CN108107136B - Method for detecting content of trimethylphenol in 2, 5-dimethylphenol by high performance liquid chromatography - Google Patents
Method for detecting content of trimethylphenol in 2, 5-dimethylphenol by high performance liquid chromatography Download PDFInfo
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- CN108107136B CN108107136B CN201711342939.6A CN201711342939A CN108107136B CN 108107136 B CN108107136 B CN 108107136B CN 201711342939 A CN201711342939 A CN 201711342939A CN 108107136 B CN108107136 B CN 108107136B
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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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
- G01N30/86—Signal analysis
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
- G01N30/8634—Peak quality criteria
Abstract
The invention belongs to the technical field of chemical raw material monomer detection and analysis, and provides a method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by using a high performance liquid chromatography, which comprises the following steps: adopting a C18 liquid chromatographic column and an ultraviolet detector; the organic phase-water phase is taken as a mobile phase, the flow rate of the mobile phase is 1mL/min, the detection wavelength is 276nm, the column temperature is 30 ℃, and the sample injection amount is 20 mu L. The method is suitable for detecting trace amount of trimethylphenol monomer, can quickly and accurately quantify trimethylphenol isomer, has good separation degree and can realize the detection purpose.
Description
Technical Field
The invention belongs to the technical field of chemical raw material monomer detection and analysis, and particularly relates to a method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by using a high performance liquid chromatography.
Background
Trimethylphenol is used as a disproportionation product in the production of 2, 5-dimethylphenol, and has great influence on the yield and quality of products in the synthesis of 2, 5-dimethylphenol. Therefore, during the synthesis of 2, 5-dimethylphenol, it is necessary to monitor the isomers of trimethylphenol.
At present, the detection method of 2, 5-dimethylphenol mainly comprises the following steps: the content of 2, 5-dimethylphenol is detected by gas chromatography, and the method has the defects that trimethylphenol is not detected; or methanol-water is used as a mobile phase to detect the content of trimethylphenol in the 2, 5-dimethylphenol, but the method cannot accurately and independently detect the trimethylphenol isomer.
Due to the problems in the prior art, a test method for detecting trimethylphenol with good separation degree is urgently needed for monitoring the synthesis process of 2, 5-dimethylphenol.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by using a high performance liquid chromatography, the method is suitable for detecting a trace amount of trimethylphenol monomer, can quickly and accurately quantify the trimethylphenol isomer, has good separation degree and can realize the detection purpose.
In order to achieve the above purpose, the solution adopted by the invention is as follows:
a method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by high performance liquid chromatography comprises the following chromatographic conditions: adopting a C18 liquid chromatographic column and an ultraviolet detector; an organic phase-water phase is taken as a mobile phase, the flow rate of the mobile phase is 1mL/min, the detection wavelength is 276nm, the column temperature is 30 ℃, and the sample injection amount is 20 mu L.
The method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by the high performance liquid chromatography provided by the invention has the beneficial effects that:
the method for detecting the content of the trimethylphenol isomer monomer by the high performance liquid chromatography provided by the invention comprises the steps of injecting a prepared sample solution into a C18 liquid chromatographic column, separating by the chromatographic column, controlling chromatographic conditions, and sequentially flowing chemical components in a sample out of the chromatographic column according to polarity and displaying the chemical components on a chromatogram in a chromatographic peak mode; and then substituting the peak area of the trimethylphenol isomer monomer into a linear equation to calculate the content of the trimethylphenol isomer monomer in the 2, 5-dimethylphenol sample.
The method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by the high performance liquid chromatography provided by the invention can realize accurate quantification, thereby achieving the control of product quality. Due to the adoption of the high performance liquid chromatograph and the synergistic cooperation between chromatographic conditions provided by the invention, the separation accuracy of trimethyl isomers is further increased, and the content of each trimethylphenol can be accurately quantified.
Drawings
FIG. 1 is a chromatogram of a 2, 5-dimethylphenol product provided in inventive Experimental example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following describes a method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by high performance liquid chromatography.
A method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by high performance liquid chromatography comprises the following steps:
(1) weighing a standard substance containing trimethylphenol, dissolving the standard substance in a volumetric flask by using pure methanol, fixing the volume, shaking up, then separating liquid, diluting by using a mobile phase, fixing the volume and shaking up to prepare a test standard substance solution.
It should be noted that the trimethylphenol in this example includes 2,4, 5-trimethylphenol and 2,3, 5-trimethylphenol.
In view of cost reduction, it is preferable to use methanol as the solvent from the viewpoint of price.
Further, in the present embodiment, the mobile phase is preferably an organic phase-aqueous phase. Wherein, in order to separate different trimethylphenols, the organic phase preferably comprises acetonitrile or methanol; more preferably, the organic phase is acetonitrile and, using methanol, there is a separation between the two trimethylphenols, but the degree of separation is poorer than with acetonitrile. The aqueous phase comprises pure water-glacial acetic acid, i.e. an aqueous solution of glacial acetic acid. For more precise separation, the concentration of the aqueous phase is preferably 2 to 3mL/L, more preferably 2 mL/L; when the column efficiency is decreased and the degree of separation between trimethylphenol isomers is deteriorated, the concentration of glacial acetic acid may be slightly increased at this time.
In this example, in order to achieve the best separation effect and to make the determination of the content of trimethylphenol isomers more accurate, it is preferable that the volume ratio of the organic phase to the aqueous phase is 40: 60.
(2) Weighing a sample containing trimethylphenol, dissolving the sample in a volumetric flask by using a mobile phase, fixing the volume, shaking up and filtering to prepare a sample solution.
(3) And (3) respectively injecting the test sample solution and the test sample solution into a high performance liquid chromatograph, and performing high performance liquid chromatography analysis according to chromatographic conditions.
Specifically, in step (3): firstly, taking a test sample solution, and diluting the test sample solution by 2 times, 4 times, 6 times and 10 times step by step to obtain 5 standard solutions with different concentrations; the 5 standard solutions of different concentrations were analyzed by high performance liquid chromatography as provided herein.
In this example, the chromatographic conditions used include: adopting a C18 liquid chromatographic column and an ultraviolet detector; the flow rate of the mobile phase is 1mL/min, the detection wavelength is 276nm, the column temperature is 30 ℃, and the sample injection amount is 20 mu L; preferably, the stationary phase of the C18 liquid chromatography column is octadecylsilane chemically bonded silica.
By adopting the chromatographic conditions, the parameters can be cooperated and synergized, so that the separation accuracy of trimethyl isomers is further increased, and the content of each trimethylphenol can be accurately quantified.
And then, taking the concentration of the trimethylphenol as a horizontal coordinate and the peak area as a vertical coordinate to prepare a standard curve to obtain a linear equation of the trimethylphenol.
And then substituting the peak area of the trimethylphenol detected by the high performance liquid chromatography of the sample solution to be tested into the linear equation, and accurately calculating to obtain the content of the 2,4, 5-trimethylphenol or the 2,3, 5-trimethylphenol in the 2, 5-dimethylphenol product or the intermediate sample in the synthesis process of the product.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by using a high performance liquid chromatography, which comprises the following steps:
test apparatus and conditions for detection:
shimadzu LC-10 ultra-high performance liquid chromatograph with ultraviolet detector; a chromatographic column: c18 column (4.6 mm. times.250 mm. times.5 um); mobile phase: the volume ratio of organic phase to aqueous phase was 40:60, isocratic elution; wherein the organic phase is acetonitrile, and the water phase is 2mL/L glacial acetic acid aqueous solution; flow rate: 1 mL/min; detection wavelength: 276 nm; column temperature: 30 ℃; sample introduction amount: 20 μ L.
Testing steps of detection:
(1) accurately weighing about 10mg of 2,4, 5-trimethylphenol standard sample, 10mg of 2, 5-dimethylphenol reference sample and 10mg of 2,3, 5-trimethylphenol standard sample in a 25mL volumetric flask, dissolving with methanol, fixing the volume, and shaking up to prepare a stock solution of a test standard solution; taking 1.0mL of standard mother liquor to a 100mL volumetric flask, fixing the volume by using a mobile phase, shaking up, and preparing a test sample solution;
(2) weighing 0.15g of 2, 5-dimethylphenol sample, dissolving the sample in a 50mL volumetric flask by using acetonitrile, fixing the volume, and shaking up to prepare a sample solution for testing;
(3) and (3) injecting the test sample and the sample solution into an ultra-high performance liquid chromatograph, and performing high performance liquid chromatography analysis according to the conditions.
Experimental example 1
The chromatogram obtained in step (3) in example 1 was recorded, and the results are shown in FIG. 1.
From the data in FIG. 1, the peak time of the trimethylphenol isomer is: the peak time of 2,4, 5-trimethylphenol is 25min, and the peak time of 2,3, 5-trimethylphenol is 27 min. The results show that the high performance liquid chromatography is used for detecting the content of the trimethylphenol isomer, and the high performance liquid chromatography has the advantages of accurate quantification, good separation degree and the like.
Experimental example 2
Taking 2mL of the stock solution of the test sample solution in example 1, diluting the stock solution to 100mL by using the mobile phase in example 1 to obtain the test sample solution, and taking the test sample solution and diluting the test sample solution by 2 times, 4 times, 6 times and 10 times step by step to obtain 5 standard solutions with different concentrations.
The 5 standard solutions with different concentrations are analyzed according to the high performance liquid chromatography provided by the invention, the sample amount is 20 mu L, and a standard curve is prepared by taking the concentration of trimethylphenol as a horizontal coordinate and taking a peak area as a vertical coordinate.
The linear equation for trimethylphenol results is: 2,4, 5-trimethylphenol Y120500X; 2,3, 5-trimethylphenol Y ═ 172700X; wherein the correlation coefficient is 0.9999; wherein X is the trimethylphenol concentration, and Y is the peak area.
Experimental example 3
Weighing 5 samples of 2, 5-dimethylphenol with known content, adding a 2,4, 5-trimethylphenol standard sample and a 2,3, 5-trimethylphenol standard sample respectively, carrying out content measurement according to the method provided by the embodiment of the invention, wherein the accuracy experiment result is shown in table 1:
TABLE 1 accuracy analysis of samples
As can be seen from the data in Table 1, the average recovery of trimethylphenol was determined as: 97.1 percent of 2,4, 5-trimethylphenol; 98.4% of 2,3, 5-trimethylphenol. The result shows that the method provided by the embodiment of the invention has high accuracy and excellent effect in measuring the content of trimethylphenol in 2, 5-dimethylphenol.
In summary, the method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by the high performance liquid chromatography provided by the embodiment of the invention has high accuracy and precision and good linear relation. According to the method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by using the high performance liquid chromatography, provided by the embodiment of the invention, the content of trimethylphenol in the 2, 5-dimethylphenol product is detected by using the ultra-high performance liquid chromatography, so that the rapid and accurate quantification is realized, and the control of the product quality is achieved.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by high performance liquid chromatography is characterized in that: the trimethylphenol comprises 2,4, 5-trimethylphenol and 2,3, 5-trimethylphenol; the chromatographic conditions of the process include: adopting a C18 liquid chromatographic column and an ultraviolet detector; taking an organic phase-water phase as a mobile phase, wherein the concentration of the water phase is 2-3mL/L, the volume ratio of the organic phase to the water phase is 40:60, the flow rate of the mobile phase is 1mL/min, the detection wavelength is 276nm, the column temperature is 30 ℃, and the sample injection amount is 20 mu L; the organic phase is acetonitrile; the aqueous phase comprises pure water-glacial acetic acid.
2. The method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by high performance liquid chromatography as claimed in claim 1, wherein the stationary phase of the C18 liquid chromatography column is octadecylsilane chemically bonded silica.
3. The method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by high performance liquid chromatography according to claim 1, which comprises the following steps:
(1) weighing a standard substance containing the trimethylphenol, dissolving the standard substance in a volumetric flask by using pure methanol, fixing the volume, shaking up, then separating liquid, diluting by using the mobile phase, fixing the volume, and shaking up to prepare a test standard substance solution;
(2) weighing a sample containing the trimethylphenol, dissolving the sample in a volumetric flask by using the mobile phase, fixing the volume, shaking up and filtering to prepare a sample solution;
(3) and (3) taking the test sample solution and the test sample solution, respectively injecting the test sample solution and the test sample solution into the high performance liquid chromatograph, and performing high performance liquid chromatography analysis according to the chromatographic conditions.
4. The method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by high performance liquid chromatography as claimed in claim 3, wherein the step (3) further comprises: taking the test sample solution and diluting the test sample solution by 2 times, 4 times, 6 times and 10 times step by step to obtain 5 standard solutions with detection concentrations; performing high performance liquid chromatography analysis according to the chromatographic conditions, wherein the sample volume is 20uL, a standard curve is prepared by taking the concentration of the trimethylphenol as a horizontal coordinate and the peak area as a vertical coordinate, and the linear equation of the trimethylphenol is obtained as follows: 2,4, 5-trimethylphenol Y120500X; 2,3, 5-trimethylphenol Y ═ 172700X; wherein X is the concentration of the trimethylphenol, and Y is the peak area.
5. The method for detecting the content of trimethylphenol in 2, 5-dimethylphenol by high performance liquid chromatography as claimed in claim 4, wherein the step (3) further comprises: substituting the peak area of the trimethylphenol detected by the high performance liquid chromatography of the sample solution to be tested into the linear equation, and calculating to obtain the content of 2,4, 5-trimethylphenol or 2,3, 5-trimethylphenol in the 2, 5-dimethylphenol product or the intermediate sample in the synthesis process of the product.
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