CN108614044A - Assay method of the bronopol in relation to substance - Google Patents
Assay method of the bronopol in relation to substance Download PDFInfo
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- CN108614044A CN108614044A CN201810381315.3A CN201810381315A CN108614044A CN 108614044 A CN108614044 A CN 108614044A CN 201810381315 A CN201810381315 A CN 201810381315A CN 108614044 A CN108614044 A CN 108614044A
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- bronopol
- phosphoric acid
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- 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
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Abstract
The present invention relates to a kind of assay method of bronopol in relation to substance, take sample about 10mg, it sets in centrifuge tube, add mobile phase 100ml, whirlpool shakes 2 minutes, filtration, takes 10 μ l injection high performance liquid chromatographs, it is tested according to chromatographic condition below and measures content, 2 times of record chromatogram to main peak retention time；Chromatographic condition：Chromatographic column is RP ODS columns, and column temperature is 30 DEG C, and Detection wavelength 210nm, flow velocity 1.0ml/min, mobile phase is phosphoric acid water：Methanol=95:5.Its advantage is shown：The present invention provides a kind of HPLC analysis methods quickly, precisely detecting bronopol, provide a kind of method of the stability of research compound Pi Lebao powder, and bronopol detaches well with other decomposition products, and specificity is strong.The method of the present invention is used to study the stability of compound Pi Lebao powder, it may be determined that its pharmacological property to be convenient for the production practices in later stage.
Description
Technical field
The present invention relates to technical field of pharmaceuticals, specifically, being assay method of the bronopol in relation to substance.
Background technology
The bronopol entitled 2- bromo-2-nitro-1,3-propylene glycols of chemistry also known as bronopol, Bronopol, bronopol,
Antibacterial alcohol and Pi Lebao etc., English entitled 2-bromo-2-nitro-1,3-propanediol, external trade name
Bronopol.It is a kind of white or light yellow crystalline powder, 120~122 DEG C of fusing point, soluble easily in water, ethyl alcohol and propylene glycol
Isopolarity solvent is insoluble in the nonpolar solvents such as chloroform, acetone and benzene.It easily decomposes in pH=8 and high temperature, can send out under light illumination
Huang has corrosiveness to aluminium.Bronopol is a kind of bromo nitryl alcohols wide-spectrum bactericide, has very high bactericidal activity and very
It is low using concentration and wider pH use scopes, non-stimulated to human skin, without allergic reaction, being U.S. FDA approval makes
One of cosmetics preservative.Compared with other preservatives, bronopol is with efficient, dosage is few, cheap, compatibility
Well, the advantages that suitable pH ranges, good water solubility.
" compound Pi Lebao powder " (U.S. graceful II)
【Main component】Pi Lebao (bronopol), ferrous sulfate
【Pharmacological action】" compound Pi Lebao powder " (mechanism of action of U.S. graceful II) is that active constituent directly acts on cell membrane
The mercapto on surface, makes disulfide, and especially big protrusion is generated in cell wall, leads to cell wall rupture, outside content
Stream, mycelium are dead, spore inactivates, while this product also has astriction, promote aquatic animal wound healing.
【Indication】Be mainly used for preventing the fungus-caused aquatic animal disease such as water mo(u)ld (such as fish-egg is mouldy, fry, at
Fish and water mildew etc.).
Chinese patent literature CN104926661A, CN102850226A etc. discloses the preparation process of bronopol.It is Chinese special
Sharp document CN102293831A discloses a kind of compounding powder of prevention saprolegniasis of aquatic animals, by Chinese gall, rheum officinale, bromine nitre
Alcohol, dispersant constant weight percentage raw material be made.Chinese patent literature CN101708187A discloses a kind of for preventing
The dry powder formulations of saprolegniasis of aquatic animals：71-79% biochemical fulvic acids, 10-15% Sodium Metabisulfites, 10-15% bronopols.
Chinese patent literature CN102920715A discloses a kind of cultured freshwater fish nosomycosis pharmaceutical formulation：Sulfosalicylic acid 20-
35%, bronopol 8-20%, miconazole nitrate 2-5%, diatomite 55-70%.But about the related object of bronopol of the present invention
The assay method of matter yet there are no report.
Invention content
First purpose of the present invention is, for deficiency in the prior art, to provide a kind of survey of the bronopol in relation to substance
Determine method.
Second object of the present invention is to provide a kind of 4stability determination of compound Pi Lebao powder.
To realize above-mentioned first purpose, the technical solution adopted by the present invention is that：A kind of HPLC analysis methods of bronopol,
The analysis method includes the following steps：Bronopol 10mg is taken, is set in centrifuge tube, mobile phase 100ml, whirlpool is added to shake 2 points
Clock, filtration take 10 μ l injection high performance liquid chromatographs, are tested according to chromatographic condition below and measure content, record chromatogram is extremely
2 times of main peak retention time；Chromatographic condition：Chromatographic column is RP-ODS columns, the specifications of RP-ODS columns be 150mm × 4.6mm, 5 μm,
Column temperature is 30 DEG C, Detection wavelength 210nm, flow velocity 1.0ml/min, and mobile phase is phosphoric acid water：Methanol=95:5(V:V), phosphoric acid
Water is phosphoric acid：Water=1:1000.
A kind of HPLC analysis methods of compound Pi Lebao powder, the analysis method include the following steps：Compound skin is taken to find pleasure in
Precious powder 10mg, sets in centrifuge tube, and mobile phase 100ml, whirlpool is added to shake 2 minutes, filtration, takes 10 μ l injection high performance liquid chromatography
Instrument is tested according to chromatographic condition below and measures content, 2 times of record chromatogram to main peak retention time；Chromatographic condition：Chromatography
Column is RP-ODS columns, the specifications of RP-ODS columns be 150mm × 4.6mm, 5 μm, column temperature is 30 DEG C, Detection wavelength 210nm, flow velocity
1.0ml/min, mobile phase are phosphoric acid water：Methanol=95:5(V:V), phosphoric acid water is phosphoric acid：Water=1:1000.
The main component of the compound Pi Lebao powder is bronopol and ferrous sulfate.
To realize above-mentioned second purpose, the technical solution adopted by the present invention is that：A kind of bronopol method for analyzing stability,
The analysis method includes Oxidative demage experiment, heating failure test, alkali failure test, sour failure test.
Oxidative demage test method is：Bronopol 10mg is taken, 30% hydrogen peroxide 5mL is added, places 1h, takes out, adds flowing
The solution containing 5mg in every 1mL, upper HPLC is made in phase dilution.
Heating failure test method is：It takes bronopol appropriate, add flowing phased soln and is diluted in every 1mL containing 5mg's
Solution is set in 100 DEG C of water-baths, and 40min is heated, and is taken out, is put to room temperature, upper HPLC.
Alkali failure test method is：Bronopol 10mg is taken, adds 1mol/L sodium hydroxide 5mL, sets in hot bath, heating 1h takes
Go out, let cool, neutralized with 1mol/L hydrochloric acid solutions, adds flowing phase dilution that the solution containing 5mg in every 1mL, upper HPLC is made.
Sour failure test method is：Bronopol 10mg is taken, adds 1mol/L hydrochloric acid solution 5mL, sets in hot bath, heating 1h takes
Go out, let cool, pH value is adjusted with 1mol/L sodium hydroxides, adds flowing phase dilution that the solution containing 5mg in every 1mL, upper HPLC is made.
HPLC conditions are：Chromatographic column is RP-ODS columns, the specifications of RP-ODS columns be 150mm × 4.6mm, 5 μm, column temperature is 30
DEG C, Detection wavelength 210nm, flow velocity 1.0ml/min, mobile phase is phosphoric acid water：Methanol=95:5(V:V), phosphoric acid water is phosphoric acid：
Water=1:1000.
The invention has the advantages that：
1, the present invention provides a kind of HPLC analysis methods quickly, precisely detecting bronopol.
2, the present invention provides a kind of research " compound Pi Lebao on the basis of the HPLC analysis methods of aforementioned bronopol
The method of the stability of powder " (U.S. graceful II), bronopol detach well with other decomposition products, and specificity is strong.
3, the method for the present invention is used to study the stability of " compound Pi Lebao powder " (U.S. graceful II), it may be determined that its pharmacological property,
Convenient for the production practices in later stage.
Description of the drawings
Attached drawing 1 is unbroken system suitability solution chromatogram.
Attached drawing 2 is Oxidative demage bronopol chromatogram.
Attached drawing 3 is high temperature bronopol chromatogram.
Attached drawing 4 is that alkali destroys bronopol chromatogram.
Attached drawing 5 is that acid destroys bronopol chromatogram.
Specific implementation mode
It elaborates to specific implementation mode provided by the invention with reference to embodiment.
Because the principle active component in " compound Pi Lebao powder " (U.S. graceful II) prescription is bronopol, we establish utilization
The method of high effective liquid chromatography for measuring bronopol simultaneously studies its stability at different conditions.
Chromatographic condition：Chromatographic column is RP-ODS columns (150mm × 4.6mm, 5 μm), and column temperature is 30 DEG C, and Detection wavelength is
210nm, flow velocity 1.0ml/min, mobile phase are phosphoric acid water (phosphoric acid：Water=1:1000)：Methanol=95:5(V:V).
This product about 10mg is taken, is set in centrifuge tube, mobile phase 100ml, whirlpool is added to shake 2 minutes, filtration takes 10 μ l injections high
Effect liquid phase chromatogram instrument is tested according to chromatographic condition below and measures content, 2 times of record chromatogram to main peak retention time.For
It if any impurity peaks in test sample solution chromatogram, is calculated by peak area normalization method, single contaminant must not exceed 4.0%, impurity peaks face
Long-pending summation must not cross 6.0%.
Reference substance：
Bronopol reference substance：Purchased from Beijing Century AudioCodes Bioisystech Co., Ltd, German Dr.Ehrenstorfer, CAS
Number 52-51-7 (Water Content0.1%, Det.Purity98.5%, Tolerance/Uncertainty+/-
0.5%, Determined by Karl-Fischer Titration).
Test sample：
" compound Pi Lebao powder " (U.S. graceful II), Changsha Co., Ltd of Bai Te biotechnologies research institute provides.
It is prepared by solution
Test solution takes this product appropriate, adds mobile phase to be diluted in every 1mL containing about the solution of bronopol 0.1mg, supplies
Test sample solution.
It is appropriate that reference substance solution precision weighs bronopol reference substance, add flowing phased soln and be diluted in every 1mL containing about
The solution of 0.1mg bronopols, as a contrast product solution.
Embodiment 1 is not destroyed
Bronopol 10mg is taken, is set in centrifuge tube, mobile phase 100ml, whirlpool is added to shake 2 minutes, filtration takes 10 μ l injections high
Effect liquid phase chromatogram instrument is tested according to chromatographic condition below and measures content, 2 times of record chromatogram to main peak retention time.
Chromatographic condition：Chromatographic column is RP-ODS columns (150mm × 4.6mm, 5 μm), and column temperature is 30 DEG C, and Detection wavelength is
210nm, flow velocity 1.0ml/min, mobile phase are phosphoric acid water (phosphoric acid：Water=1:1000)：Methanol=95:5(V:V).
Unbroken system suitability solution chromatogram is shown in attached drawing 1.
2 Oxidative demage of embodiment is tested
Bronopol 10mg is taken, 30% hydrogen peroxide 5mL is added, places 1h, is taken out, adds flowing phase dilution to be made in every 1mL and contains
The solution of 5mg, upper HPLC.
Chromatographic condition：Chromatographic column is RP-ODS columns (150mm × 4.6mm, 5 μm), and column temperature is 30 DEG C, and Detection wavelength is
210nm, flow velocity 1.0ml/min, mobile phase are phosphoric acid water (phosphoric acid：Water=1:1000)：Methanol=95:5(V:V).
Oxidative demage bronopol chromatogram is shown in attached drawing 2.It can be seen that this method can efficiently separate bronopol and its oxidized
The catabolite generated after destruction, bronopol peak detach well with other decomposition product peaks, illustrate that this law specificity is strong.
Embodiment 3 heats failure test
It takes bronopol appropriate, add flowing phased soln and is diluted to the solution containing 5mg in every 1mL, set in 100 DEG C of water-baths,
40min is heated, takes out, puts to room temperature.Upper HPLC.
Chromatographic condition：Chromatographic column is RP-ODS columns (150mm × 4.6mm, 5 μm), and column temperature is 30 DEG C, and Detection wavelength is
210nm, flow velocity 1.0ml/min, mobile phase are phosphoric acid water (phosphoric acid：Water=1:1000)：Methanol=95:5(V:V).
High temperature bronopol chromatogram is shown in attached drawing 3.It can be seen that this method can efficiently separate bronopol and its through high temperature
The catabolite generated after destruction, bronopol peak detach well with other decomposition product peaks, illustrate that this law specificity is strong.
4 alkali failure test of embodiment
Bronopol 10mg is taken, adds 1mol/L sodium hydroxide 5mL, sets in hot bath, heating 1h takes out, and lets cool, uses 1mol/L
Hydrochloric acid solution neutralizes, and adds flowing phase dilution that the solution containing 5mg in every 1mL, upper HPLC is made.
Chromatographic condition：Chromatographic column is RP-ODS columns (150mm × 4.6mm, 5 μm), and column temperature is 30 DEG C, and Detection wavelength is
210nm, flow velocity 1.0ml/min, mobile phase are phosphoric acid water (phosphoric acid：Water=1:1000)：Methanol=95:5(V:V).
Alkali destroys bronopol chromatogram and sees attached drawing 4.It can be seen that this method can efficiently separate bronopol and its be destroyed through alkali
The catabolite generated afterwards, bronopol peak detach well with other decomposition product peaks, illustrate that this law specificity is strong.
The sour failure test of embodiment 5
Bronopol 10mg is taken, adds 1mol/L hydrochloric acid solution 5mL, sets in hot bath, heating 1h takes out, and lets cool, uses 1mol/L
Sodium hydroxide adjusts pH value, adds flowing phase dilution that the solution containing 5mg in every 1mL, upper HPLC is made.
Chromatographic condition：Chromatographic column is RP-ODS columns (150mm × 4.6mm, 5 μm), and column temperature is 30 DEG C, and Detection wavelength is
210nm, flow velocity 1.0ml/min, mobile phase are phosphoric acid water (phosphoric acid：Water=1:1000)：Methanol=95:5(V:V).
Acid destroys bronopol chromatogram and sees attached drawing 5.It can be seen that this method can efficiently separate bronopol and its be destroyed through acid
The catabolite generated afterwards, bronopol peak detach well with other decomposition product peaks, illustrate that this law specificity is strong.
6 compound Pi Lebao powder stability analyses of embodiment
Compound Pi Lebao powder 10mg are taken, are set in centrifuge tube, mobile phase 100ml, whirlpool is added to shake 2 minutes, filtration takes 10 μ l
High performance liquid chromatograph is injected, is tested according to chromatographic condition below and measures content.
Chromatographic condition：Chromatographic column is RP-ODS columns (150mm × 4.6mm, 5 μm), and column temperature is 30 DEG C, and Detection wavelength is
210nm, flow velocity 1.0ml/min, mobile phase are phosphoric acid water (phosphoric acid：Water=1:1000)：Methanol=95:5(V:V).
The above method is used for compound Pi Lebao powder stability analyses, quickly, precisely, is highly convenient for the life of compound Pi Lebao powder
Production practice.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member, under the premise of not departing from the method for the present invention, can also make several improvement and supplement, these are improved and supplement also should be regarded as
Protection scope of the present invention.
Claims (9)
1. a kind of HPLC analysis methods of bronopol, which is characterized in that the analysis method includes the following steps：Take bronopol
10mg is set in centrifuge tube, and mobile phase 100ml, whirlpool is added to shake 2 minutes, filtration, is taken 10 μ l injection high performance liquid chromatographs, is pressed
It is tested according to chromatographic condition below and measures content, 2 times of record chromatogram to main peak retention time；Chromatographic condition：Chromatographic column is
RP-ODS columns, the specifications of RP-ODS columns be 150mm × 4.6mm, 5 μm, column temperature is 30 DEG C, Detection wavelength 210nm, flow velocity
1.0ml/min, mobile phase are phosphoric acid water：Methanol=95:5(V:V), phosphoric acid water is phosphoric acid：Water=1:1000.
2. a kind of HPLC analysis methods of compound Pi Lebao powder, which is characterized in that the analysis method includes the following steps：It takes
Compound Pi Lebao powder 10mg, set in centrifuge tube, and mobile phase 100ml, whirlpool is added to shake 2 minutes, and filtration takes 10 μ l to inject efficient liquid
Chromatography is tested according to chromatographic condition below and measures content, 2 times of record chromatogram to main peak retention time；Chromatostrip
Part：Chromatographic column is RP-ODS columns, the specifications of RP-ODS columns be 150mm × 4.6mm, 5 μm, column temperature is 30 DEG C, and Detection wavelength is
210nm, flow velocity 1.0ml/min, mobile phase are phosphoric acid water：Methanol=95:5(V:V), phosphoric acid water is phosphoric acid：Water=1:1000.
3. analysis method according to claim 2, which is characterized in that the main component of the compound Pi Lebao powder is bromine
Nitre alcohol and ferrous sulfate.
4. a kind of bronopol method for analyzing stability, which is characterized in that the analysis method includes Oxidative demage experiment, heating
Failure test, alkali failure test, sour failure test.
5. analysis method according to claim 4, which is characterized in that Oxidative demage test method is：Bronopol 10mg is taken,
Add 30% hydrogen peroxide 5mL, place 1h, take out, adds flowing phase dilution that the solution containing 5mg in every 1mL, upper HPLC is made.
6. analysis method according to claim 4, which is characterized in that heating failure test method is：Take bronopol appropriate,
Add flowing phased soln and be diluted to the solution containing 5mg in every 1mL, set in 100 DEG C of water-baths, heat 40min, takes out, put to room
Temperature, upper HPLC.
7. analysis method according to claim 4, which is characterized in that alkali failure test method is：Bronopol 10mg is taken, is added
1mol/L sodium hydroxide 5mL, set in hot bath, and heating 1h takes out, and lets cool, and is neutralized with 1mol/L hydrochloric acid solutions, adds mobile phase dilute
It releases and the solution containing 5mg in every 1mL, upper HPLC is made.
8. analysis method according to claim 4, which is characterized in that sour failure test method is：Bronopol 10mg is taken, is added
1mol/L hydrochloric acid solution 5mL, set in hot bath, and heating 1h takes out, and lets cool, and adjust pH value with 1mol/L sodium hydroxides, add flowing
The solution containing 5mg in every 1mL, upper HPLC is made in phase dilution.
9. according to any analysis method of claim 5~8, which is characterized in that HPLC conditions are：Chromatographic column is RP-ODS
Column, the specifications of RP-ODS columns be 150mm × 4.6mm, 5 μm, column temperature is 30 DEG C, Detection wavelength 210nm, flow velocity 1.0ml/min,
Mobile phase is phosphoric acid water：Methanol=95:5(V:V), phosphoric acid water is phosphoric acid：Water=1:1000.
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| CN201810381315.3A CN108614044A (en) | 2018-04-25 | 2018-04-25 | Assay method of the bronopol in relation to substance |
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| CN201810381315.3A CN108614044A (en) | 2018-04-25 | 2018-04-25 | Assay method of the bronopol in relation to substance |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009107133A1 (en) * | 2008-02-28 | 2009-09-03 | Bromine Compounds Ltd. | A process for the preparation of bronopol |
| WO2010141711A1 (en) * | 2009-06-03 | 2010-12-09 | Ex-Tek, Llc | Skin treatment compositions |
| KR101544049B1 (en) * | 2013-10-25 | 2015-08-19 | 경상대학교산학협력단 | Compositions for preventing and curing Scuticocilliatosis scutica in a cultivated flounder |
| CN104926661A (en) * | 2015-05-27 | 2015-09-23 | 天津市职业大学 | Synthetic method for bronopol |
| CN106631813A (en) * | 2016-12-22 | 2017-05-10 | 河北美邦工程科技股份有限公司 | Bronopol refining process |
-
2018
- 2018-04-25 CN CN201810381315.3A patent/CN108614044A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009107133A1 (en) * | 2008-02-28 | 2009-09-03 | Bromine Compounds Ltd. | A process for the preparation of bronopol |
| CN103396317A (en) * | 2008-02-28 | 2013-11-20 | 溴化合物有限公司 | Process for preparation of bronopol |
| WO2010141711A1 (en) * | 2009-06-03 | 2010-12-09 | Ex-Tek, Llc | Skin treatment compositions |
| KR101544049B1 (en) * | 2013-10-25 | 2015-08-19 | 경상대학교산학협력단 | Compositions for preventing and curing Scuticocilliatosis scutica in a cultivated flounder |
| CN104926661A (en) * | 2015-05-27 | 2015-09-23 | 天津市职业大学 | Synthetic method for bronopol |
| CN106631813A (en) * | 2016-12-22 | 2017-05-10 | 河北美邦工程科技股份有限公司 | Bronopol refining process |
Non-Patent Citations (6)
| Title |
|---|
| H.Z.LIAN等: "A study on the stability of bronopol in bronopol lotion by ion-paired reversed-phase high performance liquid chromatography", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
| 成海平: "杂质检查分析方法建立过程中破坏性试验的意义和存在的问题分析", 《中国新药杂志》 * |
| 梁赤周等: "20%溴硝醇可湿性粉剂高效液相色谱分析方法研究", 《农药科学与管理》 * |
| 由亚宁等: "卡泊三醇有关物质测定方法研究及原料稳定性考察", 《中国药物警戒》 * |
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