CN108107136A - A kind of method of pseudocuminol content in high performance liquid chromatography detection 2,5- xylenols - Google Patents
A kind of method of pseudocuminol content in high performance liquid chromatography detection 2,5- xylenols Download PDFInfo
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- CN108107136A CN108107136A CN201711342939.6A CN201711342939A CN108107136A CN 108107136 A CN108107136 A CN 108107136A CN 201711342939 A CN201711342939 A CN 201711342939A CN 108107136 A CN108107136 A CN 108107136A
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- 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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- 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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- 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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- G01N30/8624—Detection of slopes or peaks; baseline correction
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Abstract
The invention belongs to chemical raw material monomers to test and analyze technical field, provides a kind of method that high performance liquid chromatography detects pseudocuminol content in 2,5 xylenols, and this method includes：Using C18 liquid-phase chromatographic columns and UV detector；Using organic-aqueous as mobile phase, the flow velocity of mobile phase is 1mL/min, and Detection wavelength 276nm, column temperature is 30 DEG C, and sample size is 20 μ L.This method is suitable for the detection of micro pseudocuminol monomer, can rapidly and accurately quantify pseudocuminol isomers, and separating degree is good, it can be achieved that testing goal.
Description
Technical field
The invention belongs to chemical raw material monomers to test and analyze technical field, specifically, is related to a kind of high performance liquid chromatography
The method of pseudocuminol content in method detection 2,5- xylenols.
Background technology
Pseudocuminol is synthesized as a kind of disproportionation products in the production of 2,5- xylenols in 2,5- xylenols
In, it is affected to product yield and quality.Therefore, it is necessary to trimethylbenzene during 2,5- xylenols synthesize
The isomers of phenol is monitored.
At present, the detection method of 2,5- xylenols mainly has：Gas chromatography detects 2,5- dimethylphenol contents,
The defects of the method is without detection to pseudocuminol；Or methanol-water is used to be detected for mobile phase in 2,5- xylenols
Pseudocuminol content, but using this method, accurately can not individually measure pseudocuminol isomers.
Since the prior art is there are the above problem, for the monitoring in 2,5- xylenol building-up processes, there is an urgent need to
A kind of test method of the good detection pseudocuminol of separating degree.
The content of the invention
For deficiency above-mentioned in the prior art, it is an object of the invention to provide a kind of high performance liquid chromatographies to detect 2,
The method of pseudocuminol content in 5- xylenols, this method are suitable for the detection of micro pseudocuminol monomer, can be fast
Speed quantifies pseudocuminol isomers exactly, and separating degree is good, it can be achieved that testing goal.
In order to achieve the above object, the solution that uses of the present invention is：
The method of pseudocuminol content, the chromatography of method in a kind of high performance liquid chromatography detection 2,5- xylenols
Condition includes：Using C18 liquid-phase chromatographic columns and UV detector；Using organic-aqueous as mobile phase, the flow velocity of the mobile phase
For 1mL/min, Detection wavelength 276nm, column temperature is 30 DEG C, and sample size is 20 μ L.
The side of pseudocuminol content in a kind of high performance liquid chromatography detection 2,5- xylenols provided by the invention
The advantageous effect of method is：
The method of high performance liquid chromatography detection pseudocuminol isomer monomer content provided by the invention, by that will match somebody with somebody
The sample solution injection C18 liquid-phase chromatographic columns made by the separation of chromatographic column, control chromatographic condition, the chemistry in sample into
Divide and flow out chromatographic column successively according to polarity size, and be shown in the form of chromatographic peak on chromatogram；Then by pseudocuminol
The peak area of isomer monomer substitutes into linear equation, and pseudocuminol isomers in 2,5- xylenol samples is calculated
The content of monomer.
The method of pseudocuminol content in high performance liquid chromatography detection 2,5- xylenols provided by the invention
It can be achieved accurately to quantify, so as to reach the control of product quality.Just because of employing high performance liquid chromatograph and this hair
Coordinated synergy between the chromatographic condition of bright offer, it is separated accurate between trimethyl isomers so as to further increase
Degree is capable of the content of accurate quantification each pseudocuminol.
Description of the drawings
Fig. 1 is the 2,5- dimethyl benzene phenolic product chromatograms that invention experimental example 1 provides.
Specific embodiment
It, below will be in the embodiment of the present invention to make the purpose, technical scheme and advantage of the embodiment of the present invention clearer
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Below to trimethyl in a kind of high performance liquid chromatography detection 2,5- xylenols provided in an embodiment of the present invention
The method of phenol content is specifically described.
A kind of method of pseudocuminol content in high performance liquid chromatography detection 2,5- xylenols, including：.
(1) the mark product containing pseudocuminol are weighed, in volumetric flask with pure methanol dissolving, constant volume, shake up, then liquid separation,
With flowing phase dilution, constant volume shakes up and is made for test-object product solution.
It should be noted that pseudocuminol in the present embodiment includes 2,4,5- pseudocuminols and 2,3,5- tri-
Methylphenol.
It based on cost is reduced, is accounted for from price, preferably by methanol as solvent.
In addition, in the present embodiment, mobile phase is preferably organic-aqueous.Wherein, in order to produce different pseudocuminols
It is estranged from, preferably, organic phase include acetonitrile or methanol；It is further preferable that organic phase is acetonitrile, and using methanol, two kinds
There is separation between pseudocuminol, but separating degree is poor compared with using acetonitrile.Water mutually includes the water of pure water-glacial acetic acid namely glacial acetic acid
Solution.Effect is more accurately separated in order to obtain, it is preferable that the concentration of water phase is 2-3mL/L, is more preferably 2mL/L；
Being imitated when column reduces, and when separating degree is deteriorated between pseudocuminol isomers, can be slightly increased glacial acetic acid concentration at this time.
In the present embodiment, in order to reach optimal separating effect so that the measure of the content of pseudocuminol isomers
More accurate, preferably, the volume ratio of organic phase and water phase is 40:60.
(2) weigh the sample containing pseudocuminol, in volumetric flask with flowing phased soln, constant volume, shake up, filter, be made
Test sample solution.
(3) take for test-object product solution and test sample solution, be injected separately into high performance liquid chromatograph, according to chromatographic condition into
Row efficient liquid phase chromatographic analysis.
Specifically, in step (3)：It takes first for test-object product solution and dilutes 2 times, 4 times, 6 times, 10 times step by step, obtain
To the standard solution of 5 various concentrations；By the standard solution of 5 various concentrations according to high performance liquid chromatography provided by the invention
It is analyzed.
It should be noted that in the present embodiment, the chromatographic condition of use includes：Using C18 liquid-phase chromatographic columns and ultraviolet
Detector；The flow velocity of mobile phase is 1mL/min, and Detection wavelength 276nm, column temperature is 30 DEG C, and sample size is 20 μ L；As preferred
Ground, the stationary phase of C18 liquid-phase chromatographic columns is octadecylsilane chemically bonded silica.
Using above-mentioned chromatographic condition, between each parameter can coordinated synergy, it is different so as to further increase trimethyl
Separated accuracy between structure body is capable of the content of accurate quantification each pseudocuminol.
Then using the concentration of above-mentioned pseudocuminol as abscissa, peak area makes standard curve for ordinate, obtains three
The linear equation of methylphenol.
Then, on the peak area of the pseudocuminol then by test sample solution obtained through high performance liquid chromatography detection substitutes into
Linear equation is stated, 2,4,5- trimethyls in 2,5- dimethyl benzenes phenolic product or the meso sample of its building-up process are accurately calculated
The content of phenol or 2,3,5- pseudocuminols.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
Present embodiments provide pseudocuminol content in a kind of high performance liquid chromatography detection 2,5- xylenols
Method, including：
The test apparatus and condition of detection：
Shimadzu LC-10 Ultra Performance Liquid Chromatography instruments, band UV detector；Chromatographic column：C18 columns (4.6mm × 250mm ×
5um)；Mobile phase：The volume ratio of organic-aqueous is 40：60, isocratic elution；Wherein, organic phase is acetonitrile, and water is mutually
The glacial acetic acid aqueous solution of 2mL/L；Flow velocity：1mL/min；Detection wavelength：276nm；Column temperature：30℃；Sample size：20μL.
The test procedure of detection：
(1) the 2 of the tri- cresols standard specimens of 2,4,5- of about 10mg, the 2,5- xylenols reference substance of 10mg and 10mg accurately is weighed,
3,5- tri- cresols standard specimens, with methanol dissolving and constant volume, shake up in 25mL volumetric flasks, are available test-object product solution stoste；It takes
1.0mL standards mother liquor, with mobile phase constant volume, shakes up into 100mL volumetric flasks, and available test-object product solution is used；
(2) 2, the 5- xylenol samples of 0.15g are weighed, in 50mL volumetric flasks, is dissolved, constant volume, shaken up with acetonitrile,
Available test agent solution is used；
(3) above-mentioned confession test-object product and sample solution are taken, injects Ultra Performance Liquid Chromatography instrument, is carried out according to above-mentioned condition efficient
Liquid-phase chromatographic analysis.
Experimental example 1
Record chromatogram, the result is shown in Figure 1 obtained by step (3) in embodiment 1.
It was found from Fig. 1 data, the appearance time of pseudocuminol isomers is：The appearance time of 2,4,5- pseudocuminols
For 25min, the appearance time of 2,3,5-TEP is 27min.The above results show to utilize the high performance liquid chromatography detection
The content of pseudocuminol isomers, has many advantages, such as accurate quantitative analysis, and separating degree is good.
Experimental example 2
Test-object product solution stoste 2mL is supplied in Example 1,100mL is diluted to the mobile phase of embodiment 1 and is supplied
Test-object product solution takes for test-object product solution and dilutes 2 times, 4 times, 6 times, 10 times step by step, and the standard for obtaining 5 various concentrations is molten
Liquid.
The standard solution of 5 various concentrations is analyzed according to high performance liquid chromatography provided by the invention, sample size
It is 20 μ L, using the concentration of pseudocuminol as abscissa, peak area makes standard curve for ordinate.
As a result the linear equation for obtaining pseudocuminol is：2,4,5- pseudocuminols Y=120500X；2,3,5- front threes
Base phenol Y=172700X；Wherein, related coefficient 0.9999；Wherein, X is pseudocuminol concentration, and Y is peak area.
Experimental example 3
2, the 5- xylenol samples of known content is taken to weigh 5 samples, be separately added into 2,4,5- tri- cresols standard specimens and
2,3,5- tri- cresols standard specimens carry out assay, accuracy experimental result such as 1 institute of table according to method provided in an embodiment of the present invention
Show：
The accuracy analysis of 1 sample of table
From the data in table 1, it can be seen that the average recovery rate for measuring pseudocuminol is：2,4,5- pseudocuminols are 97.1%；
2,3,5- pseudocuminols are 98.4%.The above results show to measure 2,5- diformazans using method provided in an embodiment of the present invention
Pseudocuminol content accuracy rate is high in base phenol, excellent effect.
In conclusion by a kind of high performance liquid chromatography detection 2,5- xylenols provided in an embodiment of the present invention three
The method of methylphenol content, has higher accuracy and precision, and linear relationship is good.Provided in an embodiment of the present invention one
The method of pseudocuminol content in kind of high performance liquid chromatography detection 2,5- xylenols, by by ultra performance liquid chromatography
Method is applied to the content of the pseudocuminol in detection 2,5- dimethyl benzene phenolic products, realizes and fast and accurately quantifies, so as to
Reach the control of product quality.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of method of pseudocuminol content in high performance liquid chromatography detection 2,5- xylenols, it is characterised in that：
The chromatographic condition of the method includes：Using C18 liquid-phase chromatographic columns and UV detector；Using organic-aqueous as mobile phase, institute
The flow velocity of mobile phase is stated as 1mL/min, Detection wavelength 276nm, column temperature is 30 DEG C, and sample size is 20 μ L.
2. the side of pseudocuminol content in high performance liquid chromatography detection 2,5- xylenols according to claim 1
Method, which is characterized in that the stationary phase of the C18 liquid-phase chromatographic columns is octadecylsilane chemically bonded silica.
3. the side of pseudocuminol content in high performance liquid chromatography detection 2,5- xylenols according to claim 1
Method, which is characterized in that the organic phase includes acetonitrile or methanol；The water mutually includes pure water-glacial acetic acid.
4. the side of pseudocuminol content in high performance liquid chromatography detection 2,5- xylenols according to claim 3
Method, which is characterized in that the concentration of the water phase is 2-3mL/L.
5. the side of pseudocuminol content in high performance liquid chromatography detection 2,5- xylenols according to claim 3
Method, which is characterized in that the volume ratio of the organic phase and the water phase is 40:60.
6. the side of pseudocuminol content in high performance liquid chromatography detection 2,5- xylenols according to claim 1
Method, which is characterized in that the pseudocuminol includes 2,4,5- pseudocuminols and 2,3,5-TEP.
7. the side of pseudocuminol content in high performance liquid chromatography detection 2,5- xylenols according to claim 6
Method, which is characterized in that including：
(1) the mark product containing the pseudocuminol are weighed, in volumetric flask with pure methanol dissolving, constant volume, shake up, then liquid separation,
With the flowing phase dilution, constant volume shakes up and is made for test-object product solution；
(2) weigh the sample containing the pseudocuminol, in volumetric flask with flowing phased soln, the constant volume, shake up, filter,
Test sample solution is made；
(3) confession test-object product solution and the test sample solution are taken, the high performance liquid chromatograph is injected separately into, according to institute
It states chromatographic condition and carries out efficient liquid phase chromatographic analysis.
8. the side of pseudocuminol content in high performance liquid chromatography detection 2,5- xylenols according to claim 7
Method, which is characterized in that step (3) further includes：Take it is described for test-object product solution and it is diluted step by step 2 times, 4 times, 6 times, 10
The standard solution of 5 detectable concentrations is obtained again；Efficient liquid phase chromatographic analysis is carried out according to the chromatographic condition, sample size is
20uL, using the concentration of the pseudocuminol as abscissa, peak area makes standard curve for ordinate, obtains the trimethyl
The linear equation of phenol is：2,4,5- pseudocuminols Y=120500X；2,3,5- pseudocuminols Y=172700X；Wherein, X
For the concentration of the pseudocuminol, Y is peak area.
9. the side of pseudocuminol content in high performance liquid chromatography detection 2,5- xylenols according to claim 8
Method, which is characterized in that step (3) further includes：Described three that the test sample solution is obtained through high performance liquid chromatography detection
The peak area of methylphenol substitutes into the linear equation, and 2,5- dimethyl benzenes phenolic product or the centre of its building-up process is calculated
The content of 2,4,5- pseudocuminols or 2,3,5- pseudocuminols in sample.
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Citations (2)
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| CN105021754A (en) * | 2015-07-03 | 2015-11-04 | 中华人民共和国台州出入境检验检疫局 | Liquid chromatography-tandem mass spectrometry method for simultaneous determination of specific migration of 18 phenols or phenol derivatives in five plastic food simulants |
| CN106645537A (en) * | 2017-01-23 | 2017-05-10 | 中国烟草总公司郑州烟草研究院 | Method for simultaneously measuring 19 smoke incense ingredients in main stream smoke of cigarette |
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|---|---|---|---|---|
| CN105021754A (en) * | 2015-07-03 | 2015-11-04 | 中华人民共和国台州出入境检验检疫局 | Liquid chromatography-tandem mass spectrometry method for simultaneous determination of specific migration of 18 phenols or phenol derivatives in five plastic food simulants |
| CN106645537A (en) * | 2017-01-23 | 2017-05-10 | 中国烟草总公司郑州烟草研究院 | Method for simultaneously measuring 19 smoke incense ingredients in main stream smoke of cigarette |
Non-Patent Citations (3)
| Title |
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| J. F. SCHABRON 等: "Separation of alkylphenols by normal-phase and reversed-phase high-performance liquid chromatography", 《ANALYTICAL CHEMISTRY》 * |
| KENNETH OGAN 等: "Liquid chromatographic separation of alkylphenols with fluorescence and ultraviolet detection", 《ANALYTICAL CHEMISTRY》 * |
| 陈志荣 等: "2,3,6-三甲基苯酚气-液-液氧化反应与传质过程", 《化工学报》 * |
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