CN111122483A - Method for measuring content of chlorphenesin by ultraviolet spectrophotometry - Google Patents
Method for measuring content of chlorphenesin by ultraviolet spectrophotometry Download PDFInfo
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- CN111122483A CN111122483A CN201911393547.1A CN201911393547A CN111122483A CN 111122483 A CN111122483 A CN 111122483A CN 201911393547 A CN201911393547 A CN 201911393547A CN 111122483 A CN111122483 A CN 111122483A
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- MXOAEAUPQDYUQM-QMMMGPOBSA-N (S)-chlorphenesin Chemical compound OC[C@H](O)COC1=CC=C(Cl)C=C1 MXOAEAUPQDYUQM-QMMMGPOBSA-N 0.000 title claims abstract description 53
- 229960003993 chlorphenesin Drugs 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000002798 spectrophotometry method Methods 0.000 title claims abstract description 13
- JGJLWPGRMCADHB-UHFFFAOYSA-N hypobromite Inorganic materials Br[O-] JGJLWPGRMCADHB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000031700 light absorption Effects 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 19
- 239000000523 sample Substances 0.000 claims description 12
- 239000012488 sample solution Substances 0.000 claims description 10
- 239000011550 stock solution Substances 0.000 claims description 8
- 239000012086 standard solution Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000012417 linear regression Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000003556 assay Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 1
- ISPYQTSUDJAMAB-UHFFFAOYSA-N 2-chlorophenol Chemical compound OC1=CC=CC=C1Cl ISPYQTSUDJAMAB-UHFFFAOYSA-N 0.000 abstract 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 abstract 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 abstract 1
- 229910052794 bromium Inorganic materials 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000002835 absorbance Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- WXNZTHHGJRFXKQ-UHFFFAOYSA-N 4-chlorophenol Chemical compound OC1=CC=C(Cl)C=C1 WXNZTHHGJRFXKQ-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 241000224526 Trichomonas Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000000843 anti-fungal effect Effects 0.000 description 1
- 229940121375 antifungal agent Drugs 0.000 description 1
- 238000005251 capillar electrophoresis Methods 0.000 description 1
- MXOAEAUPQDYUQM-UHFFFAOYSA-N chlorphenesin Chemical compound OCC(O)COC1=CC=C(Cl)C=C1 MXOAEAUPQDYUQM-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000002124 endocrine Effects 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- -1 nipagin ester Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004809 thin layer chromatography Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
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- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Pathology (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Molecular Biology (AREA)
- Biomedical Technology (AREA)
- Engineering & Computer Science (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
A method for measuring the content of chlorphenesin by ultraviolet spectrophotometry is characterized in that bromine water is added to eliminate the interference of chlorphenesin to chlorophenol, and Na is dripped2S2O3Removing excessive bromine from the solution, filtering the solution by filter paper, measuring the light absorption value of the obtained filtrate at 280nm, and calculating the content of chlorphenesin according to a standard curve. The method can quickly and accurately detect the content of the chlorphenesin, eliminates the influence on the chlorophenol, has simple steps, low instrument requirement and good accuracy and repeatability, and can be used as a method for determining chlorphenesin in industrial production.
Description
Technical Field
The invention belongs to the technical field of analysis and detection, and particularly relates to a method for determining the content of chlorphenesin by using an ultraviolet spectrophotometry.
Background
Chlorphenesin, chemical name 3- (4-chlorophenoxy) -1, 2-propanediol, white crystalline or amorphous powder. In the aspect of medicine, chlorphenesin belongs to antifungal medicines, is suitable for resisting diseases of fungi, bacteria, vaginal mold and trichomonas, and has a plurality of pharmaceutical dosage forms. In the aspect of cosmetics, chlorphenesin can effectively resist gram-positive and gram-negative bacteria and keep the safety and stability of the product. At present, the commonly used cosmetic preservatives on the market are of the nipagin ester type, and European Union researches report that the preservatives can cause endocrine disturbance and have great harm to women. In recent years, chlorphenesin, which is highly safe and effective, has attracted much attention.
At present, methods for detecting chlorphenesin are high performance liquid chromatography, thin layer chromatography, capillary electrophoresis and the like. The most common and effective method is high performance liquid chromatography, which is accurate and feasible, and has the disadvantages of expensive chromatograph and high measuring cost.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a method for measuring the content of chlorphenesin by using an ultraviolet spectrophotometry. The chlorphenesin is simply, conveniently and accurately measured by adopting an ultraviolet spectrophotometry, and the method has high precision, good reproducibility and high reliability of a detection result.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for measuring the content of chlorphenesin by using an ultraviolet spectrophotometry is characterized by comprising the following steps:
1) establishing a standard curve:
accurately weighing chlorphenesin standard substance, dissolving the chlorphenesin standard substance in methanol to prepare chlorphenesin stock solution, accurately transferring chlorphenesin stock solution with different volumes into a volumetric flask, adding 2mL of bromine water, shaking up to enable the solution to be light yellow, and then dropwise adding Na with the concentration of 5-10 g/L2S2O3Adding methanol to a constant volume until the color of the solution is colorless, measuring the light absorption value at 280nm, and drawing a standard curve to obtain a linear regression equation;
y＝1.987x-0.006，R2＝0.999，
wherein x is the concentration of chlorphenesin and y is the light absorption value;
2) sample handling and assay:
accurately weighing a sample in a beaker, adding 2mL of bromine water, shaking up to enable the solution to be light yellow in color and generate fine precipitates, and then dropwise adding Na with the concentration of 5-10 g/L2S2O3Filtering the solution with filter paper until the solution is colorless, transferring the filtrate into a volumetric flask, adding methanol to constant volume, and measuring the light absorption value at 280 nm;
3) according to the light absorption value of the sample solution and a linear regression equation, the concentration C of the chlorphenesin in the sample solution can be calculated;
content of chlorphenesin in the sample:
in the above formula:
c, the concentration of chlorphenesin in the sample solution, g/L;
v is the volume of sample solution, mL;
m is sample mass, g.
The volume of the chlorphenesin stock solution is 0, 0.5, 1.0, 1.5, 2.0, 2.5, 3.0 and 4.0 mL.
The aperture of the filter paper in the step (2) is 5 μm.
The concentration range of the appropriate chlorphenesin standard solution for drawing the standard curve is below 0.5 g/L.
The concentration of the chlorphenesin in the sample solution is below 0.4g/L, which is suitable for measurement.
Compared with the prior art, the invention has the following advantages:
(1) the method adopts the spectrophotometry for measuring the content of the chlorphenesin for the first time, and is simple, convenient and easy to operate and high in analysis speed. The p-chlorophenol and chlorphenesin both have ultraviolet absorption at 280nm, the p-chlorophenol is precipitated by adding bromine water, the solution is changed from colorless to light yellow by excessive bromine water, and the solution is drippedAdding Na2S2O3The solution can remove the excess bromine water, and simultaneously, the color of the solution is changed back to colorless, and the solution can be directly measured after being filtered.
(2) The method has high precision, good reproducibility and high reliability of detection results.
(3) The cost is relatively low by adopting an ultraviolet spectrophotometry.
Drawings
FIG. 1 is a standard curve diagram of absorbance versus concentration of chlorphenesin at 280 nm.
Detailed Description
The invention will be further described with reference to the accompanying drawings, but the invention is not limited to the following examples.
Instruments and reagents
752N ultraviolet-visible spectrophotometer, 1cm quartz cuvette, analytical balance. Bromine water (analytically pure), Na2S2O3(analytical reagent)
Establishing a standard curve
Preparing a chlorphenesin standard solution: accurately weighing 0.5000g of chlorphenesin standard, dissolving the standard with methanol, transferring the solution to a 100mL volumetric flask, and fixing the volume to the scale to obtain 5g/L chlorphenesin stock solution. Respectively adding 0, 0.5, 1.0, 1.5, 2.0, 2.5, 3.0 and 4.0mL of chlorphenesin stock solution into a series of 50mL volumetric flasks, respectively adding 2mL of bromine water, stirring uniformly, dropwise adding 5g/LNa2S2O3Adding methanol until the solution is colorless, and adding methanol to a constant volume of 50mL to obtain standard solutions with concentrations of 0.05g/L, 0.1g/L, 0.15g/L, 0.2g/L, 0.25g/L, 0.3g/L and 0.4 g/L. Absorbance at 280nm was measured to obtain a standard curve, as shown in FIG. 1. The regression equation is that y is 1.987x-0.006, R2Where x is the concentration of chlorphenesin and y is the absorbance, 0.999.
Sample processing and assay
Accurately weighing a parallel sample 1(0.0100g) and a parallel sample 1' (0.0115g) in a beaker, respectively adding 2mL of bromine water, shaking up, and then dropwise adding 5g/LNa2S2O3The solution was allowed to stand until the solution was colorless. Filtering with 5 μm filter paperThe filter flask is washed by alcohol for several times, the filtrate is placed in a volumetric flask, methanol is added to the volumetric flask to achieve a constant volume of 50mL, the absorbance values measured at 280nm are respectively 0.388 and 0.446, and the contents of the chlorphenesin in the sample are calculated to be 99.14 percent and 98.90 percent, and the average content is 99.02 percent.
Precision test
Taking 0.4g/L chlorphenesin standard solution, measuring the light absorption value at 280nm, continuously measuring for 6 times, and calculating the relative standard deviation to be 1.752%.
Recovery rate of added standard
And respectively adding known-content chlorphenesin samples into chlorphenesin standard solutions, measuring according to the method, calculating the recovery rate, and obtaining the result shown in the standard recovery rate test in the table 1.
TABLE 1
Comparative test
Parallel 1 and parallel 1' were subjected to liquid chromatography analysis, respectively. The results are shown in Table 2 for comparison of the present invention with chromatography.
TABLE 2
As can be seen from tables 1 and 2, the results obtained by the method of the present invention are relatively stable and are relatively close to those obtained by chromatography. Therefore, the method for determining the content of the chlorphenesin by using the ultraviolet spectrophotometry can be applied to the analysis and detection of the chlorphenesin.
Claims (5)
1. A method for measuring the content of chlorphenesin by using an ultraviolet spectrophotometry is characterized by comprising the following steps:
1) establishing a standard curve:
accurately weighing chlorphenesinDissolving a standard substance with methanol to prepare a chlorphenesin stock solution, accurately transferring the chlorphenesin stock solutions with different volumes into a volumetric flask, adding 2mL of bromine water, shaking up, enabling the solution to be light yellow, and then dropwise adding Na with the concentration of 5-10 g/L2S2O3Adding methanol to a constant volume until the color of the solution is colorless, measuring the light absorption value at 280nm, and drawing a standard curve to obtain a linear regression equation;
y＝1.987x-0.006，R2＝0.999，
wherein x is the concentration of chlorphenesin and y is the light absorption value;
2) sample handling and assay:
accurately weighing a sample in a beaker, adding 2mL of bromine water, shaking up to enable the solution to be light yellow in color and generate fine precipitates, and then dropwise adding Na with the concentration of 5-10 g/L2S2O3Filtering the solution with filter paper until the solution is colorless, transferring the filtrate into a volumetric flask, adding methanol to constant volume, and measuring the light absorption value at 280 nm;
3) according to the light absorption value of the sample solution and a linear regression equation, the concentration C of the chlorphenesin in the sample solution can be calculated;
content of chlorphenesin in the sample:
in the above formula:
c, the concentration of chlorphenesin in the sample solution, g/L;
v is the volume of sample solution, mL;
m is sample mass, g.
2. The method as claimed in claim 1, wherein the volume of the stock solution of chlorphenesin is 0, 0.5, 1.0, 1.5, 2.0, 2.5, 3.0, 4.0 mL.
3. The method for measuring the content of chlorphenesin by ultraviolet spectrophotometry as claimed in claim 1, wherein the filter paper in step (2) has a pore size of 5 μm.
4. The method for measuring the content of chlorphenesin by ultraviolet spectrophotometry as claimed in claim 1, wherein the concentration range of the proper chlorphenesin standard solution for drawing the standard curve is below 0.5 g/L.
5. The method as claimed in claim 1, wherein the concentration of chlorphenesin in the sample solution is 0.4g/L or less, which is suitable for measurement.
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| CN201911393547.1A CN111122483A (en) | 2019-12-30 | 2019-12-30 | Method for measuring content of chlorphenesin by ultraviolet spectrophotometry |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108440253A (en) * | 2018-05-09 | 2018-08-24 | 广西大学 | A kind of method of green high-efficient selectivity synthesis Chlorphenesin |
| CN109856289A (en) * | 2019-04-02 | 2019-06-07 | 义乌市产品(商品)质量监督检验研究院 | The liquid chromatography detecting method of Chlorphenesin in a kind of toy material |
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- 2019-12-30 CN CN201911393547.1A patent/CN111122483A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108440253A (en) * | 2018-05-09 | 2018-08-24 | 广西大学 | A kind of method of green high-efficient selectivity synthesis Chlorphenesin |
| CN109856289A (en) * | 2019-04-02 | 2019-06-07 | 义乌市产品(商品)质量监督检验研究院 | The liquid chromatography detecting method of Chlorphenesin in a kind of toy material |
Non-Patent Citations (2)
| Title |
|---|
| 朱会卷: "高效液相色谱分析化妆品中的防腐剂氯苯甘醚", 《色谱》 * |
| 高清芳等: "《现代临床药学》", 31 March 1997 * |
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Address after: No.61 Xiyan Road, Xi'an City, Shaanxi Province 710054 Applicant after: Shaanxi Chemical Research Institute Co.,Ltd. Address before: No.61 Xiyan Road, Xi'an City, Shaanxi Province 710054 Applicant before: SHAANXI RESEARCH DESIGN INSTITUTE OF PETROLEUM CHEMICAL INDUSTRY |
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Application publication date: 20200508 |