CN106198836A - Clearing brain tablet method of quality control - Google Patents

Clearing brain tablet method of quality control Download PDF

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Publication number
CN106198836A
CN106198836A CN201610483062.1A CN201610483062A CN106198836A CN 106198836 A CN106198836 A CN 106198836A CN 201610483062 A CN201610483062 A CN 201610483062A CN 106198836 A CN106198836 A CN 106198836A
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China
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solution
radix angelicae
quality control
rhizoma chuanxiong
take
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谢国旗
郝少君
苏峰
王希东
马珍珍
李文俊
张正臣
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No371 Hospital Of Pla
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No371 Hospital Of Pla
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/90Plate chromatography, e.g. thin layer or paper chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Biological Materials (AREA)

Abstract

The invention discloses a kind of clearing brain tablet method of quality control, differentiate and Rhizoma Chuanxiong discriminating including utilizing thin layer chromatography to carry out the Radix Angelicae Dahuricae;High performance liquid chromatography is utilized to carry out ferulaic acid content mensuration.The clearing brain tablet method of quality control of the present invention, provide the Radix Angelicae Dahuricae and the method for Rhizoma Chuanxiong in discriminating medicine, and use main flavour of a drug Rhizoma Chuanxiong and Radix Angelicae Sinensis in high-efficient liquid phase technique the other side to carry out assay with ferulic acid for index, this method of quality control can better control over the quality of medicine, having stronger specificity and good repeatability, real embodiment drug safety is effective, quality controllable.

Description

Clearing brain tablet method of quality control
Technical field
The invention belongs to technical field of pharmaceuticals, specifically, relate to a kind of clearing brain tablet method of quality control.
Background technology
Headache, because of multiterminal, is careless by daily life, and sitting and lying works as wind, is affected by the cold damp and hot caused.Nothing more than Exogenous and internal injuries two Big class.Treatment is preferably invigorated blood circulation sensible, the clear profit head.Have a headache after cerebral concussion the most common.Modern medicine thinks that it occurs Substantial connection is had with factors such as increased intracranial pressure, blood-brain barrier disruption, microcirculation dysfunctions." Ling Shu Miraculous Pivot or Divine Axis sea opinion " is said: " the brain being the reservoir of the marrow ".Li Shizhen (1518-1593 A.D.) is said: " the brain being the house of mentality ".After craniocerebral injury venation is impaired, and QI and blood is inverse disorderly, blockage of main and collateral channels, gas Stagnant blood stasis, adds terrified worry etc. and causes depression of liver-QI, catharsis dereliction of duty etc. to form the clinical manifestation based on qi depression to blood stasis.
The Radix Angelicae Dahuricae in clearing brain tablet side, pungent, warm, there is the scattered wind that induces sweat, the effect of sensible pain relieving, for monarch drug.Radix Angelicae Sinensis, pungent, warm, return Liver, heart spleen channel, have enrich blood, invigorate blood circulation, the effect of pain relieving.Rhizoma Chuanxiong, pungent, warm, there is effect of blood-activating and qi-promoting, wind-expelling pain-stopping.Hook Rattan, nature and flavor are sweet, be slightly cold, and have endogenous wind stopping relieving convulsion, effect of heat clearing away suppressing the hyperactive liver.Herba Asari, nature and flavor are pungent, warm, have expelling wind and cold, sensible only Effect of pain.Four medicines share as ministerial drug.Os Draconis, nature and flavor are sweet, puckery, flat, and GUIXIN, liver, kidney channel have tranquillizing the mind by relieving convulsion, suppressing the hyperactive liver and subsiding YANG, Restrain astringent or styptic treatment for spontaneous sweating effect, for adjuvant drug.Herba Menthae, nature and flavor are pungent, cool, have dispelling wind and heat pathogens, and effect of the clear profit head, for making medicine.Above Seven medicines share, have invigorate blood circulation, circulation of qi promoting, sensible pain relieving, the effect of the clear profit head.Lose after treating headache, dizziness, cerebral concussion Disease.By clinical observation, clearing brain tablet curative effect in clinical practice is better than somedon, is worthy of popularization.
For ensureing the stability of preparation and curative effect, clearing brain tablet is formulated comprehensive quality standard, Rhizoma Chuanxiong and clear when be classified as Main flavour of a drug in brain sheet, this law uses Rhizoma Chuanxiong and Radix Angelicae Sinensis in high-efficient liquid phase technique the other side to carry out assay with ferulic acid for index, With thin layer chromatography respectively to the Radix Angelicae Dahuricae and Rhizoma Chuanxiong qualitative identification.Preparation has been carried out long-term stable experiment, and result shows at 24 In month, the quality of preparation is without significantly change, provides strong evidence for formulating the effect duration of preparation.
Summary of the invention
In view of this, an object of the present invention is to provide the method for quality control of a kind of clearing brain tablet, and the method can be fast The Radix Angelicae Dahuricae in speed, accurately discriminating health kidney oral liquid and Rhizoma Chuanxiong, and by ferulic acid in high effective liquid chromatography for measuring clearing brain tablet Content.
The invention discloses a kind of clearing brain tablet method of quality control, carry out Radix Angelicae Dahuricae discriminating and river including utilizing thin layer chromatography Rhizome of chuanxiong differentiates;High performance liquid chromatography is utilized to carry out ferulaic acid content mensuration.
Further, described Radix Angelicae Dahuricae discrimination method is: take clearing brain tablet 10, removes coating, finely ground one-tenth powder, adds diethyl ether 20ml shakes, and places 1 hour, filters, and filtrate volatilizes, and residue adds ethyl acetate 1ml makes dissolving, as need testing solution;
Take Radix Angelicae Dahuricae control medicinal material and be made in the same way of control medicinal material solution;
Take the negative sample without the Radix Angelicae Dahuricae and be made in the same way of negative control solution;
Take imperatorin reference substance, accurately weighed, add ethyl acetate and make every 1ml solution containing 1mg, molten as reference substance Liquid;
Test according to thin layer chromatography, draw each 4 μ l of above-mentioned four kinds of solution, put respectively and in same with sodium carboxymethyl cellulose be On the silica gel g thin-layer plate of adhesive, with petroleum ether-ether (3:2) as developing solvent, launch below 25 DEG C, take out, dry;
Observe silica gel g thin-layer plate, inspect under ultra-violet lamp 365nm, in test sample chromatograph, corresponding with reference substance chromatograph On position, the fluorescence speckle of aobvious same color.
Further, described petroleum ether boiling range is 30-60 DEG C.
Further, described Rhizoma Chuanxiong discrimination method is: take clearing brain tablet 10, removes coating, finely ground one-tenth powder, adds diethyl ether 50ml, supersound process 20 minutes, filter, filtrate volatilizes, and residue adds chloroform 1ml makes dissolving, as need testing solution;
Taking Rhizoma Chuanxiong control medicinal material 1g, add diethyl ether 20ml, is made in the same way of control medicinal material solution;
Take the negative sample without Rhizoma Chuanxiong and be made in the same way of negative control solution;
Test according to thin layer chromatography, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with body Long-pending is developing solvent than the normal hexane-ethyl acetate for 9:1, launches, takes out, dry;
Observe silica gel g thin-layer plate, inspect under ultra-violet lamp 365nm, in test sample chromatograph, corresponding to control medicinal material chromatograph Position on, the fluorescence speckle of aobvious same color.
Further, described ferulaic acid content assay method is:
Chromatographic condition and system suitability, with octadecylsilane chemically bonded silica as filler;With volume ratio 17:83 It is flowing phase for acetonitrile-0.085% phosphoric acid solution;Detection wavelength is 320nm, number of theoretical plate press ferulic acid peak calculate should >= 1500;
The preparation of reference substance solution, precision weighs ferulic acid reference substance, puts in brown measuring bottle, adds methanol and makes every 1ml containing 5 The solution of μ g, to obtain final product;
The preparation of need testing solution, takes clearing brain tablet 10, removes coating, finely ground one-tenth powder, takes described powder 1g, accurate title Fixed, put in tool plug conical flask, accurate addition methanol 15ml, close plug, weighed weight, supersound process, let cool, more weighed weight, add Methanol supplies the weight of less loss, shakes up, and filters, takes subsequent filtrate, to obtain final product;
Assay method: precision draws reference substance solution and each 20 μ l of need testing solution respectively, injects chromatograph of liquid, surveys Fixed, calculate and get final product, this product every in terms of ferulic acid, must not be less than 0.010mg containing Radix Angelicae Sinensis, Rhizoma Chuanxiong.
Further, in described ferulaic acid content assay method, the sonification power of need testing solution preparation process is 160W, supersonic frequency is 50kHz, ultrasonic time 60 minutes.
Compared with prior art, the present invention can obtain and include techniques below effect:
1) the clearing brain tablet method of quality control of the present invention, it is provided that differentiate the Radix Angelicae Dahuricae and the method for Rhizoma Chuanxiong in medicine, and use In high-efficient liquid phase technique the other side, main flavour of a drug Rhizoma Chuanxiong and Radix Angelicae Sinensis carry out assay with ferulic acid for index.
2) method of quality control of the present invention can better control over the quality of medicine, has stronger specificity and good Repeatability, real embodiment drug safety is effective, quality controllable.
Certainly, the arbitrary product implementing the present invention must be not necessarily required to reach all the above technique effect simultaneously.
Accompanying drawing explanation
Accompanying drawing described herein is used for providing a further understanding of the present invention, constitutes the part of the present invention, this Bright schematic description and description is used for explaining the present invention, is not intended that inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 show the Radix Angelicae Dahuricae of clearing brain tablet method of quality control of the present invention and differentiates thin-layer chromatogram (uviol lamp 365nm);
Fig. 2 show the Rhizoma Chuanxiong of clearing brain tablet method of quality control of the present invention and differentiates thin-layer chromatogram (uviol lamp 365nm);
Fig. 3 show the ferulaic acid content of clearing brain tablet method of quality control of the present invention and measures reference substance high performance liquid chromatography Figure;
Fig. 4 show the ferulaic acid content of clearing brain tablet method of quality control of the present invention and measures test sample high performance liquid chromatography Figure;
Fig. 5 show the ferulaic acid content of clearing brain tablet method of quality control of the present invention and measures negative control high performance liquid chromatography Figure.
Detailed description of the invention
Describe embodiments of the present invention in detail below in conjunction with drawings and Examples, thereby how the present invention is applied Technological means solves technical problem and reaches the process that realizes of technology effect and can fully understand and implement according to this.
Embodiment 1, the discriminating of the Radix Angelicae Dahuricae
Taking clearing brain tablet 10, remove coating, finely ground, the 20ml that adds diethyl ether shakes, and places 1 hour, filters, and filtrate volatilizes, residual Slag adds ethyl acetate 1ml makes dissolving, as need testing solution.
Take Radix Angelicae Dahuricae control medicinal material and be made in the same way of control medicinal material solution.
Take the negative sample without the Radix Angelicae Dahuricae and be made in the same way of negative control solution.
Take imperatorin reference substance, accurately weighed, add ethyl acetate and make every 1ml solution containing 1mg, molten as reference substance Liquid.
Test according to thin layer chromatography, draw each 4 μ l of above-mentioned four kinds of solution, put respectively and in same with sodium carboxymethyl cellulose be On the silica gel g thin-layer plate of adhesive, with petroleum ether (30-60 DEG C)-ether (3:2) as developing solvent, launch below 25 DEG C, take Go out, dry, put and inspect under ultra-violet lamp 365nm.
The Radix Angelicae Dahuricae of result such as Fig. 1 clearing brain tablet of the present invention method of quality control differentiates thin-layer chromatogram (uviol lamp 365nm) institute Showing, in figure, 1 is imperatorin reference substance, and 2 is Radix Angelicae Dahuricae control medicinal material, and 3-5 is test sample, and 6 is negative control.Test sample color in figure In spectrum, on position corresponding with reference substance chromatograph, the fluorescence speckle of aobvious same color.In negative control sample chromatograph, with On reference substance chromatograph relevant position, have no corresponding speckle.Show in clearing brain tablet containing the Radix Angelicae Dahuricae.
Embodiment 2, the discriminating of Rhizoma Chuanxiong
Taking clearing brain tablet 10, remove coating, finely ground, add diethyl ether 50ml, supersound process 20 minutes, filters, and filtrate volatilizes, residual Slag adds chloroform 1ml makes dissolving, as need testing solution.
Taking Rhizoma Chuanxiong control medicinal material 1g, add diethyl ether 20ml, is made in the same way of control medicinal material solution.
Take the negative sample without Rhizoma Chuanxiong and be made in the same way of negative control solution.
Test according to thin layer chromatography, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with body Long-pending is developing solvent than the normal hexane-ethyl acetate for 9:1, launches, takes out, dry, put and inspect under ultra-violet lamp 365nm.
The Rhizoma Chuanxiong of result such as Fig. 2 clearing brain tablet of the present invention method of quality control differentiates thin-layer chromatogram (uviol lamp 365nm) institute Showing, in figure, 1 is Rhizoma Chuanxiong control medicinal material, and 2-4 is test sample, and 5 is negative control.In figure in test sample chromatograph, with reference substance color Compose on corresponding position, the fluorescence speckle of aobvious same color.In negative control sample chromatograph, with reference substance chromatograph relevant position On, have no corresponding speckle.Show in clearing brain tablet containing Rhizoma Chuanxiong.
Embodiment 3, the assay of ferulic acid
(1) method of assay
Rhizoma Chuanxiong and when be classified as in clearing brain tablet main flavour of a drug, this law uses in high-efficient liquid phase technique the other side Rhizoma Chuanxiong and Radix Angelicae Sinensis with Resina Ferulae Acid carries out assay for index.
Chromatographic condition and system suitability: with octadecylsilane chemically bonded silica as filler;With acetonitrile- 0.085% phosphoric acid solution=17:83 is flowing phase;Detection wavelength is 320nm.Number of theoretical plate is calculated should be not less than by ferulic acid peak 1500。
The preparation of reference substance solution: take ferulic acid reference substance appropriate, accurately weighed, put in brown measuring bottle, add methanol and make Every 1ml solution containing 5 μ g, to obtain final product.
The preparation of need testing solution: take clearing brain tablet 10, removes coating, finely ground, takes 1g, accurately weighed, puts tool plug taper In Ping, accurate addition methanol 15ml, close plug, weighed weight, supersound process (power 160W, frequency 50kHz) 60 minutes, let cool, The most weighed weight, supplies the weight of less loss, shakes up with methanol, filters, takes subsequent filtrate, to obtain final product.
The preparation of negative control solution: take the negative sample without Rhizoma Chuanxiong and Radix Angelicae Sinensis, according to the preparation method of need testing solution, Prepare with method.
Algoscopy: precision measures need testing solution and each 20 μ l of ferulic acid reference substance inject chromatograph of liquid, records chromatograph Figure, goes out the content of ferulic acid in test sample by external standard method with calculated by peak area, to obtain final product.
(2) methodological study of assay
The determination of 2.1 detection wavelength
With acetonitrile-0.085% phosphoric acid solution=17:83 as solvent, to ferulic acid standard substance in the range of 220-350nm Being scanned, ferulic acid standard substance, in this solvent, have absorption maximum at 320nm.
2.2 system suitability
Under above-mentioned chromatographic condition, take reference substance solution, need testing solution and negative control solution, each sampling volume respectively 20 μ l, record chromatogram.Measurement result is as in Figure 3-5.In sample, ferulic acid theoretical cam curve calculates: n=5820 (> 1500);Main peak is 0.98 with the separating degree of impurity peaks;Negative control solution without absorbing, shows adjuvant at reference substance absworption peak And various catabolite is less to main peak interference, meet the requirement of system suitability.
2.3 linear relationship tests
Take ferulic acid reference substance 2.70mg, put in 50ml measuring bottle, add flowing and make dissolving mutually and be diluted to scale, shake up, essence Close measure 1,2,4,5,10ml, put in 50ml measuring bottle, add flowing phase dilution to scale, shake up.Precision measures each 20 μ l, notes respectively Enter chromatograph of liquid, measure peak area.With peak area (X), sample introduction concentration (C, μ g/ml) being carried out linear regression, regression equation is Y=53551x+7970.7 coefficient R2=0.9991, result shows, ferulic acid concentration in the range of 1.08~54 μ g/ml, Peak area is good with concentration linear relationship, is shown in Table 1.
Table 1 ferulic acid linear relationship result of the test
Sequence number 1 2 3 4 5 6
Concentration (X, μ g/ml) 1.08 2.16 4.32 5.40 10.80 54.00
Peak area (Y) 72819 121736 238512 288532 590631 2955633
2.4 minimum detectable activity
No. 1 solution under line taking sexual relationship test item, precision measures 2ml, puts in 10ml measuring bottle, adds flowing phase dilution to carving Degree, shakes up, and precision measures 20 μ l, is injected separately into chromatograph of liquid, measures, in chromatogram, and signal to noise ratio > 10:1, so minimum inspection Output < 0.2 μ g/ml.
2.5 precision test
Taking No. 2 reference substance solution, precision measures 20 μ l, METHOD FOR CONTINUOUS DETERMINATION 6 times, the results are shown in Table 2.Meansigma methods is 123220, RSD It is 4.3%.This law precision is good.
Table 2 Precision test result
Sequence number 1 2 3 4 5 6
Peak area 121736 117085 130638 118855 122781 128225
2.6 stability test
Take clearing brain tablet 10, be prepared into need testing solution by method below assay item;Accurate absorption need testing solution 20 μ L, sample introduction measures once at regular intervals, measures 8 hours altogether, the results are shown in Table 3.RSD is 3.4%, and result shows, test sample is molten Liquid is basicly stable in 8 hours.
Table 3 stability test result
Sequence number 1 2 3 4
Peak area 234334 235623 245698 222489
Sequence number 5 6 7 8
Peak area 229638 248612 230237 256864
The clearing brain tablet method of quality control of the present invention, it is provided that differentiate the Radix Angelicae Dahuricae and the method for Rhizoma Chuanxiong in medicine, and use height In effect liquid phase method the other side, main flavour of a drug Rhizoma Chuanxiong and Radix Angelicae Sinensis carry out assay with ferulic acid for index, and this method of quality control can be more Controlling well the quality of medicine, have stronger specificity and good repeatability, real embodiment drug safety is effectively, quality can Control.
As employed some vocabulary in the middle of description and claim to censure special component or method.Art technology Personnel are it is to be appreciated that same composition may be called with different nouns in different regions.This specification and claims are not In the way of the difference of title is used as distinguishing composition." comprising " as mentioned by the middle of description and claim in the whole text is One open language, therefore " comprise but be not limited to " should be construed to." substantially " refer in receivable range of error, this area Technical staff can solve described technical problem in the range of certain error, basically reaches described technique effect.Description is follow-up It is described as implementing the better embodiment of the present invention, for the purpose of right described description is the rule so that the present invention to be described, not In order to limit the scope of the present invention.Protection scope of the present invention is when being as the criterion depending on the defined person of claims.
Also, it should be noted term " includes ", " comprising " or its any other variant are intended to nonexcludability Comprise, so that include that the commodity of a series of key element or system not only include those key elements, but also include the most clearly Other key elements listed, or also include the key element intrinsic for this commodity or system.In the feelings not having more restriction Under condition, statement " including ... " key element limited, it is not excluded that in the commodity including described key element or system There is also other identical element.
Described above illustrate and describes some preferred embodiments of the present invention, but as previously mentioned, it should be understood that the present invention Be not limited to form disclosed herein, be not to be taken as the eliminating to other embodiments, and can be used for other combinations various, Amendment and environment, and can be in invention contemplated scope described herein, by above-mentioned teaching or the technology of association area or knowledge It is modified.And the change that those skilled in the art are carried out and change are without departing from the spirit and scope of the present invention, the most all should be at this In the protection domain of bright claims.

Claims (6)

1. clearing brain tablet method of quality control, it is characterised in that include that utilizing thin layer chromatography to carry out the Radix Angelicae Dahuricae differentiates and Rhizoma Chuanxiong discriminating; High performance liquid chromatography is utilized to carry out ferulaic acid content mensuration.
2. clearing brain tablet method of quality control as claimed in claim 1, it is characterised in that described Radix Angelicae Dahuricae discrimination method is: take clear Brain sheet 10, removes coating, finely ground one-tenth powder, and the 20ml that adds diethyl ether shakes, places 1 hour, filters, and filtrate volatilizes, and residue adds second Acetoacetic ester 1ml makes dissolving, as need testing solution;
Take Radix Angelicae Dahuricae control medicinal material and be made in the same way of control medicinal material solution;
Take the negative sample without the Radix Angelicae Dahuricae and be made in the same way of negative control solution;
Take imperatorin reference substance, add ethyl acetate and make every 1ml solution containing 1mg, as reference substance solution;
Test according to thin layer chromatography, draw each 4 μ l of above-mentioned four kinds of solution, put respectively in same with sodium carboxymethyl cellulose for binding On the silica gel g thin-layer plate of agent, the petroleum ether-ether with volume ratio as 3:2, as developing solvent, launches below 25 DEG C, takes out, dries in the air Dry;
Observe described silica gel g thin-layer plate, inspect under ultra-violet lamp 365nm, in test sample chromatograph, corresponding with reference substance chromatograph On position, the fluorescence speckle of aobvious same color.
3. clearing brain tablet method of quality control as claimed in claim 2, it is characterised in that described petroleum ether boiling range is 30-60 DEG C.
4. clearing brain tablet method of quality control as claimed in claim 1, it is characterised in that described Rhizoma Chuanxiong discrimination method is: take clear Brain sheet 10, removes coating, finely ground one-tenth powder, and add diethyl ether 50ml, supersound process 20 minutes, filters, and filtrate volatilizes, and residue adds three Chloromethanes 1ml makes dissolving, as need testing solution;
Taking Rhizoma Chuanxiong control medicinal material 1g, add diethyl ether 20ml, is made in the same way of control medicinal material solution;
Take the negative sample without Rhizoma Chuanxiong and be made in the same way of negative control solution;
Test according to thin layer chromatography, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with volume ratio Normal hexane-ethyl acetate for 9:1 is developing solvent, launches, and takes out, dries;
Observe described silica gel g thin-layer plate, inspect under ultra-violet lamp 365nm, in test sample chromatograph, corresponding to control medicinal material chromatograph Position on, the fluorescence speckle of aobvious same color.
5. clearing brain tablet method of quality control as claimed in claim 1, it is characterised in that described ferulaic acid content assay method For:
Chromatographic condition and system suitability: with octadecylsilane chemically bonded silica as filler;With volume ratio 17:83 as second Nitrile-0.085% phosphoric acid solution is flowing phase;Detection wavelength is 320nm, and number of theoretical plate is pressed ferulic acid peak and calculated >=1500;
The preparation of reference substance solution: precision weighs ferulic acid reference substance, puts in brown measuring bottle, adds methanol and makes every 1ml containing 5 μ g's Solution, to obtain final product;
The preparation of need testing solution: take clearing brain tablet 10, removes coating, finely ground one-tenth powder, takes described powder 1g, accurately weighed, Put in tool plug conical flask, accurate addition methanol 15ml, close plug, weighed weight, supersound process, let cool, more weighed weight, add methanol Supply the weight of less loss, shake up, filter, take subsequent filtrate, to obtain final product;
Assay method: precision draws reference substance solution and each 20 μ l of need testing solution respectively, injects chromatograph of liquid, measures, meter Calculating and get final product, this product every in terms of ferulic acid, must not be less than 0.010mg containing Radix Angelicae Sinensis, Rhizoma Chuanxiong.
6. clearing brain tablet method of quality control as claimed in claim 5, it is characterised in that described ferulaic acid content assay method In, the sonification power of need testing solution preparation process is 160W, and supersonic frequency is 50kHz, ultrasonic time 60 minutes.
CN201610483062.1A 2016-06-24 2016-06-24 Clearing brain tablet method of quality control Pending CN106198836A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101254284A (en) * 2007-02-26 2008-09-03 北京亚东生物制药有限公司 Rheumatism treating medicine combination, preparation and quality control method
CN102100818A (en) * 2009-12-16 2011-06-22 天津中新药业集团股份有限公司隆顺榕制药厂 Quality control method for lophanthus antifebrile tablets
CN103630614A (en) * 2012-08-22 2014-03-12 天士力制药集团股份有限公司 High performance liquid chromatography detection method of Yangxueqingnao granule

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101254284A (en) * 2007-02-26 2008-09-03 北京亚东生物制药有限公司 Rheumatism treating medicine combination, preparation and quality control method
CN102100818A (en) * 2009-12-16 2011-06-22 天津中新药业集团股份有限公司隆顺榕制药厂 Quality control method for lophanthus antifebrile tablets
CN103630614A (en) * 2012-08-22 2014-03-12 天士力制药集团股份有限公司 High performance liquid chromatography detection method of Yangxueqingnao granule

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
刘纪青 等: "蛇毒清丸的质量标准研究初探", 《河北中医药学报》 *
成培光 等: "冠心通胶囊质量控制", 《中国医院药学杂志》 *
范莉莉 等: "清脑片中阿魏酸的HPLC含量测定方法", 《河南中医》 *

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