CN105319333B - Quality detection method for Jingxuening capsule - Google Patents
Quality detection method for Jingxuening capsule Download PDFInfo
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Abstract
The invention relates to a quality detection method for a Jingxuening capsule and belongs to the technical field of traditional Chinese medicines. The quality detection method comprises the following steps: identifying and qualifying the main ingredients (whitebackleaf mallotus leaf and herba euonymi) by the thin layer chromatography; using the ultraviolet-spectrophotometry to measure the content of general flavone in a Jingxuening capsule; using the high performance liquid chromatography to measure the contents of kaempferol-3,7-dirhamnoside and apigenin-7-O-beta-D-glycocide, wherein the content of general flavone (counted by anhydrous rutin) in each Jingxuening capsule (0.35 g) is not less than 56 mg, and the contents of kaempferol-3,7-dirhamnoside and apigenin-7-O-beta-D-glycocide in each Jingxuening capsule is not less than 0.30 mg and 4.5 mg. For the first time, the quality detection method uses the qualitative identification and quantitative detection methods to detect the Jingxuening capsule, so that the accuracy, the advancement and the effectiveness of the quality detection standard are guaranteed.
Description
Technical field
The present invention relates to the quality inspection of a kind of quality determining method of Chinese medicinal composition preparation, more particularly to Jing Xue Ning Capsule
Survey method.
Background technology
Jing Xue Ning Capsule is by the Chinese patent drug of Guangxi Gold show shrine medicine company Co., Ltd production, Chinese medicines quasi-word
B20020057.Its primary efficacy is：Dissolving stasis and hemostasis；Suitable for stagnation of blood stasis disease menorrhalgia, Jing colors purple is black block, and stomachache is refused
By grade disease；Can also be used for the auxiliary treatment of light moderate hemorrhage of digestive tract；Can also be used for the auxiliary treatment of light moderate hemorrhage of digestive tract.
It is by Whitebackleaf Mallotus Root, the taste medicinal material of winter creeper two is processed makes Chinese medicinal capsule preparation, Guangxi Gold show shrine medicine company Co., Ltd
With Chemistry and Chemical Engineering College of Guangxi University in document《The screening of the quality control standard substance of the peaceful particle of menses》One is literary（Popular section
Skill；2 months 2014 total 174 phases of volume 16）In establish the quality control standard of the peaceful particle of menses, author：Xu Zijing, Tang Yan
Show, Pang Guo.With one of primary raw material therein Whitebackleaf Mallotus Root, separated purifying obtains chemical compounds I to the peaceful particle of the menses, by qualitative
It is accredited as flavonoid glycoside；HPLC is detected as single pure compound；It is 564 that MS determines chemical molecular amount；H NMR and C NMR datas
Analysis is consistent with Corymboside, is cassia corymbosa glycosides, and molecular formula is C26H28O14Therefore using chemical compounds I as the peaceful particle of menses
Quality control standard substance.
But it is simple that qualitative or detection Jing Xue Ning Capsule is come with wherein one of raw material, and also deposit as major quality controlling standard
In problems, inventor is analyzed by the physico-chemical property to Jing Xue Ning Capsule, synchronous Qualitive test Whitebackleaf Mallotus Root and winter creeper, and
The active principle contained to it with reference to Ultraviolet spectrophotometry and high performance liquid chromatography carries out content detection, can be with effective control
The quality of Jing Xue Ning Capsule product.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, there is provided it is a kind of can comprehensively qualitative and quantitative analysis medicine into
Point Jing Xue Ning Capsule quality determining method, this method has that detection means is simple, testing result more accurately, it is reliable special
Point.
The present invention is achieved by the following technical solutions：
The quality determining method of Jing Xue Ning Capsule, including following three kinds of processes：Differentiate qualitative with thin-layered chromatography；With purple
Outward-spectrophotometry general flavone（In terms of rutin）The content of composition；With high effective liquid chromatography for measuring Kaempferol -3,7-
The content of two kinds of compositions of two rhamnosides and api-genin-7-O-β-D-glucoside.
（1）The method that winter creeper, Whitebackleaf Mallotus Root are differentiated using thin-layered chromatography：Winter creeper is with Kaempferol -3, the rhamnoses of 7- bis-
Glycosides（C27H30O16）Meter（Also include the rhamnosides of Kaempferol -3,7- (4 '-acetyl group)-O- α-L- two）, Whitebackleaf Mallotus Root with apiolin-
7-O- β-D-Glucose glycosides meter.
It is prepared by a need testing solutions：
This product content 2g is taken, in putting 50ml round-bottomed flasks, add water 4ml, stirred, make flowing paste, plus acetic acid second
Ester 20ml, 70 DEG C of water-baths flow back 2 hours, let cool, and filtrate is moved to into separatory funnel, draw upper strata ethyl acetate layer, are concentrated into
4ml, it is standby；
It is prepared by b contrast solutions：
Winter creeper control medicinal material 2g, plus 70% ethanol 30ml are taken, is put and be heated to reflux in water-bath 1 hour, filtered, the dregs of a decoction use 70%
Ethanol is washed 3 times, each 10ml, merges ethanol solution, is evaporated, and residue adds 30ml water dissolves, is extracted with ethyl acetate 3 times, every time
20ml, reclaims ethyl acetate, and residue adds methyl alcohol 1ml to be allowed to dissolve, makes winter creeper control medicinal material solution, standby；
Whitebackleaf Mallotus Root control medicinal material 1g is taken, by " preparation method of winter creeper control medicinal material solution " Whitebackleaf Mallotus Root control medicinal material is made
Solution, it is standby；
Take Kaempferol -3, the rhamnosides of 7- bis-, Kaempferol -3, the rhamnosides of 7- (4 '-acetyl group)-O- α-L- two and celery
Dish element -7-O- β-D-Glucose glycosides reference substance, plus methyl alcohol make 1ml respectively containing 1mg solution, it is standby as reference substance solution；
Thin-layered chromatography is tested：Press（2010 editions annex VI B of Chinese Pharmacopoeia）Test, draw the μ l of need testing solution 10, on
Two kinds of control medicinal material solution and each 2 μ l of reference substance solution are stated, is put respectively on same silica gel g thin-layer plate, with chloroform-methanol-second
Acid（40∶10∶0.1）Launch for solvent, taking-up is dried；In uviol lamp（254nm）Lower observation；It is and right in test sample chromatogram
According to the spot for showing same color on product and the corresponding position of control medicinal material chromatogram；
（2）Ultraviolet spectrophotometry determines general flavone（In terms of rutin）Content：
The preparation of a reference substance solutions
Control substance of Rutin 30mg being dried to constant weight is taken, accurately weighed, in putting 100ml volumetric flasks, plus absolute ethyl alcohol is to quarter
Degree, shakes up, and makes rutin standard solutions of every 1ml containing 0.3mg；Precision measures 10ml solution, in putting 50ml measuring bottles, plus 60%
Ethanol shakes up to scale, obtains final product（Per 1ml μ g containing anhydrous rutin 60）；
B Specification Curve of Increasing
Respectively accurate control substance of Rutin solution 1ml, 2ml, 3ml, 4ml, 5ml of drawing is put respectively in 10ml measuring bottles, is respectively added
0.1mol/L aluminum trichloride solution 2ml, 1mol/L liquor kalii acetici 3ml, plus 60% ethanol shakes up to scale, places 30 minutes；
With corresponding reagent as blank, immediately according to UV-VIS spectrophotometry（《Chinese Pharmacopoeia》Version one in 2010, annex VA）,
Mensuration absorbance at the wavelength of 420nm, with absorbance as ordinate, concentration be abscissa draw calibration curve；
It is prepared by c need testing solutions
This product content 0.1g is taken, it is accurately weighed, in putting 10ml measuring bottles, plus 60% ethanol 7ml, put low-grade fever in water-bath, and when
When shake 30 minutes, let cool, plus 60% ethanol shakes up to scale；Precision measures solution 1ml, in putting 10ml measuring bottles, plus 0.1mol/
L aluminum trichloride solution 2ml, 1mol/L liquor kalii acetici 3ml, plus 60% ethanol shakes up to scale, places 30 minutes, centrifuging and taking
Supernatant makees need testing solution, standby；This product content 0.1g is separately taken, it is accurately weighed, in putting 10ml measuring bottles, plus the dilution of 60% ethanol
To scale, precision measures 1ml, and in putting 10ml measuring bottles, plus 60% ethanol shakes up to scale, as blank solution, determines in accordance with the law and inhales
Luminosity, the content of sample general flavone is read from calibration curve；Every Jing Xue Ning Capsule（0.35g）Containing general flavone with anhydrous rutin
Meter, must not be less than 56.0mg；
（3）The rhamnosides of high effective liquid chromatography for measuring Kaempferol -3,7- two and api-genin-7-O-β-D-glucoside
Content：
A chromatographic conditions
With octadecylsilane chemically bonded silica as filler；With acetonitrile-methanol=10：2 (V/V) are mobile phase A；Water-phosphorus
Acid=100：0.05 (V/V) is Mobile phase B, and gradient elution is carried out as follows：
| Time (min) | A | B |
| 0 | 16 | 84 |
| 25 | 20 | 80 |
| 50 | 40 | 60 |
| 80 | 80 | 20 |
Detection wavelength is 340 nm, and theoretical cam curve presses Kaempferol -3, and the rhamnosides of 7- bis- are calculated and should be not less than 3000；
The preparation of b reference substance solutions
Respectively precision weighs the rhamnoside 8.8mg of reference substance Kaempferol -3,7- two, api-genin-7-O-β-D-glucoside
2.5mg, in being respectively placed in 10ml volumetric flasks, plus methanol constant volume, shake up, it is respectively prepared in every 1ml containing 0.88mg and 0.25mg
Solution, as reference substance solution；
The preparation of c need testing solutions takes the content about 1.0g under content uniformity item, accurately weighed, puts conical flask with cover
In, plus 60% methyl alcohol 25ml, weighed weight, water-bath backflow 30 minutes, let cool, less loss quality is supplied with 60% methyl alcohol, shake up, filter
Cross, obtain final product；
D determination methods
It is accurate respectively to draw reference substance solution and each 10 l of need testing solution, liquid chromatograph is injected, determine, obtain final product；
Every Jing Xue Ning Capsule（0.35g）Containing winter creeper with Kaempferol -3, the rhamnosides of 7- bis-（C27H30O16）Meter, much
In 0.30mg;, every Jing Xue Ning Capsule（0.35g）Containing Whitebackleaf Mallotus Root in terms of api-genin-7-O-β-D-glucoside, it is no less than
4.5mg。
The present invention is also investigated to the methodology of winter creeper and Whitebackleaf Mallotus Root active constituent content measuring method, as a result such as
Under：
（1）Linear relationship：Precision measures the rhamnoside reference substance mother liquors of Kaempferol -3,7- two（0.88mg/ml）And celery
Element -7-O- β-D-Glucose glycosides reference substance mother liquor（0.25mg/ml）0.25,0.5,1,2,5ml, in being placed in 10ml measuring bottles, plus stream
Dynamic phase dilution shakes up to scale.In the present inventive method, inject in high performance liquid chromatograph, determine Kaempferol -3, the mouse of 7- bis-
Lee's glucosides and api-genin-7-O-β-D-glucoside peak area.With sample size（m）For abscissa, peak area（A）For ordinate,
Calibration curve is drawn, regression equation is calculated：The rhamnosides of Kaempferol -3,7- two：A=153.8m-126.4, r=0.9997；Celery
Element -7-O- β-D-Glucose glycosides：A=2001.7m-2038.3, r=0.9994, illustrate Kaempferol -3, and the rhamnosides of 7- bis- exist
The offline sexual intercourse of 0.22-4.4mg/ml concentration is good, and api-genin-7-O-β-D-glucoside is dense in 0.0625mg-1.25mg/ml
Spend offline sexual intercourse good.
（2）Precision test：Taking the rhamnosides of Kaempferol -3,7- two and concentration that concentration is 0.88mg/ml is
The control sample solution of 0.25mg/ml api-genin-7-O-β-D-glucosides, each accurate absorption 10ul, injects liquid chromatograph,
The peak area of two active ingredient is determined, as a result METHOD FOR CONTINUOUS DETERMINATION 6 times see the table below 1.
The rhamnoside Precision test results of 1 Kaempferol -3,7- of table two
The api-genin-7-O-β-D-glucoside Precision test result of table 2
Result above shows that this method precision is good.
（3）Stability test：This product need testing solution is taken, at regular intervals, liquid chromatograph is injected, kaempferia galamga is determined
Phenol -3, the rhamnosides of 7- bis- and api-genin-7-O-β-D-glucoside peak area, the results are shown in Table 3 and table 4.
The rhamnoside stability test results of 3 Kaempferol -3,7- of table two
The api-genin-7-O-β-D-glucoside stability test result of table 4
Result above shows that sample is stable in 4 hours, and this method has good stability.
（4）Reappearance test：5 parts of this product is taken, is determined by the inventive method, the results are shown in Table 5.
The rhamnoside reproducible test results of 5 Kaempferol -3,7- of table two
The api-genin-7-O-β-D-glucoside reproducible test results of table 6
Result above shows that this method reappearance is good.
（5）Recovery test：Precision measures this product 2ml, and precision adds reference substance mother liquor appropriate, determines by the inventive method
Kaempferol -3, the rhamnosides of 7- bis- and api-genin-7-O-β-D-glucoside content, are calculated as follows the rate of recovery, the results are shown in Table
7。
The rate of recovery=（Measured amount-known quantity）/ addition * 100
The rhamnoside recovery test results of 7 Kaempferol -3,7- of table two
The api-genin-7-O-β-D-glucoside recovery test result of table 8
Result above shows that this method rate of recovery is good.
（6）Negative interference test：Take without winter creeper and negative controls made by Whitebackleaf Mallotus Root medicinal material, by the inventive method
The peak area of Kaempferol -3, the rhamnosides of 7- bis- and api-genin-7-O-β-D-glucoside is determined, is as a result shown noiseless.
（7）Sample determination：This product 5 batches is taken, by the inventive method, Kaempferol -3, the rhamnosides of 7- bis- and celery is determined
Element -7-O- β-D-Glucose glycosides content, the results are shown in Table
Active constituent content measuring result in 95 batches of Identifications of Qingzhuo Qudu Pill of table
Present invention has the advantages that：Differentiate two kinds of active ingredients of Whitebackleaf Mallotus Root and winter creeper using thin-layer identification method, use
Ultraviolet-spectrophotometry general flavone content, in terms of anhydrous rutin content；Using high effective liquid chromatography for measuring Kaempferol -3,
The rhamnosides of 7- bis- and api-genin-7-O-β-D-glucoside content, method is easy, result is accurate, favorable reproducibility.Existing document
Simply Qualitive test is carried out to Whitebackleaf Mallotus Root in Plays, without carrying out quantitative determination to it, limitation is big, it is difficult to control Jing
The quality of blood Yiganning capsule, the present invention establish in terms of qualitative, quantitative two to the main component Whitebackleaf Mallotus Root in Jing Xue Ning Capsule and
Winter creeper carries out quality control, substantially increases the accuracy of quality control.Drug quality is carried out by above detection project
Effective control, with it is stable, quick, sensitive, reliable the characteristics of, product inherent quality is further ensured that, to promoting product
Sale, it is ensured that patient medication security implications are great.
Specific embodiment
Embodiment 1
Quality control is carried out to Jing Xue Ning Capsule using following quality determining method.
（1）Winter creeper, Whitebackleaf Mallotus Root are differentiated using thin-layered chromatography：
It is prepared by a need testing solutions：
Jing Xue Ning Capsule content 2g is taken, in putting 50ml round-bottomed flasks, add water 4ml, stirred, make flowing paste, plus
Ethyl acetate 20ml, 70 DEG C of water-baths flow back 2 hours, let cool, and filtrate is moved to into separatory funnel, draw upper strata ethyl acetate layer, dense
4ml is reduced to, it is standby.
It is prepared by b contrast solutions：
Winter creeper control medicinal material 2g, plus 70% ethanol 30ml are taken, is put and be heated to reflux in water-bath 1 hour, filtered, the dregs of a decoction use 70%
Ethanol is washed 3 times, each 10ml, merges ethanol solution, is evaporated, and residue adds 30ml water dissolves, is extracted with ethyl acetate 3 times, every time
20ml, reclaims ethyl acetate, and residue adds methyl alcohol 1ml to be allowed to dissolve, makes winter creeper control medicinal material solution, standby.
Whitebackleaf Mallotus Root control medicinal material 1g is taken, by " preparation method of winter creeper control medicinal material solution " Whitebackleaf Mallotus Root control medicinal material is made
Solution, it is standby.
Take Kaempferol -3, the rhamnosides of 7- bis-, Kaempferol -3, the rhamnosides of 7- (4 '-acetyl group)-O- α-L- two and celery
Dish element -7-O- β-D-Glucose glycosides reference substance, plus methyl alcohol make 1ml respectively containing 1mg solution, it is standby as reference substance solution.
Thin-layered chromatography is tested：Press（2010 editions annex VI B of Chinese Pharmacopoeia）Test, draw the μ l of need testing solution 10, on
Two kinds of control medicinal material solution and each 2 μ l of reference substance solution are stated, is put respectively on same silica gel g thin-layer plate, with chloroform-methanol-second
Acid（40∶10∶0.1）Launch for solvent, taking-up is dried；In uviol lamp（254nm）Lower observation.
As a result it is as follows：In test sample Jing Xue Ning Capsule chromatogram, on position corresponding with reference substance and control medicinal material chromatogram
The spot of aobvious same color；It is noiseless, without conditions of streaking.
（2）Ultraviolet spectrophotometry determines general flavone（In terms of rutin）Content：
The preparation of a reference substance solutions
Control substance of Rutin 30mg being dried to constant weight is taken, accurately weighed, in putting 100ml volumetric flasks, plus absolute ethyl alcohol is to quarter
Degree, shakes up, and makes rutin standard solutions of every 1ml containing 0.3mg；Precision measures 10ml solution, in putting 50ml measuring bottles, plus 60%
Ethanol shakes up to scale, obtains final product（Per 1ml μ g containing anhydrous rutin 60）.
B Specification Curve of Increasing
Respectively accurate control substance of Rutin solution 1ml, 2ml, 3ml, 4ml, 5ml of drawing is put respectively in 10ml measuring bottles, is respectively added
0.1mol/L aluminum trichloride solution 2ml, 1mol/L liquor kalii acetici 3ml, plus 60% ethanol shakes up to scale, places 30 minutes；
With corresponding reagent as blank, immediately according to UV-VIS spectrophotometry（《Chinese Pharmacopoeia》Version one in 2010, annex VA）,
Mensuration absorbance at the wavelength of 420nm, with absorbance as ordinate, concentration be abscissa draw calibration curve.
It is prepared by c need testing solutions
Jing Xue Ning Capsule is taken, 2014010130 batches of sampling Detections of lot number take content 0.1g, accurately weighed, put 10ml amounts
In bottle, plus 60% ethanol 7ml, low-grade fever in water-bath is put, and constantly shake 30 minutes, let cool, plus 60% ethanol shakes up to scale；Essence
It is close to measure solution 1ml, in putting 10ml measuring bottles, plus 0.1mol/L aluminum trichloride solution 2ml, 1mol/L liquor kalii acetici 3ml, plus
60% ethanol shakes up to scale, places 30 minutes, and centrifuging and taking supernatant makees need testing solution, standby；Separately take this product content
0.1g, accurately weighed, in putting 10ml measuring bottles, plus 60% ethanol is diluted to scale, and precision measures 1ml, in putting 10ml measuring bottles, plus 60%
Ethanol shakes up to scale, and used as blank solution, in accordance with the law mensuration absorbance, the content of sample general flavone is read from calibration curve.
As a result it is as follows：
This batch of Jing Xue Ning Capsule is containing general flavone with anhydrous rutin（C27H30O16）Meter, is 75.0mg；
（3）The rhamnosides of high effective liquid chromatography for measuring Kaempferol -3,7- two and apiolin -7-O-β- D-Glucose glycosides
Content：
A chromatographic conditions
With octadecylsilane chemically bonded silica as filler；With acetonitrile-methanol=10：2 (V/V) are mobile phase A；Water-phosphorus
Acid=100：0.05 (V/V) is Mobile phase B, and gradient elution is carried out as follows：
0min：A-B is 16：84；
25min：A-B is 20：80；
50min：A-B is 40:60；
80min：A-B is 80:20；
Detection wavelength is 340 nm, and theoretical cam curve presses Kaempferol -3, and the rhamnosides of 7- bis- are calculated and should be not less than 3000.
The preparation of b reference substance solutions
Respectively precision weighs the rhamnoside 8.8mg of reference substance Kaempferol -3,7- two, api-genin-7-O-β-D-glucoside
2.5mg, in being respectively placed in 10ml volumetric flasks, plus methanol constant volume, shake up, it is respectively prepared in every 1ml containing 0.88mg and 0.25mg
Solution, as reference substance solution.
The preparation of c need testing solutions takes the content about 1.0g under content uniformity item, accurately weighed, puts conical flask with cover
In, plus 60% methyl alcohol 25ml, weighed weight, water-bath backflow 30 minutes, let cool, less loss quality is supplied with 60% methyl alcohol, shake up, filter
Cross, obtain final product.
D determination methods
It is accurate respectively to draw reference substance solution and each 10 l of need testing solution, liquid chromatograph is injected, determine, obtain final product.
Every Jing Xue Ning Capsule（0.35g）Containing winter creeper with Kaempferol -3, the rhamnoside meters of 7- bis-, no less than 0.30mg;,
Every Jing Xue Ning Capsule（0.35g）Containing Whitebackleaf Mallotus Root in terms of api-genin-7-O-β-D-glucoside, no less than 4.5mg.Inventor presses
Also the Jing Xue Ning Capsule from production in -2014 years 2012 is inspected by random samples according to above method, it is as a result as follows：
2012-2014 Jing Xue Ning Capsules different batches inspect assay result by random samples
As can be seen that by carrying out content detection, Ke Yiyou to the Jing Xue Ning Capsule that 2012-2014 different batches are produced
Effect ensures product quality, and Jing repetition tests are the quality determining method specificity, reproducible, therefore as Jing Xue Ning Capsule
Quality control qualitative checking method, to Jing Xue Ning Capsule quality control is carried out.
Claims (1)
1. a kind of quality determining method of Jing Xue Ning Capsule, it is characterised in that：Including following three kinds of detection process：（1）Use thin layer
Chromatography differentiates qualitative；（2）The content of rutin composition in general flavone is determined with Ultraviolet spectrophotometry；（3）Use high-efficient liquid phase color
Spectrometry determines the rhamnosides of Kaempferol -3,7- two and apiolin -7-O-βThe content of two kinds of compositions of-D-Glucose glycosides；
Thin-layered chromatography differentiate winter creeper, Whitebackleaf Mallotus Root method it is as follows：
It is prepared by a need testing solutions：
This product content 2g is taken, in putting 50ml round-bottomed flasks, add water 4ml, stirred, make flowing paste, plus ethyl acetate
20ml, 70 DEG C of water-baths flow back 2 hours, let cool filtration, and filtrate is moved to into separatory funnel, draw upper strata ethyl acetate layer, are concentrated into
4ml, it is standby；
It is prepared by b contrast solutions：
Winter creeper control medicinal material 2g, plus 70% ethanol 30ml are taken, is put and be heated to reflux in water-bath 1 hour, filtered, 70% ethanol of the dregs of a decoction
Wash 3 times, each 10ml, merge ethanol solution, be evaporated, residue adds 30ml water dissolves, is extracted with ethyl acetate 3 times, each 20ml,
Ethyl acetate is reclaimed, residue adds methyl alcohol 1ml to be allowed to dissolve, makes winter creeper control medicinal material solution, standby；
Whitebackleaf Mallotus Root control medicinal material 1g is taken, Whitebackleaf Mallotus Root control medicinal material is made by " preparation method of winter creeper control medicinal material solution " molten
Liquid, it is standby；
Take Kaempferol -3, the rhamnosides of 7- bis-, Kaempferol -3, the rhamnosides of 7- (4 '-acetyl group)-O- α-L- two and apiolin -
7-O- β-D-Glucose glycosides reference substance, plus methyl alcohol make 1ml respectively containing 1mg solution, it is standby as reference substance solution；
Thin-layered chromatography is tested：By 2010 editions annex VI B tests of Chinese Pharmacopoeia, the μ l of need testing solution 10, above two are drawn
Control medicinal material solution and each 2 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-acetic acid volume
Than=40: be solvent expansion at 10: 0.1, and taking-up is dried；Observe under 254nm uviol lamps；In test sample chromatogram, with reference substance
And on the corresponding position of control medicinal material chromatogram show same color spot；
It is as follows that the Ultraviolet spectrophotometry determines general flavone method of content in terms of rutin：
The preparation of a reference substance solutions
Control substance of Rutin 30mg being dried to constant weight is taken, accurately weighed, in putting 100ml volumetric flasks, plus absolute ethyl alcohol is to scale, shakes
It is even, make rutin standard solutions of every 1ml containing 0.3mg；Precision measures 10ml solution, and in putting 50ml measuring bottles, plus 60% ethanol is extremely
Scale, shakes up, and obtains final product, now, per 1ml μ g containing anhydrous rutin 60；
B Specification Curve of Increasing
Respectively accurate control substance of Rutin solution 1ml, 2ml, 3ml, 4ml, 5ml of drawing is put respectively in 10ml measuring bottles, respectively adds 0.1mol/
L aluminum trichloride solution 2ml, 1mol/L liquor kalii acetici 3ml, plus 60% ethanol shakes up to scale, places 30 minutes；Mutually to take an entrance examination
Agent for blank, immediately according to《Chinese Pharmacopoeia》Version one in 2010, the UV-VIS spectrophotometry described in annex VA,
Mensuration absorbance at the wavelength of 420nm, with absorbance as ordinate, concentration be abscissa draw calibration curve；
It is prepared by c need testing solutions
This product content 0.1g is taken, it is accurately weighed, in putting 10ml measuring bottles, plus 60% ethanol 7ml, low-grade fever in water-bath is put, and constantly shake
Shake 30 minutes, let cool, plus 60% ethanol shakes up to scale；Precision measures solution 1ml, in putting 10ml measuring bottles, plus 0.1mol/L tri-
Liquor alumini chloridi 2ml, 1mol/L liquor kalii acetici 3ml, plus 60% ethanol shakes up to scale, places 30 minutes, centrifuging and taking supernatant
Liquid makees need testing solution, standby；This product content 0.1g is separately taken, accurately weighed, in putting 10ml measuring bottles, plus 60% ethanol is diluted to
Scale, precision measures 1ml, and in putting 10ml measuring bottles, plus 60% ethanol shakes up to scale, as blank solution, extinction is determined in accordance with the law
Degree, the content of sample general flavone is read from calibration curve；Every Jing Xue Ning Capsule 0.35g is containing general flavone with anhydrous rutin
（C27H30O16）Meter, must not be less than 56.0mg；
The rhamnosides of high effective liquid chromatography for measuring Kaempferol -3,7- two and apiolin -7-O-β- D-Glucose glycosides contains
Amount method is as follows：
A chromatographic conditions
With octadecylsilane chemically bonded silica as filler；With acetonitrile-methanol=10：2 (V/V) are mobile phase A；Water-phosphoric acid=
100：0.05 (V/V) is Mobile phase B, and gradient elution is carried out as follows：
0min：A-B is 16：84；
25min：A-B is 20：80；
50min：A-B is 40:60；
80min：A-B is 80:20；
Detection wavelength is 340 nm, and theoretical cam curve presses Kaempferol -3, and the rhamnosides of 7- bis- are calculated and should be not less than 3000；
The preparation of b reference substance solutions
Respectively precision weighs the rhamnoside 8.8mg of reference substance Kaempferol -3,7- two, api-genin-7-O-β-D-glucoside
2.5mg, in being respectively placed in 10ml volumetric flasks, plus methanol constant volume, shake up, it is respectively prepared in every 1ml containing 0.88mg and 0.25mg
Solution, as reference substance solution；
The preparation of c need testing solutions takes the content about 1.0g under content uniformity item, accurately weighed, in putting conical flask with cover, plus
60% methyl alcohol 25ml, weighed weight, water-bath flows back 30 minutes, lets cool, and with 60% methyl alcohol less loss quality is supplied, and shakes up, and filters, i.e.,
；
D determination methods
It is accurate respectively to draw reference substance solution and each 10 l of need testing solution, liquid chromatograph is injected, determine, obtain final product；
Every Jing Xue Ning Capsule, weight 0.35g, containing winter creeper with Kaempferol -3, the rhamnosides of 7- bis-（C27H30O16）Meter, much
In 0.30mg;, every Jing Xue Ning Capsule, weight 0.35g containing Whitebackleaf Mallotus Root in terms of api-genin-7-O-β-D-glucoside, is no less than
4.5mg。
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