to be measured is taken, is scattered in sodium chloride solution, is stood, add diethyl ether extraction, and filtering, filter residue is cleaned with ether, closes
And filtrate, be evaporated, residue add ethyl acetate to dissolve to get；
The Rhizoma Chuanxiong toothpaste is using Rhizoma Chuanxiong and cogongrass root herb as raw material, after extracted, concentration, drying, in addition daily use chemicals are used
The toothpaste that acceptable auxiliary material is prepared into product.
Further, the concentration of the sodium chloride solution is 0.4g/ml；The quality of the toothpaste to be measured and sodium chloride solution
Volume ratio is 2g:1ml；The time of the standing is 10min；The additional amount of the ether is 5 times of amount v/w toothpaste to be measured；It is described
It is extracted as ultrasonic extraction, extraction time 30min；It is described to be cleaned twice with ether, each 20ml；The addition of the ethyl acetate
Amount is 2ml.
The present invention also provides a kind of for measuring the configuration method of the sample solution of ferulaic acid content in Rhizoma Chuanxiong toothpaste, it
Include the following steps:
Toothpaste to be measured is taken, sodium chloride and water are added, is mixed thoroughly, n-butanol extraction, filtering are saturated with water, filter residue is saturated with water positive fourth
Alcohol cleaning, merging filtrate are evaporated, and 70% methanol is added to dissolve, constant volume, and filtering takes subsequent filtrate to obtain the final product；
Further, the mass volume ratio of the toothpaste to be measured and sodium chloride and water is 10g:2g:5ml；It is described full with water
It is 10 times of amount v/w toothpaste to be measured with the amount that n-butanol extracts；Described to be extracted as ultrasonic extraction, the ultrasonic extraction time is 30min；Institute
It states and is saturated with water n-butanol cleaning twice, each 20ml；It is described to add 70% methanol constant volume to 10ml.
The present invention also provides a kind of identification methods of Rhizoma Chuanxiong toothpaste, it includes the following steps:
A, reference substance solution: taking Levistilide A reference substance, add ethyl acetate to dissolve to get；
B, control medicinal material solution: taking Rhizoma Chuanxiong control medicinal material, and add diethyl ether extraction, and filtration, filtrate is evaporated, and residue adds ethyl acetate
Dissolution, as control medicinal material solution；
C, test solution: the sample solution for being previously used for identification Rhizoma Chuanxiong toothpaste is taken, as test solution；
D, reference substance solution, control medicinal material solution and test solution are drawn, is put respectively in same GF254 lamellae, with
N-hexane-ethyl acetate is solvent, and expansion dries, sets and inspect under ultraviolet lamp.
Further, Levistilide A concentration is 0.1mg/ml in reference substance solution described in step a；The reference substance is molten
Liquid is kept in dark place；And/or the mass volume ratio of Rhizoma Chuanxiong control medicinal material and ether described in step b is 1g:20ml；It is described to be extracted as
Ultrasonic extraction, ultrasonic extraction time are 60min；The additional amount of the ethyl acetate is 2ml.
Further, the amount of absorption reference substance solution, control medicinal material solution and test solution described in step d is respectively 15
μl；The ratio of the n-hexane-ethyl acetate is 3:1；The a length of 254nm of ultraviolet light wave.
The present invention finally provides ferulaic acid content measuring method in a kind of Rhizoma Chuanxiong toothpaste, it includes the following steps:
1) reference substance solution: taking ferulic acid reference substance, add 70% methanol dissolution to get；
2) test solution: the sample solution for being previously used for ferulaic acid content in measurement Rhizoma Chuanxiong toothpaste is taken, as test sample
Solution；
3) reference substance solution is drawn respectively and test solution injects liquid chromatograph, chromatographic peak area is measured, by external standard
Method is with calculated by peak area ferulaic acid content；Chromatographic condition are as follows:
Chromatographic column: using octadecylsilane chemically bonded silica as filler, mobile phase: using methanol as mobile phase A phase, with 1%
Acetum is Mobile phase B phase；Isocratic elution program is A phase: B phase=30:70.
Further, asafoetide acid concentration is 20 μ g/ml in the step 1) reference substance solution.
Further, the step 3) reference substance solution and the amount of test solution drawn is 10ul；The chromatographic condition
The specification of middle chromatographic column be 4.6mm × 250,5 μm, Detection wavelength 321nm, flow velocity 1ml/min, 30 DEG C of column temperature, separating degree
Greater than 1.5, number of theoretical plate is not less than 4000.
Rhizoma Chuanxiong toothpaste quality detection method of the invention is effectively extracted with specific toothpaste sample processing method
Active constituent in toothpaste, while eliminating interference component when detection, realizes the accurate identification of Rhizoma Chuanxiong toothpaste, and effectively at
Point quantitative detection, the method for the present invention is easy, reproducible, as a result reliably, for Rhizoma Chuanxiong toothpaste quality control provide it is practical
Method, provide guarantee for Product Safety and validity, have a good application prospect.
Obviously, above content according to the present invention is not being departed from according to the ordinary technical knowledge and customary means of this field
Under the premise of the above-mentioned basic fundamental thought of the present invention, the modification, replacement or change of other diversified forms can also be made.
The specific embodiment of form by the following examples remakes further specifically above content of the invention
It is bright.But the range that this should not be interpreted as to the above-mentioned theme of the present invention is only limitted to example below.It is all to be based on above content of the present invention
The technology realized all belongs to the scope of the present invention.
Detailed description of the invention
Fig. 1 Rhizoma Chuanxiong toothpaste TLC identifies figure, and (1: Levistilide A reference substance, 2: Rhizoma Chuanxiong control medicinal material, 3: Rhizoma Chuanxiong toothpaste supplies
Test product)
Fig. 2 ferulic acid and toothpaste test sample high-efficient liquid phase chromatogram
Specific embodiment
1, material, reagent and instrument
1.1 material
Rhizoma Chuanxiong toothpaste: four batches, Rhizoma Chuanxiong toothpaste (YG18030801, YG18030802, YG18030803, YG18030804),
From Sichuan green herbal development in science and technology Co., Ltd.
Reference substance: Levistilide A (lot number: wkq18010408, purchased from the limited public affairs of Sichuan Province's dimension gram parasitic animal and plant science and technology
Department), ferulic acid (lot number 110773-201614, be purchased from National Institute for Food and Drugs Control)
Control medicinal material: Rhizoma Chuanxiong control medicinal material (lot number: 120918-201110 is purchased from National Institute for Food and Drugs Control)
1.2 reagent
Methanol is chromatographically pure, remaining reagent is that analysis is pure, is purchased from Chengdu Cologne Chemical Company；Water is ultrapure
Water, from Sichuan green herbal development in science and technology Co., Ltd.
1.3 instrument
Shimadzu LC-20AD high performance liquid chromatograph；ME204E/02, MS205D Μ, XP26 electronic balance (Mei Tele-Tuo Li
Multiple instruments Co., Ltd)；Semi-automatic point sample instrument；Thin-layer chromatography digital imaging system；Cellular type 1810A ultrapure water machine (rubs in Shanghai
Strangle scientific instrument Co., Ltd)；KQ5200DB type ultrasonic cleaner (600W, 40KHz；The limited public affairs of city of Kunshan's ultrasonic instrument
Department).
The identification of 1 Rhizoma Chuanxiong toothpaste thin-layer chromatography (TLC) of embodiment
1) prepared by reference substance solution: taking Levistilide A reference substance, adds ethyl acetate that every l ml is made containing the molten of 0.1mg
Liquid (is set in brown measuring bottle), as reference substance solution；
2) prepared by control medicinal material solution: taking Rhizoma Chuanxiong control medicinal material 1g, add diethyl ether 20ml, ultrasonic 60min, and filtration, filtrate is steamed
Dry, residue adds ethyl acetate 2ml to dissolve, as control medicinal material solution.
3) prepared by test solution: taking sodium chloride 4g, is placed in the triangular flask of 250ml, add water 10ml, shaking is allowed to mixed
It closes, takes 1, toothpaste to be measured, the lotion that lotion discards front 10cm long is squeezed out from dentifrice tube, precision weighs toothpaste 20g, sets
It states in 250ml triangular flask, stirring is allowed to be uniformly dispersed, and places 10min, and 100ml ether is added, and stirring is allowed to disperse, and ultrasound mentions
It takes 30 minutes, is filtered with filter paper, residue is washed twice with ether, each 20ml, and merging filtrate sets water-bath Back stroke in evaporating dish
Dry, residue adds ethyl acetate 2ml to dissolve, as test solution；
4) reference substance solution, 15 μ L of control medicinal material solution and test solution are drawn respectively, are put respectively in same silica gel
GF254On lamellae, with n-hexane-ethyl acetate (3:1) for solvent, it is unfolded, takes out, dry, set ultraviolet lamp (254nm)
Under inspect.Thin-layer chromatogram is shown in Fig. 1.
As seen from Figure 1: in sample chromatogram, on reference substance chromatography corresponding position, showing the spot of same color.With
The spot of 4 same colors is shown in reference medicine chromatography figure.
Ferulaic acid content measures in 2 Rhizoma Chuanxiong toothpaste of embodiment
(1) preparation of reference substance solution: taking ferulic acid reference substance, accurately weighed, sets in brown measuring bottle, adds 70% methanol system
At every 1ml containing 20 μ g solution to get；
(2) preparation of test solution: taking 1, toothpaste to be measured, and lotion is squeezed out from dentifrice tube and discards front 10cm's long
Lotion, precision weigh toothpaste 10g, set in 250ml triangular flask, and sodium chloride 2g is added, and add water 5ml, and shaking makes to mix.Stirring makes point
It dissipates uniformly, adds 100mL water-saturated n-butanol, close plug, weighed weight, ultrasonic extraction 30min filters with filter paper, and residue is full with water
It is rinsed twice with n-butanol, each 20ml, merging filtrate is set and volatilized in water-bath in evaporating dish, and residue is dissolved with 70% methanol
And be transferred in the volumetric flask of 10ml, be settled to scale, filter, take subsequent filtrate to get；
(3) reference substance solution is drawn respectively and test solution injects liquid chromatograph, measure the content of ferulic acid；Chromatography
Condition are as follows: Agilent C18 chromatographic column (4.6mm × 250,5 μm)；With -1% acetum of methanol (30:70) for mobile phase；Inspection
Survey wavelength is 321nm；Volume flow 1ml/min；30 DEG C of column temperature；Sample introduction 10ul.Under above-mentioned chromatographic condition, ferulic acid can be with
Adjacent chromatographic peak reaches baseline separation, and separating degree is greater than 1.5, and number of theoretical plate is not less than 4000.
Reference substance and sample chromatogram figure are shown in Fig. 2.
Beneficial effects of the present invention are further illustrated below by way of the mode of test example:
Test example 1
1, ferulaic acid content method is linearly investigated in Rhizoma Chuanxiong toothpaste
(1) preparation of reference substance solution: taking ferulic acid reference substance, accurately weighed, sets in brown measuring bottle, adds 70% methanol system
At every 1ml containing 20 μ g solution to get；
(2) 1,2,5,10,15,20,25 μ L of reference substance solution is drawn respectively, distinguishes sample introduction by chromatographic condition in embodiment 2,
Using peak area as ordinate, to compare quality (μ g) as abscissa, standard curve is drawn.Acquiring regression equation is Y=
5205704.2334x-2875.4195(R2=1.0000), the results showed that ferulic acid is linear in 0.0193~0.4817 μ g/ml
Well.
2, ferulaic acid content method precision is investigated in Rhizoma Chuanxiong toothpaste
(1) preparation of reference substance solution: taking ferulic acid reference substance, accurately weighed, sets in brown measuring bottle, adds 70% methanol system
At every 1ml containing 20 μ g solution to get；
(2) accurate to draw 10 μ L of ferulic acid reference substance solution, by chromatographic condition in embodiment 2, continuous sample introduction 6 times, record
And chromatogram is analyzed, measurement peak area RSD value is 0.39%, shows that instrument precision is good.
3, ferulaic acid content method study on the stability in Rhizoma Chuanxiong toothpaste
(1) preparation of test solution: taking 1, toothpaste to be measured, and lotion is squeezed out from dentifrice tube and discards front 10cm's long
Lotion, precision weigh toothpaste 10g, set in 250ml triangular flask, and sodium chloride 2g is added, and add water 5ml, and shaking makes to mix.Stirring makes point
It dissipates uniformly, adds 100mL water-saturated n-butanol, close plug, weighed weight, ultrasonic extraction 30min filters with filter paper, and residue is full with water
It is rinsed twice with n-butanol, each 20ml, merging filtrate is set and volatilized in water-bath in evaporating dish, and residue is dissolved with 70% methanol
And be transferred in the volumetric flask of 10ml, be settled to scale, filter, take subsequent filtrate to get；
(2) accurate respectively to draw 10 μ L of test solution, in 0,2,4,8,12, for 24 hours, respectively by chromatostrip in embodiment 2
Part sample introduction records chromatographic peak area.The RSD value of ferulic acid component content is 0.52% in stability test, shows that test sample is molten
Liquid has good stability in interior for 24 hours.
4, ferulaic acid content method repeatability is investigated in Rhizoma Chuanxiong toothpaste
(1) it the preparation of test solution: takes with a collection of 6, toothpaste, every is pressed toothpaste content preparation method of test article respectively
Sample preparation, i.e., squeeze out the lotion that lotion discards front 10cm long from dentifrice tube, and precision weighs toothpaste 10g, sets 250ml triangular flask
In, sodium chloride 2g is added, adds water 5ml, shaking makes to mix.Stirring makes to be uniformly dispersed, and adds 100mL water-saturated n-butanol, and close plug claims
Determine weight, ultrasonic extraction 30min is filtered with filter paper, and residue is saturated with water n-butanol and rinses twice, each 20ml, merging filtrate
In evaporating dish, to set and volatilized in water-bath, residue is dissolved and is transferred in the volumetric flask of 10ml with 70% methanol, it is settled to scale,
Filtration, take subsequent filtrate to get；
(2) accurate to draw each 10 μ L of 6 parts of test solutions, respectively by chromatographic condition sample introduction in embodiment 2, record chromatographic peak
Area.The RSD value of ferulic acid component content is 1.03% in repetitive test, shows that the repeatability of this method is good.
5, the recycling of ferulaic acid content method sample-adding is investigated in Rhizoma Chuanxiong toothpaste
(1) preparation of test solution: precision weighs 6 parts of the consistent toothpaste of ingredient amount, and every part of 5g is placed in 250ml's
In stuffed conical flask, sodium chloride 1g being added, adds water 2.5ml, shakes, stirring makes to be uniformly dispersed, add 100mL water-saturated n-butanol,
Stirring makes to disperse, and close plug, ultrasonic extraction 30min is filtered with filter paper, and residue is saturated with water n-butanol and rinses twice, each 20ml,
Merging filtrate is set and is volatilized in water-bath in evaporating dish, the ferulic acid reference substance 2ml of 0.034mg/ml is separately added into, with 70% first
Alcohol is settled to 10ml, filtration, take subsequent filtrate to get.
(2) accurate to draw each 10 μ L of 6 parts of test solutions, respectively by chromatographic condition sample introduction in embodiment 2, record chromatographic peak
Area.Measuring average recovery rate is 100.20%, and the RSD value of ferulaic acid content is 0.57% in test sample.
To sum up: the TLC discrimination test of Rhizoma Chuanxiong is shown in Rhizoma Chuanxiong toothpaste, as a result clear spot, is had operability, be can be used as
The qualitative identification method of Rhizoma Chuanxiong toothpaste；It is measured using content of the HPLC method to ferulic acid in Rhizoma Chuanxiong toothpaste, result precision
Height, method are easy, reproducible.The method of the present invention can effectively control the quality of Rhizoma Chuanxiong toothpaste, for Product Safety and effectively
Property provides safeguard.
Claims (10)
1. a kind of for identifying the configuration method of the sample solution of Rhizoma Chuanxiong toothpaste, it is characterised in that: it includes the following steps:
Toothpaste to be measured is taken, is scattered in sodium chloride solution, is stood, add diethyl ether extraction, and filtering, filter residue is cleaned with ether, merges filter
Liquid is evaporated, residue add ethyl acetate to dissolve to get；
The Rhizoma Chuanxiong toothpaste is using Rhizoma Chuanxiong and cogongrass root herb as raw material, after extracted, concentration, drying, in addition in daily chemical product
The toothpaste that acceptable auxiliary material is prepared into.
2. configuration method according to claim 1, which is characterized in that the concentration of the sodium chloride solution is 0.4g/ml；Institute
The mass volume ratio for stating toothpaste and sodium chloride solution to be measured is 2g:1ml；The time of the standing is 10min；The ether adds
Entering amount is 5 times of amount v/w toothpaste to be measured；It is described to be extracted as ultrasonic extraction, extraction time 30min；It is described to be cleaned twice with ether,
Each 20ml；The additional amount of the ethyl acetate is 2ml.
3. a kind of for measuring the configuration method of the sample solution of ferulaic acid content in Rhizoma Chuanxiong toothpaste, it is characterised in that: it includes
Following steps:
Toothpaste to be measured is taken, sodium chloride and water are added, is mixed thoroughly, is saturated with water n-butanol extraction, filtering, it is clear that filter residue is saturated with water n-butanol
It washes, merging filtrate is evaporated, and 70% methanol is added to dissolve, and constant volume, filtering takes subsequent filtrate to obtain the final product.
4. configuration method according to claim 3, which is characterized in that the mass body of the toothpaste to be measured and sodium chloride and water
Product is than being 10g:2g:5ml；The amount for being saturated with water n-butanol extraction is 10 times of amount v/w toothpaste to be measured；It is described to be extracted as ultrasound
It extracts, the ultrasonic extraction time is 30min；It is described to be saturated with water n-butanol cleaning twice, each 20ml；Described plus 70% methanol is fixed
Hold to 10ml.
5. a kind of identification method of Rhizoma Chuanxiong toothpaste, which is characterized in that it includes the following steps:
A, reference substance solution: taking Levistilide A reference substance, add ethyl acetate to dissolve to get；
B, control medicinal material solution: taking Rhizoma Chuanxiong control medicinal material, and add diethyl ether extraction, and filtration, filtrate is evaporated, and residue adds ethyl acetate molten
Solution, as control medicinal material solution；
C, test solution: claim 1 gained sample solution is taken, as test solution；
D, reference substance solution, control medicinal material solution and test solution are drawn, is put respectively in same GF254Lamellae, with just oneself
Alkane-ethyl acetate is solvent, and expansion dries, sets and inspect under ultraviolet lamp.
6. identification method according to claim 5, which is characterized in that Levistilide A in reference substance solution described in step a
Concentration is 0.1mg/ml；The reference substance solution is kept in dark place；And/or the quality of Rhizoma Chuanxiong control medicinal material and ether described in step b
Volume ratio is 1g:20ml；Described to be extracted as ultrasonic extraction, the ultrasonic extraction time is 60min；The additional amount of the ethyl acetate is
2ml。
7. identification method according to claim 5, which is characterized in that draw reference substance solution, control medicinal material described in step d
The amount of solution and test solution is respectively 15 μ l；The ratio of the n-hexane-ethyl acetate is 3:1；The ultraviolet wavelength
For 254nm.
8. ferulaic acid content measuring method in a kind of Rhizoma Chuanxiong toothpaste, it is characterised in that: it includes the following steps:
1) reference substance solution: taking ferulic acid reference substance, add 70% methanol dissolution to get；
2) test solution: claim 3 gained sample solution is taken, as test solution；
3) reference substance solution and test solution are drawn respectively and inject liquid chromatograph, measure chromatographic peak area, by external standard method with
Calculated by peak area ferulaic acid content；Chromatographic condition are as follows:
Chromatographic column: using octadecylsilane chemically bonded silica as filler, mobile phase: using methanol as mobile phase A phase, with 1% acetic acid
Solution is Mobile phase B phase；Isocratic elution program is A phase: B phase=30:70.
9. measuring method according to claim 8, it is characterised in that: asafoetide acid concentration in the step 1) reference substance solution
For 20 μ g/ml.
10. measuring method according to claim 8, it is characterised in that: step 3) the absorption reference substance solution and for examination
The amount of product solution is 10ul；In the chromatographic condition specification of chromatographic column be 4.6mm × 250,5 μm, Detection wavelength 321nm,
Flow velocity is 1ml/min, and 30 DEG C of column temperature, separating degree is greater than 1.5, and number of theoretical plate is not less than 4000.
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