CN107389826A - A kind of naphcon and its detection method about material - Google Patents
A kind of naphcon and its detection method about material Download PDFInfo
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- CN107389826A CN107389826A CN201710701060.XA CN201710701060A CN107389826A CN 107389826 A CN107389826 A CN 107389826A CN 201710701060 A CN201710701060 A CN 201710701060A CN 107389826 A CN107389826 A CN 107389826A
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- naphcon
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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
The present invention relates to chemicals analysis method technical field, more particularly to a kind of naphcon and its detection method about material.It is characterized in that：Gradient elution is carried out on high performance liquid chromatograph, its chromatographic condition includes：Chromatographic column is octadecylsilane chemically bonded silica chromatographic column, and using octane sulfonate sodium solution as mobile phase A, acetonitrile is Mobile phase B, and Detection wavelength is 275~285nm, 20 40 DEG C of column temperature, flow velocity：0.9 1.1mL/min, carry out gradient elution；Wherein mobile phase A compound method is：Perfluorooctane sulfonate and potassium dihydrogen phosphate are taken, is dissolved with water and is diluted to 1000mL, add triethylamine 5mL, with phosphorus acid for adjusting pH value to 2.6 3.0.The present invention can be efficiently separated naphcon and its relevant material, and separating degree is good, so as to effectively control the quality of naphcon.
Description
（One）Technical field
The present invention relates to chemicals analysis method technical field, more particularly to a kind of naphcon and its relevant material
Detection method.
（Two）Background technology
It is well known that influence of the pharmaceutical purity to patient is very big.It is to cause adverse drug reaction to inject drug impurity（Such as
Allergy, drug fever etc.）The main reason for.Oral drugs are impure, may increase the incidence of adverse reaction, such as Nausea and vomiting, abdomen
Bitterly, diarrhoea etc..Meanwhile may influence be medicine absorption, so as to influence curative effect of medication.Therefore, the detection side of pharmaceutical purity
Method is just particularly important, relevant material（Telated substances）Refer to the starting material brought into production of raw medicine
The materials such as material, reagent, intermediate, accessory substance, it is also possible to preparation caused degraded production in production, storage and transportation
The special impurities such as thing, polymer or crystal transfer.Species and the close phase of synthetic route and production technology of medicine about material
To close, different synthetic route and production technology, the impurity spectrum of medicine can also change, therefore, it is necessary to according to different synthesis
Route and production technology establish suitable analysis method, reach to naphcon about the accurate and effective detection of material and
Monitoring.
At present, the detection method for pharmaceutical purity also has a variety of, wherein, relevant material detection is control drug quality
Important indicator.Naphcon（Naphazoline Hydrochloride）, entitled 4, the 5- dihydros -2- of chemistry（1- naphthalene first
Base）- 1H- imidazole hydrochlorides, its molecular formula are C14H14N2 HCl, and molecular weight 246.74, No. CAS is 550-99-2, and it is tied
Structure formula is as follows：
Naphcon is sympathomimetic amine medicine, directly acts on the alpha adrenergic receptor of conjunctiva parteriole, makes vessel retraction,
Alleviate the conjunctival congestion caused by anaphylaxis and inflammation, in order to ensure the safe and effective of medicine, it is necessary to relevant material to medicine
Studied, detected and monitored.Chinese Pharmacopoeia two naphcon standard regulations of version in 2015 determine relevant thing with TLC methods
Matter.
Subject matter existing for the technical scheme is that its relevant substance method is thin-layered chromatography（TLC methods）, in relevant thing
During quality inspection is looked into, each impurity can not be quantitative determined, detection sensitivity is low, so thin-layered chromatography is not so good as high performance liquid chromatography.
（Three）The content of the invention
The present invention is in order to make up the deficiencies in the prior art, there is provided a kind of naphcon and its detection side about material
Method.
The present invention is achieved through the following technical solutions：
A kind of naphcon and its detection method about material, it is characterised in that：Carried out on high performance liquid chromatograph
Gradient elution, its chromatographic condition include：Chromatographic column is octadecylsilane chemically bonded silica chromatographic column, using octane sulfonate sodium solution as
Mobile phase A, acetonitrile are Mobile phase B, and Detection wavelength is 275~285nm, 20-40 DEG C of column temperature, flow velocity：0.9-1.1mL/min, enter
Row gradient elution；Wherein mobile phase A compound method is：Perfluorooctane sulfonate and potassium dihydrogen phosphate are taken, is dissolved and is diluted to water
1000mL, add triethylamine 5mL, with phosphorus acid for adjusting pH value to 2.6-3.0.
Further, the process of the gradient elution is：In 0~20min, the volume ratio of mobile phase A and Mobile phase B is from 78:
22 at the uniform velocity gradual changes are to 74:26；In 20~32min, the volume ratio of mobile phase A and Mobile phase B is 74:26；In 32~60min, stream
The volume ratio of dynamic phase A and Mobile phase B is from 74:26 at the uniform velocity gradual changes are to 50:50；In 60~65min, the body of mobile phase A and Mobile phase B
Product is than being 50:50；In 65~66min, the volume ratio of mobile phase A and Mobile phase B is from 50:50 at the uniform velocity gradual changes are to 78:22；66~
In 80min, the volume ratio of mobile phase A and Mobile phase B is 78:22.
Wherein, in mobile phase A, the concentration of octane sulfonate sodium solution is 1.41g/L~1.73g/L.
More excellent, the concentration of the octane sulfonate sodium solution is 1.57g/L.
Wherein, in mobile phase A, the concentration of the solution of potassium dihydrogen phosphate is 1.53g/L~1.87g/L.
More excellent, the concentration of the potassium dihydrogen phosphate is 1.7g/L.
Wherein, the length of the chromatographic column is 250mm, and a diameter of 4.6mm, packing material size is 5 μm.
Wherein, the Detection wavelength is 280nm.
Wherein, the column temperature is 30 DEG C.
Wherein, the flow velocity is 1.0mL/min.
In the present invention, the relevant material is
（Impurity A）（Impurity B）
（Impurity C）（Impurity D）
In above-mentioned impurity, impurity A~B is degradation impurity, and C~D is process contaminants.
The beneficial effects of the invention are as follows：
The present invention can be efficiently separated naphcon and its relevant material, and separating degree is good, so as to effective
Control the quality of naphcon.The present invention method can simply, fast and accurately separation detection goes out naphcon
And its about material and associated potential impurity, and specificity is strong, high sensitivity, stability are good, favorable reproducibility, precision
Height, peak shape are good, the effective control that can be used in actual production.
（Four）Brief description of the drawings
The present invention is further illustrated below in conjunction with the accompanying drawings.
Fig. 1 is the chromatogram of the blank solution of embodiment 1.
Fig. 2 is the chromatogram of the mixed reference substance solution of embodiment 1.
Fig. 3 is the chromatogram of the naphcon test sample of embodiment 1.
Fig. 4 is the chromatogram of the mixed reference substance solution of embodiment 2.
Fig. 5 is the chromatogram of the naphcon need testing solution of embodiment 2.
Fig. 6 is the chromatogram of the mixed reference substance solution of embodiment 3.
Fig. 7 is the chromatogram of the naphcon need testing solution of embodiment 3.
Fig. 8 is the chromatogram of the mixed reference substance solution of embodiment 4.
Fig. 9 is the chromatogram of the naphcon need testing solution of embodiment 4.
Figure 10 is the mixed reference substance solution chromatogram of embodiment 5.
Figure 11 is the chromatogram of the naphcon need testing solution of embodiment 5.
（Five）Embodiment
Embodiment 1
（1）Testing conditions
Instrument：Waters e2695 high performance liquid chromatographs, 2998PDA detectors, Detection wavelength：280nm；
Chromatographic column：waters XBridge C18（250mm × 4.6mm, 5 μm）Chromatographic column；
Solvent：Mobile phase A：Octane sulfonate sodium solution（Perfluorooctane sulfonate 1.57g and potassium dihydrogen phosphate 1.7g are taken, with water dissolving simultaneously
1000ml is diluted to, adds triethylamine 5ml, with phosphorus acid for adjusting pH value to 2.8）；Mobile phase B：Acetonitrile；Mobile phase A and Mobile phase B body
Accumulating ratio is：80:20；
Flow velocity：1.0mL/min
Column temperature：30℃；
Sample size：20μL；
Linear gradient elution is carried out by table 1.
Table 1
（2）Detecting step
The preparation of mixed reference substance solution：D pairs of naphcon reference substance, impurity A, impurity B, impurity C and impurity are taken respectively
It is each appropriate according to product, it is accurately weighed, the solution that every 1ml contains 0.5 μ g is dissolved and is diluted to solvent, as mixed reference substance solution.
The preparation of need testing solution：Naphcon test sample about 25mg is taken, it is accurately weighed, put in 50ml measuring bottles, use
Solvent dissolves and is diluted to scale, shakes up, as need testing solution.Precision measures blank solution, mixed reference substance solution respectively
With each 20 μ L of need testing solution, liquid chromatograph is injected, chromatogram is recorded, sees Fig. 1, Fig. 2, Fig. 3；As a result show：In fig. 2,
Each peak is followed successively by naphcon（12.733min）, impurity A（13.565min）, impurity D（16.035min）, impurity B
（26.248min）, impurity C（46.616min）.
Embodiment 2
According to the similar detection method of embodiment 1, wherein, octane sulfonate sodium solution concentration replaces with 1.41g/L.It mixes control
The collection of illustrative plates of product is shown in Fig. 4, the chromatogram of test sample is shown in Fig. 5.
Embodiment 3
According to the similar detection method of embodiment 1, wherein, octane sulfonate sodium solution concentration replaces with 1.73g/L.It mixes control
The chromatogram of product is shown in Fig. 6, the chromatogram of test sample is shown in Fig. 7.
Embodiment 4
According to the similar detection method of embodiment 1, wherein, the concentration of potassium dihydrogen phosphate replaces with 1.53g/L.Its mixing pair
According to product collection of illustrative plates see Fig. 8, the collection of illustrative plates of test sample is shown in Fig. 9.
Embodiment 5
According to the similar detection method of embodiment 1, wherein, the concentration of potassium dihydrogen phosphate replaces with 1.87g/L.Its mixing pair
According to product solution collection of illustrative plates see Figure 10, the chromatogram of test sample is shown in Figure 11.
Reagent used in the present invention can be bought from the market.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (10)
1. a kind of naphcon and its detection method about material, it is characterised in that：It is enterprising in high performance liquid chromatograph
Row gradient elution, its chromatographic condition include：Chromatographic column is octadecylsilane chemically bonded silica chromatographic column, with octane sulfonate sodium solution
For mobile phase A, acetonitrile is Mobile phase B, and Detection wavelength is 275~285nm, 20-40 DEG C of column temperature, flow velocity：0.9-1.1mL/min,
Carry out gradient elution；Wherein mobile phase A compound method is：Perfluorooctane sulfonate and potassium dihydrogen phosphate are taken, is dissolved and is diluted to water
1000mL, add triethylamine 5mL, with phosphorus acid for adjusting pH value to 2.6-3.0.
2. naphcon according to claim 1 and its detection method about material, it is characterised in that：The ladder
Spending the process eluted is：In 0~20min, the volume ratio of mobile phase A and Mobile phase B is from 78:22 at the uniform velocity gradual changes are to 74:26；20~
In 32min, the volume ratio of mobile phase A and Mobile phase B is 74:26；In 32~60min, the volume ratio of mobile phase A and Mobile phase B
From 74:26 at the uniform velocity gradual changes are to 50:50；In 60~65min, the volume ratio of mobile phase A and Mobile phase B is 50:50；65~66min
Interior, the volume ratio of mobile phase A and Mobile phase B is from 50:50 at the uniform velocity gradual changes are to 78:22；In 66~80min, mobile phase A and mobile phase
B volume ratio is 78:22.
3. naphcon according to claim 1 and its detection method about material, it is characterised in that：Mobile phase
In A, the concentration of octane sulfonate sodium solution is 1.41g/L~1.73g/L.
4. the naphcon stated according to claim 3 and its detection method about material, it is characterised in that：The octane
The concentration of sodium sulfonate solution is 1.57g/L.
5. naphcon according to claim 1 and its detection method about material, it is characterised in that：Mobile phase
In A, the concentration of the solution of potassium dihydrogen phosphate is 1.53g/L~1.87g/L.
6. the naphcon stated according to claim 5 and its detection method about material, it is characterised in that：The phosphoric acid
The concentration of potassium dihydrogen is 1.7g/L.
7. naphcon according to claim 1 and its detection method about material, it is characterised in that：The color
The length of spectrum post is 250mm, and a diameter of 4.6mm, packing material size is 5 μm.
8. naphcon according to claim 1 and its detection method about material, it is characterised in that：The inspection
Survey wavelength is 280nm.
9. naphcon according to claim 1 and its detection method about material, it is characterised in that：The post
Temperature is 30 DEG C.
10. naphcon according to claim 1 and its detection method about material, it is characterised in that：It is described
Flow velocity is 1.0mL/min.
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| CN201710701060.XA CN107389826A (en) | 2017-08-16 | 2017-08-16 | A kind of naphcon and its detection method about material |
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| CN201710701060.XA CN107389826A (en) | 2017-08-16 | 2017-08-16 | A kind of naphcon and its detection method about material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956795A (en) * | 2018-04-20 | 2018-12-07 | 公安部物证鉴定中心 | Detection method for imidazolines drug in criminal investigation purpose biological fluid |
| CN116008439A (en) * | 2023-02-20 | 2023-04-25 | 山东绿叶制药有限公司 | Method for detecting impurities in 2, 6-dioxaspiro [4,5] decane compounds or salts thereof |
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| CN101196495A (en) * | 2006-12-06 | 2008-06-11 | 安军永 | Method for measuring content of triamcinolone acetonide chloromycetin solution |
| CN106344602A (en) * | 2016-08-29 | 2017-01-25 | 安徽艾珂尔制药有限公司 | Naphazoline hydrochloride, chlorphenamine maleate and vitamin B12 eyedrop compound preparation and preparation method thereof |
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2017
- 2017-08-16 CN CN201710701060.XA patent/CN107389826A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101196495A (en) * | 2006-12-06 | 2008-06-11 | 安军永 | Method for measuring content of triamcinolone acetonide chloromycetin solution |
| CN106344602A (en) * | 2016-08-29 | 2017-01-25 | 安徽艾珂尔制药有限公司 | Naphazoline hydrochloride, chlorphenamine maleate and vitamin B12 eyedrop compound preparation and preparation method thereof |
Non-Patent Citations (3)
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| EUROPEAN PHARMACOPOEIA: "Naphazolini hydrochloridum", 《EUROPEAN PHARMACOPOEIA 8.0》 * |
| 张晓平等: "高效液相色谱法测定盐酸萘甲唑啉含量", 《天津药学》 * |
| 袁宇琳等: "HPLC测定复方萘甲唑啉鼻喷剂中的有关物质", 《华西药学杂志》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108956795A (en) * | 2018-04-20 | 2018-12-07 | 公安部物证鉴定中心 | Detection method for imidazolines drug in criminal investigation purpose biological fluid |
| CN108956795B (en) * | 2018-04-20 | 2021-08-06 | 公安部物证鉴定中心 | Method for detecting imidazoline drugs in biological body fluid for criminal investigation |
| CN116008439A (en) * | 2023-02-20 | 2023-04-25 | 山东绿叶制药有限公司 | Method for detecting impurities in 2, 6-dioxaspiro [4,5] decane compounds or salts thereof |
| CN116008439B (en) * | 2023-02-20 | 2023-10-27 | 山东绿叶制药有限公司 | Method for detecting impurities in 2, 6-dioxaspiro [4,5] decane compounds or salts thereof |
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Application publication date: 20171124 |