CN106950294A - A kind of antiphlogistic Chunwang capsule quality determining method - Google Patents
A kind of antiphlogistic Chunwang capsule quality determining method Download PDFInfo
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- CN106950294A CN106950294A CN201710096429.9A CN201710096429A CN106950294A CN 106950294 A CN106950294 A CN 106950294A CN 201710096429 A CN201710096429 A CN 201710096429A CN 106950294 A CN106950294 A CN 106950294A
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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
A kind of antiphlogistic Chunwang capsule quality determining method, belongs to drug quality detection technique field.The present invention is by determining to andrographolide and Determination of Dehydroandrographoliin and reaching the quality testing of antiphlogistic Chunwang capsule to the method for Genkwanin assay.The present invention is by multi objective assay, and quality that can be more fully to antiphlogistic Chunwang capsule is evaluated, it is ensured that the stability of product quality and the validity of clinical application and security.The present invention can more be adapted to the requirement that quick inspection and traditional Chinese medicine quality control are improved with the characteristics of detection means is simple, testing result is accurate, quality surveillance is more comprehensive.
Description
Technical field
The invention belongs to drug quality detection technique field, a kind of quality standard detection of antiphlogistic Chunwang capsule is particularly belonged to
Method.
Background technology
Antiphlogistic Chunwang capsule prescription is made up of Herba Andrographitis and the taste Chinese medicine of Wikstroemia indica two, and wherein Herba Andrographitis is worn for acanthaceous plant
The dry aerial parts of heart lotus, be《Chinese Pharmacopoeia》And the local drug standards are recorded, for the hot cough and asthma of phlegm, suffer from abdominal pain, and it is anxious slow
Property tonsillitis, sphagitis, pneumonia, acute gastroenteritis, acute bacillary dysentery are shown in above symptom..Principle active component is Herba Andrographitis
The diterpene-kind compounds such as lactone, Dehydro and drographolide and flavone compound, Wikstroemia indica are the dry of Isolated From Thymelaeaceae Species Wikstroemia indica
Dry or root skin, contain a variety of chemical compositions such as Genkwanin.At present, only Dehydro and drographolide is entered in existing quality standard
Assay is gone.Assay is not carried out to index composition in Wikstroemia indica, it is impossible to ensure medicine in process of production
Inherent quality.Instant invention overcomes the deficiency of original standard, establish to two taste medicine Herba Andrographitis and Wikstroemia indica middle finger in the product
Mark the content assaying method of composition.Product quality can effectively be controlled, it is ensured that the stability of the product quality.
The content of the invention
The purpose of the present invention is simple there is provided a kind of detection means in view of the shortcomings of the prior art, and testing result is accurate
The quality determining method of antiphlogistic Chunwang capsule, by determining and andrographolide and Determination of Dehydroandrographoliin to Genkwanin
Content assaying method reaches the quality testing to antiphlogistic Chunwang capsule.
The present invention is achieved through the following technical solutions.
A kind of antiphlogistic Chunwang capsule quality determining method, it is characterised in that comprise the following steps：
（1）Andrographolide and Determination of Dehydroandrographoliin are determined
A chromatographic conditions and system suitability test：It is filler with octadecylsilane chemically bonded silica, with methanol-water（35~
45：65~55）For mobile phase；Andrographolide Detection wavelength is 225nm, Dehydro and drographolide 254nm；Column temperature：20 DEG C~
30℃；Flow velocity：1.0mL/min；Number of theoretical plate is calculated by andrographolide and Dehydro and drographolide all should be not less than 3000；
The preparation of b reference substance solutions：Precision weighs andrographolide and Dehydro and drographolide reference substance is appropriate, plus methanol system
Into solution of every 1ml containing about 40ug and 30ug, produce；
The preparation of c need testing solutions：This product about 0.2~0.5g is taken, it is finely ground, it is accurately weighed, put in 50ml measuring bottles, precision is added
Methanol 50ml, weighed weight ultrasonically treated 30~60 minutes, adds methanol to supply the weight of less loss, filtration is filtered with micropore after letting cool
Membrane filtration mistake, takes subsequent filtrate, produces；
D is determined：It is accurate respectively to draw reference substance solution and each 5~20ul of need testing solution, liquid chromatograph is injected separately into, is surveyed
It is fixed, produce；
Every sample of this product is containing Herba Andrographitis with Dehydro and drographolide（C20H28O4）Meter, every dress 0.22g of specification one must not be less than
0.3mg, every dress 0.44g of specification two must not be less than 0.6mg.
Every sample of this product is containing Herba Andrographitis with andrographolide（C20H30O5）Meter, every dress 0.22g of specification one must not be less than
0.2mg, every dress 0.44g of specification two must not be less than 0.4mg；
（2）Genkwanin assay
A chromatographic conditions and system suitability test：Using octadecylsilane chemically bonded silica as filler；With methanol：0.2% phosphoric acid
Solution (65~85：35~15) be mobile phase；Genkwanin Detection wavelength is 330~350nm；Column temperature：20 DEG C~30 DEG C；Flow velocity：
1.0mL/min；Number of theoretical plate is calculated by Genkwanin peak should be not less than 2000；
The preparation of b reference substance solutions：Take Genkwanin reference substance appropriate, it is accurately weighed, put in brown measuring bottle, plus methanol is made often
1ml contains 20 μ g solution, produces；
The preparation of c need testing solutions：This product about 0.5~1.5g is taken, it is finely ground, it is accurately weighed, put in 50ml measuring bottles, precision is added
Methanol 50ml, ultrasound 30~60 minutes, filtration takes subsequent filtrate, produced；
D is determined：Precision draws reference substance solution and each 5~20ul of need testing solution, is injected separately into liquid chromatograph, determines, i.e.,
；
Every sample of this product is containing Wikstroemia indica with Genkwanin（C16H12O5）Meter, every dress 0.22g of specification one must not be less than 0.06mg,
The every dress 0.44g of specification two must not be less than 0.012mg.
The beneficial effects of the invention are as follows：The present invention, can be more fully to Chuanwang anti-inflammation glue by multi objective assay
The quality of capsule is evaluated, it is ensured that the stability of product quality and the validity of clinical application and security.The present invention has inspection
Survey means are simple, testing result accurate, the characteristics of quality surveillance is more comprehensive, can more be adapted to quick examine and traditional Chinese medicine quality control
The requirement of raising.
Brief description of the drawings
Accompanying drawing 1：Example andrographolide reference substance collection of illustrative plates.
Accompanying drawing 2：Example Dehydro and drographolide reference substance collection of illustrative plates.
Accompanying drawing 3：Example Determination of Andrographolide determination sample collection of illustrative plates.
Accompanying drawing 4：Example Determination of Dehydroandrographoliin determination sample collection of illustrative plates.
Accompanying drawing 5：Example Genkwanin reference substance collection of illustrative plates.
Accompanying drawing 6：Example Genkwanin assay sample collection of illustrative plates.
Embodiment
Technical scheme is elaborated below by embodiment and its accompanying drawing, the embodiment and accompanying drawing pair enumerated
The present invention is not limited.
A kind of antiphlogistic Chunwang capsule quality determining method, comprises the following steps：
（1）Andrographolide and Determination of Dehydroandrographoliin are determined
A chromatographic conditions and system suitability test：It is filler with octadecylsilane chemically bonded silica, with methanol-water（50：
50）For mobile phase；Andrographolide Detection wavelength is 225nm, Dehydro and drographolide 254nm；Column temperature：30℃；Flow velocity：
1.0mL/min number of theoretical plates are calculated by andrographolide and Dehydro and drographolide all should be not less than 3000.
The preparation of b reference substance solutions：Precision weighs andrographolide and Dehydro and drographolide reference substance is appropriate, plus first
Solution of every 1ml containing 40ug and 30ug is made in alcohol, produces.
The preparation of c need testing solutions：This product 0.2g is taken, it is finely ground, it is accurately weighed, put in 50ml measuring bottles, precision adds methanol
50ml, weighed weight ultrasonically treated 30 minutes, adds methanol to supply the weight of less loss, filtration is filtered with miillpore filter after letting cool,
Subsequent filtrate is taken, is produced.
D is determined：It is accurate respectively to draw reference substance solution and each 10ul of need testing solution, liquid chromatograph is injected separately into, is surveyed
It is fixed, produce.
Every sample of this product is containing Herba Andrographitis with Dehydro and drographolide（C20H28O4）Meter, specification（1）Every dress 0.22g must not
Less than 0.3mg, specification（2）Every dress 0.44g must not be less than 0.6mg.
Every sample of this product is containing Herba Andrographitis with andrographolide（C20H30O5）Meter, specification（1）Every dress 0.22g must not be less than
0.2mg, specification（2）Every dress 0.44g must not be less than 0.4mg.
（2）Genkwanin assay
A chromatographic conditions and system suitability test：Using octadecylsilane chemically bonded silica as filler；With methanol：0.2% phosphoric acid
Solution (55：45) it is mobile phase；Genkwanin Detection wavelength is 346nm；Column temperature：30℃；Flow velocity：1.0mL/min number of theoretical plates are pressed
Genkwanin peak, which is calculated, should be not less than 2000.
The preparation of b reference substance solutions：Take Genkwanin reference substance appropriate, it is accurately weighed, put in brown measuring bottle, plus methanol system
Contain 20 μ g solution into every 1ml, produce.
The preparation of c need testing solutions：The preparation of need testing solution：This product 1.0g is taken, it is finely ground, it is accurately weighed, put 50ml amounts
In bottle, precision adds methanol 50ml, and ultrasound filters, takes subsequent filtrate, produce for 30 minutes.
D is determined：Precision draws reference substance solution and each 10ul of need testing solution, is injected separately into liquid chromatograph, determines,
Produce.
Every sample of this product is containing Wikstroemia indica with Genkwanin（C16H12O5）Meter, specification（1）Every dress 0.22g must not be less than
0.06mg, specification（2）Every dress 0.44g must not be less than 0.012mg.
Claims (3)
1. a kind of antiphlogistic Chunwang capsule quality determining method, it is characterised in that comprise the following steps：
（1）Andrographolide and Determination of Dehydroandrographoliin are determined
A chromatographic conditions and system suitability test：It is filler with octadecylsilane chemically bonded silica, using methanol-water as flowing
Phase；Andrographolide Detection wavelength is 225nm, Dehydro and drographolide 254nm；Column temperature：20 DEG C~30 DEG C；Flow velocity：1.0mL/
min；Number of theoretical plate is calculated by andrographolide and Dehydro and drographolide all should be not less than 3000；
The preparation of b reference substance solutions：Precision weighs andrographolide and Dehydro and drographolide reference substance is appropriate, plus methanol system
Into solution of every 1ml containing about 40ug and 30ug, produce；
The preparation of c need testing solutions：This product about 0.2~0.5g is taken, it is finely ground, it is accurately weighed, put in 50ml measuring bottles, precision is added
Methanol 50ml, weighed weight ultrasonically treated 30~60 minutes, adds methanol to supply the weight of less loss, filtration is filtered with micropore after letting cool
Membrane filtration mistake, takes subsequent filtrate, produces；
D is determined：It is accurate respectively to draw reference substance solution and each 5~20ul of need testing solution, liquid chromatograph is injected separately into, is surveyed
It is fixed, produce；
Every sample of this product is containing Herba Andrographitis with Dehydro and drographolide（C20H28O4）Meter, every dress 0.22g of specification one must not be less than
0.3mg, every dress 0.44g of specification two must not be less than 0.6mg；
Every sample of this product is containing Herba Andrographitis with andrographolide（C20H30O5）Meter, every dress 0.22g of specification one must not be less than
0.2mg, every dress 0.44g of specification two must not be less than 0.4mg；
（2）Genkwanin assay
A chromatographic conditions and system suitability test：Using octadecylsilane chemically bonded silica as filler；With methanol：0.2% phosphoric acid
Solution is mobile phase；Genkwanin Detection wavelength is 330~350nm；Column temperature：20 DEG C~30 DEG C；Flow velocity：1.0mL/min；Theoretical plate
Number is calculated by Genkwanin peak should be not less than 2000；
The preparation of b reference substance solutions：Take Genkwanin reference substance appropriate, it is accurately weighed, put in brown measuring bottle, plus methanol is made often
1ml contains 20 μ g solution, produces；
The preparation of c need testing solutions：This product about 0.5~1.5g is taken, it is finely ground, it is accurately weighed, put in 50ml measuring bottles, precision is added
Methanol 50ml, ultrasound 30~60 minutes, filtration takes subsequent filtrate, produced；
D is determined：Precision draws reference substance solution and each 5~20ul of need testing solution, is injected separately into liquid chromatograph, determines, i.e.,
；
Every sample of this product is containing Wikstroemia indica with Genkwanin（C16H12O5）Meter, every dress 0.22g of specification one must not be less than 0.06mg, rule
The every dress 0.44g of lattice two must not be less than 0.012mg.
2. a kind of antiphlogistic Chunwang capsule quality determining method according to claim 1, it is characterised in that：Step（1）Middle chromatogram
Condition and methanol in system suitability test：Water is 35~45：65~55.
3. a kind of antiphlogistic Chunwang capsule quality determining method according to claim 1, it is characterised in that：Step（2）Middle chromatogram
Condition and methanol in system suitability test：0.2% phosphoric acid solution is 65~85：35~15.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710096429.9A CN106950294A (en) | 2017-02-22 | 2017-02-22 | A kind of antiphlogistic Chunwang capsule quality determining method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710096429.9A CN106950294A (en) | 2017-02-22 | 2017-02-22 | A kind of antiphlogistic Chunwang capsule quality determining method |
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| CN106950294A true CN106950294A (en) | 2017-07-14 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107449848A (en) * | 2017-09-22 | 2017-12-08 | 完美（中国）有限公司 | A kind of method of La Ruia extracts in discriminating cosmetic material |
| CN108452094A (en) * | 2018-02-28 | 2018-08-28 | 广东力罗定制药有限公司 | A kind of Chuanwang anti-inflammation piece and its preparation process |
| CN109142588A (en) * | 2018-10-25 | 2019-01-04 | 广州白云山光华制药股份有限公司 | A kind of LianZhixiaoyan Capsule HPLC characteristic spectrum and its construction method and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107449848A (en) * | 2017-09-22 | 2017-12-08 | 完美（中国）有限公司 | A kind of method of La Ruia extracts in discriminating cosmetic material |
| CN108452094A (en) * | 2018-02-28 | 2018-08-28 | 广东力罗定制药有限公司 | A kind of Chuanwang anti-inflammation piece and its preparation process |
| CN109142588A (en) * | 2018-10-25 | 2019-01-04 | 广州白云山光华制药股份有限公司 | A kind of LianZhixiaoyan Capsule HPLC characteristic spectrum and its construction method and application |
| CN109142588B (en) * | 2018-10-25 | 2021-07-09 | 广州白云山光华制药股份有限公司 | HPLC (high performance liquid chromatography) characteristic spectrum of Lianzhi anti-inflammation capsules as well as construction method and application thereof |
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Application publication date: 20170714 |