CN104777122A - 11-alpha-hydroxycarvenone determination method - Google Patents
11-alpha-hydroxycarvenone determination method Download PDFInfo
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- CN104777122A CN104777122A CN201510137380.8A CN201510137380A CN104777122A CN 104777122 A CN104777122 A CN 104777122A CN 201510137380 A CN201510137380 A CN 201510137380A CN 104777122 A CN104777122 A CN 104777122A
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Abstract
The present invention discloses a 11-alpha-hydroxycarvenone determination method, which comprises: a, respectively weighing 5 mg, 10 mg, 20 mg, 30 mg and 40 mg of a standard substance, respectively transferring to 50 ml volumetric flasks, carrying out volume metering with methanol, and completely and uniformly mixing; b, turning on the power supply of an ultraviolet spectrophotometer, preheating the ultraviolet spectrophotometer for 30 min, and setting the determination wavelength as 280 nm; c, rinsing a cuvette with dehydrated ethanol, rinsing three times with deionized water, pouring a methanol solution to rinse again, adopting a methanol solution as a blank solution, and placing into a colorimetric pool to carry out zero calibration; and d, after completing the zero calibration, pouring out the methanol at the tested end, respectively pouring the prepared standard substance solutions with the series of concentrations, determining the absorbance values of the standard solutions at each concentration, recording the data, and generating the 11-alpha-hydroxycarvenone concentration measurement standard curve. With the determination method of the present invention, the determination time is shortened, and the work efficiency is increased.
Description
Technical field
The present invention relates to method for measurement of concentration application, particularly a kind of assay method of 11 alpha hydroxy-canrenone concentration.
Background technology
Canrenone is a kind of steroid hormone class cardiovascular drugs, and 11 alpha hydroxy-canrenones, as its derivant, play an important role in human body, it is compared with canrenone, there is the advantages such as spinoff is little, curative effect is high, and as the important medicine intermediate of eplerenone, have the significant market demand.
At present, the assay method of the concentration of 11 traditional alpha hydroxy-canrenones is mainly based on high performance liquid chromatography, and costly, and operating process is also more numerous and diverse, is very restricted in actual applications for the analytical instrument that its mensuration process uses.Because 11 alpha hydroxy-canrenones are only at the C of canrenone
11position is a many hydroxyl (-OH), extremely similar to canrenone in structure, therefore the two all can have obvious absorption at ultraviolet wavelength 280nm place.
Summary of the invention
For solving Problems existing in above-mentioned background technology, the object of the present invention is to provide a kind of assay method of 11 alpha hydroxy-canrenones, to reach shortening minute, the object of increasing work efficiency.
For achieving the above object, technical scheme of the present invention is as follows:
An assay method for 11 alpha hydroxy-canrenones, comprises the following steps:
A, accurately take the 11 alpha hydroxy-canrenone standard items of 5mg, 10mg, 20mg, 30mg, 40mg respectively, be transferred to 50ml volumetric flask respectively, use methanol constant volume respectively, fully mix, stand-by;
B, connection ultraviolet spectrophotometer power supply, open switch, and after making photometer preheating 30min, arranging its wavelength measured is 280nm;
C, cuvette absolute ethyl alcohol is rinsed one time, then use deionized water rinsing three times, then pour methanol solution rinse into one time, then, using methanol solution as blank solution, put into colorimetric pool and carry out school zero;
D, school zero are complete, methyl alcohol in test lead cuvette is poured out, pour the standard solution of 0.1mg/ml, 0.2mg/ml, 0.4mg/ml, 0.6mg/ml, 0.8mg/ml series concentration of above-mentioned preparation more respectively into, measure the absorbance of standard solution under each concentration, and record data, generate the typical curve of 11 alpha hydroxy-canrenone measurement of concetrations.
Pass through technique scheme, the assay method of a kind of 11 alpha hydroxy-canrenones provided by the invention, by adopting the concentration of determined by ultraviolet spectrophotometry 11 alpha hydroxy-canrenone, shorten minute, improve work efficiency, without the need to the instrument and equipment of costliness, the process measuring post analysis is also relatively simple, analysis result has higher accuracy and repeatability, is more suitable for applying more widely.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below.
Fig. 1 is the typical curve schematic diagram of the assay method of a kind of 11 alpha hydroxy-canrenones of the embodiment of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described.
The assay method of a kind of 11 alpha hydroxy-canrenones provided by the invention, as shown in Figure 1, comprises the following steps:
A, accurately take the 11 alpha hydroxy-canrenone standard items of 5mg, 10mg, 20mg, 30mg, 40mg respectively, be transferred to 50ml volumetric flask respectively, use methanol constant volume respectively, fully mix, stand-by;
B, connection ultraviolet spectrophotometer power supply, open switch, and after making photometer preheating 30min, arranging its wavelength measured is 280nm;
C, cuvette absolute ethyl alcohol is rinsed one time, then use deionized water rinsing three times, then pour methanol solution rinse into one time, then, using methanol solution as blank solution, put into colorimetric pool and carry out school zero;
D, school zero are complete, methyl alcohol in test lead cuvette is poured out, pour the standard solution of 0.1mg/ml, 0.2mg/ml, 0.4mg/ml, 0.6mg/ml, 0.8mg/ml series concentration of above-mentioned preparation more respectively into, measure the absorbance of standard solution under each concentration, and record data, generate the typical curve of 11 alpha hydroxy-canrenone measurement of concetrations.
Measure and terminate, cuvette is clean with deionized water rinsing, store under being placed in dry environment, keep the drying of colorimetric pool.
Principle of the present invention: 11 alpha hydroxy-canrenones are a kind of compounds containing cyclopentanoperhy drophenanthrene core, it is condensed by A, B, C, D tetra-rings and forms in chemical constitution, wherein A, B, C ring is hexatomic ring, D is five-membered ring, respectively there is an angular methyl at the usual A/B ring place of condensing and the C/D ring place of condensing, there is partial double bond in A ring and B ring, this structure makes it have very strong characteristic absorption at ultraviolet wavelength 280nm place, and the proportional relation of the concentration of uv absorption intensity and 11 alpha hydroxy-canrenones.
Adopt ultraviolet spectrophotometer, by measuring the absorbance of 11 alpha hydroxy-canrenone standard solutions of a series of concentration known at ultraviolet wavelength 280nm place, Criterion curve, thus the concentration computing formula determining 11 alpha hydroxy-canrenones.
The assay method of a kind of 11 alpha hydroxy-canrenones disclosed by the invention, by adopting the concentration of determined by ultraviolet spectrophotometry 11 alpha hydroxy-canrenone, shorten minute, improve work efficiency, without the need to the instrument and equipment of costliness, the process measuring post analysis is also relatively simple, and analysis result has higher accuracy and repeatability, is more suitable for applying more widely.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (1)
1. an assay method for 11 alpha hydroxy-canrenones, is characterized in that, comprises the following steps:
A, accurately take the 11 alpha hydroxy-canrenone standard items of 5mg, 10mg, 20mg, 30mg, 40mg respectively, be transferred to 50ml volumetric flask respectively, use methanol constant volume respectively, fully mix, stand-by;
B, connection ultraviolet spectrophotometer power supply, open switch, and after making photometer preheating 30min, arranging its wavelength measured is 280nm;
C, cuvette absolute ethyl alcohol is rinsed one time, then use deionized water rinsing three times, then pour methanol solution rinse into one time, then, using methanol solution as blank solution, put into colorimetric pool and carry out school zero;
D, school zero are complete, methyl alcohol in test lead cuvette is poured out, pour the standard solution of 0.1mg/ml, 0.2mg/ml, 0.4mg/ml, 0.6mg/ml, 0.8mg/ml series concentration of above-mentioned preparation more respectively into, measure the absorbance of standard solution under each concentration, and record data, generate the typical curve of 11 alpha hydroxy-canrenone measurement of concetrations.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1748740A (en) * | 2004-09-17 | 2006-03-22 | 王英锋 | Imature bitter orange total flavone and its preparing mthod for its preparation and quality control method |
| CN102232981A (en) * | 2010-04-29 | 2011-11-09 | 秦引林 | Determination method of content of radix serratulae total sterone |
| CN102608053A (en) * | 2012-02-23 | 2012-07-25 | 北京水泥厂有限责任公司 | Detection method for mineral oil in sludge |
| CN102866125A (en) * | 2012-09-21 | 2013-01-09 | 山西大学 | Method for rapidly and simply measuring sulfur dioxide |
| WO2014000834A1 (en) * | 2012-06-26 | 2014-01-03 | Curiosity Diagnostics Sp. Z O.O. | Method for performing quantitation assays |
-
2015
- 2015-03-26 CN CN201510137380.8A patent/CN104777122A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1748740A (en) * | 2004-09-17 | 2006-03-22 | 王英锋 | Imature bitter orange total flavone and its preparing mthod for its preparation and quality control method |
| CN102232981A (en) * | 2010-04-29 | 2011-11-09 | 秦引林 | Determination method of content of radix serratulae total sterone |
| CN102608053A (en) * | 2012-02-23 | 2012-07-25 | 北京水泥厂有限责任公司 | Detection method for mineral oil in sludge |
| WO2014000834A1 (en) * | 2012-06-26 | 2014-01-03 | Curiosity Diagnostics Sp. Z O.O. | Method for performing quantitation assays |
| CN102866125A (en) * | 2012-09-21 | 2013-01-09 | 山西大学 | Method for rapidly and simply measuring sulfur dioxide |
Non-Patent Citations (2)
| Title |
|---|
| 张云贵 等: "《生物化学实验指导》", 31 July 2013 * |
| 牟晓然: "赭曲霉制备心血管药物C(11)α羟基化坎利酮培养条件的研究", 《中国优秀硕士论文全文数据库 工程科技辑》 * |
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