CN111307963A - Chromatographic detection method of nonionic surfactant - Google Patents
Chromatographic detection method of nonionic surfactant Download PDFInfo
- Publication number
- CN111307963A CN111307963A CN201911267080.6A CN201911267080A CN111307963A CN 111307963 A CN111307963 A CN 111307963A CN 201911267080 A CN201911267080 A CN 201911267080A CN 111307963 A CN111307963 A CN 111307963A
- Authority
- CN
- China
- Prior art keywords
- concentration
- detected
- chromatographic
- standard
- nonionic surfactant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
-
- 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
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
-
- 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
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
- G01N2030/324—Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a chromatographic detection method of a nonionic surfactant, which uses a hydrophilic interaction chromatogram to determine the components and the content of the nonionic surfactant by a high performance liquid chromatogram-mass spectrum or other detectors under a proper organic phase ratio, sample detection needs to be carried out by pretreatment to remove non-target impurities and unreacted oily group substances, a to-be-detected product is subjected to gradient elution in an HILIC chromatographic column by taking acetonitrile-water (containing 0.1 percent of formic acid) as a mobile phase, components with different polymerization degrees are analyzed by a mass spectrum analysis or an evaporative light scattering detector ELSD, an ultraviolet visible light detector and a fluorescence detector, and the qualitative performance of a standard product and the quantitative performance of a standard working curve are adopted. The detection method has the advantages of high sensitivity, high accuracy, good precision and low cost, and does not need to perform derivatization treatment on the sample.
Description
Technical Field
The invention relates to the technical field of determination of components of nonionic surfactants, in particular to a chromatographic detection method of a nonionic surfactant.
Background
In recent years, a novel chromatographic separation mode, namely, hydrophilic interaction chromatography HILIC is widely applied to various fields such as environmental analysis, drug quantitative detection, food safety inspection and the like, the chromatography integrates the advantages of economy and cheapness of reverse phase chromatography and normal phase chromatography, effectively supplements the defects of the two chromatographs, and plays an important role in the separation and analysis process of hydrophilic substances along with the deep research. In HILIC, the polarity strength of the solvent of the mobile phase is the most important factor influencing the retention time of the compound, the hydrophilic action of the chromatographic column is obviously enhanced along with the reduction of the polarity of the eluent, when the acetonitrile content in the mobile phase is increased from 50 percent to 95 percent, the retention of the object to be detected is gradually enhanced, which is the typical characteristic of hydrophilic action chromatography, correspondingly, the retention behavior of the analyte in the high organic solvent mobile phase reflects the hydrophilic property of the chromatographic stationary phase.
The nonionic surfactant is second to the anionic surfactant in yield and variety, has good detergency, better emulsification, solubilization and lower foam, and plays an important role in industrial auxiliaries. The nonionic surfactant is not in an ionic state in an aqueous solution, so the nonionic surfactant has high stability, is not easily influenced by acid, alkali and strong electrolyte inorganic salts, has good compatibility with other surfactants, has good solubility in water and organic solvents, and has obvious difference in structure. When the oxyethylene group is bonded to the lipophilic group, the longer the bonded oxyethylene group is, the better the water solubility is, and thus the variety specifications which can be produced are extremely large and the applications are extremely wide. Therefore, an accurate and reliable detection method is crucial to verifying whether the synthesized nonionic surfactant product reaches the designed target molecular weight. On the other hand, due to the difference of the synthesis process, the components of the molecular chains of different polymerization degrees of the nonionic surfactant are different, the product shows the difference of performance, and the surfactants with different polymerization degrees have different performance and application, so that the regularity between the polymerization degree and molecular weight composition of the surfactant and an application system needs to be mastered. The multi-component nonionic surfactant is analyzed and characterized through hydrophilic chromatography tandem mass spectrometry or evaporative light scattering, the composition of each component in the surfactant is explored, chromatographic analysis conditions are optimized, an efficient and reliable qualitative and quantitative evaluation method of the surfactant is established, and a scientific method is provided for selection and adjustment of a production process of the surfactant and guarantee of product stability.
Disclosure of Invention
The present invention is directed to a chromatographic detection method for nonionic surfactants, which solves the above problems of the prior art.
In order to achieve the purpose, the invention provides the following technical scheme: a chromatographic detection method of a nonionic surfactant comprises the following steps:
A. purifying and preparing a sample: pre-treating a to-be-detected article, weighing a certain amount of the to-be-detected article, washing the to-be-detected article with purified water which is 5-10 times the weight of the to-be-detected article, standing and layering the to-be-detected article to remove and synthesize an oil phase monomer which is not completely reacted, then carrying out reduced pressure distillation on a non-ionic surfactant dissolved in water, preparing a purified sample with a proper concentration range by using a liquid chromatogram initial flow phase as a stock solution, and filtering the sample to be detected by using a 0.45 mu m;
B. preparing a qualitative and quantitative standard working curve solution: preparing a stock solution from a standard reagent by using a liquid chromatogram initial mobile phase under a proper concentration, diluting the stock solution downwards into a series of working solutions with target concentration at equal intervals according to a mode of 'stock solution concentration taking quantity as target concentration and constant volume', and filtering the working solutions with 0.45 mu m of polytetrafluoroethylene needle type filter for later use;
C. mobile phase gradient elution: gradient eluting the solution to be detected with acetonitrile (A) -water (B) as mobile phase in HILIC chromatographic column with gradient elution parameter of 0-5min and 50% A; 5-10min, 70% A; 10-15min, 90% A; 15-20min, 95% A;
D. and (3) flow rate control: controlling the flow rate to be 0.3-1.2 mL/min;
E. performing hydrophilic chromatography-mass spectrometry;
F. hydrophilicity chromatography-evaporative light scattering assay.
Preferably, the determination method in step E is as follows:
a) and (3) qualitative determination: b, detecting the to-be-detected product obtained in the step A, if the retention time of the chromatographic peak of the excimer ions in the total ion flow graph is consistent with that of the standard product; and when the relative standard deviation of the mass number of the standard substance with the mass number equivalent to the concentration does not exceed a limit value, judging that the to-be-detected substance is the target substance; or judging the mass number of the product to be detected according to the mass-to-charge ratio of the molecular ion peak in the mass spectrogram;
b) quantitative determination: performing HILIC-MS measurement on the standard working solution with each concentration in the step B, and performing regression analysis by taking the concentration of the standard working solution as an X axis and the chromatographic peak area of the standard working solution with each concentration as a Y axis to obtain a standard working curve; and C, carrying out HILIC-MS measurement on the to-be-measured substance obtained in the step B under the same condition, measuring the chromatographic peak area of the to-be-measured substance, and substituting the chromatographic peak area into a standard curve to obtain the concentration of the to-be-measured substance.
Preferably, the determination method in step F is as follows:
a) and (3) qualitative determination: b, detecting the to-be-detected product obtained in the step B, and if the retention time of the liquid chromatogram peak is consistent with that of the standard product, judging that the to-be-detected product is the target substance;
b) quantitative determination: performing HILIC-ELSD (high intensity liquid-electron scattering diffraction) determination on the standard working solution with each concentration in the step C, and performing regression analysis by taking the concentration of the standard working solution as an X axis and the chromatographic peak area of the standard working solution with each concentration as a Y axis to obtain a standard working curve; and C, carrying out HILIC-ELSD measurement on the to-be-measured substance obtained in the step B under the same condition, measuring the chromatographic peak area of the to-be-measured substance, and substituting the chromatographic peak area into a standard curve to obtain the concentration of the to-be-measured substance.
Preferably, the water phase pressure distillation washing temperature in the step A is set to be 80-95 ℃, and the filter membrane is an organic polytetrafluoroethylene membrane or a nylon membrane.
Preferably, according to the gradient selection principle in the step C, the initial proportion of the mobile phase acetonitrile-water mixed solution or methanol-water mixed solution is adjusted according to the content of the hydrophilic group in the molecular chain and the strength of the hydrophilic property of the product to be detected, and formic acid is added to adjust the pH value to optimize the peak shape.
Preferably, the column used in step E, F is a hydrophilic interaction chromatography column, including any one of bare silica gel, amino silica gel, amide modified silica gel, alkyl betaine sulfonate modified silica gel, carboxyl betaine type silica gel, anionic and cationic silica gel, carbohydrate modified silica gel, cyano silica gel, diol silica gel, triazole modified silica gel, imidazole chimeric amino silica gel, and polymer matrix monolithic columns.
Preferably, the electrospray ion source is used for mass spectrometry in the step E, the positive ion mode and the negative ion mode can be used, the to-be-detected product can adopt a multi-reaction monitoring mode or a full-scanning mode, and the selective ion detection can be adopted for the standard working solution, wherein the ion source temperature is 120-.
Preferably, the mass spectrometry detection in the step E uses a first-order full scan mode.
Compared with the prior art, the invention has the beneficial effects that: the nonionic surfactant detected by the invention is a temperature-sensitive surfactant with cloud point, so that the detection process can not only adjust and separate the peak condition by changing the proportion of inorganic solvent components in a mobile phase, but also adjust and separate the peak condition by adjusting the column temperature of a hydrophilic interaction chromatographic column, and the separation efficiency can be further improved by utilizing the stationary phase hydrophilic interaction chromatographic column of isopropyl acrylamide with certain temperature response capability; the invention utilizes HILIC hydrophilic interaction chromatography to separate the components of the nonionic surfactant, and the established HPLC-MS/MS detection method is successfully applied to the detection of the components of the nonionic surfactant. The newly established detection method has the advantages of no need of derivatization in sample treatment and short detection time, and has the characteristics of high accuracy, good sensitivity and the like.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides the following technical scheme: a chromatographic detection method of a nonionic surfactant comprises the following steps:
A. purifying and preparing a sample: pre-treating a to-be-detected article, weighing a certain amount of the to-be-detected article, washing the to-be-detected article with purified water which is 5-10 times the weight of the to-be-detected article, standing and layering the to-be-detected article to remove and synthesize an oil phase monomer which is not completely reacted, then carrying out reduced pressure distillation on a non-ionic surfactant dissolved in water, preparing a purified sample with a proper concentration range by using a liquid chromatogram initial flow phase as a stock solution, and filtering the sample to be detected by using a 0.45 mu m;
B. preparing a qualitative and quantitative standard working curve solution: preparing a stock solution from a standard reagent by using a liquid chromatogram initial mobile phase under a proper concentration, diluting the stock solution downwards into a series of working solutions with target concentration at equal intervals according to a mode of 'stock solution concentration taking quantity as target concentration and constant volume', and filtering the working solutions with 0.45 mu m of polytetrafluoroethylene needle type filter for later use;
C. mobile phase gradient elution: gradient eluting the solution to be detected with acetonitrile (A) -water (B) as mobile phase in HILIC chromatographic column with gradient elution parameter of 0-5min and 50% A; 5-10min, 70% A; 10-15min, 90% A; 15-20min, 95% A;
D. and (3) flow rate control: controlling the flow rate to be 0.3-1.2 mL/min;
E. performing hydrophilic chromatography-mass spectrometry;
F. hydrophilicity chromatography-evaporative light scattering assay.
In this example, the measurement method in step E is as follows:
a) and (3) qualitative determination: b, detecting the to-be-detected product obtained in the step A, if the retention time of the chromatographic peak of the excimer ions in the total ion flow graph is consistent with that of the standard product; and when the relative standard deviation of the mass number of the standard substance with the mass number equivalent to the concentration does not exceed a limit value, judging that the to-be-detected substance is the target substance; or judging the mass number of the product to be detected according to the mass-to-charge ratio of the molecular ion peak in the mass spectrogram;
b) quantitative determination: performing HILIC-MS measurement on the standard working solution with each concentration in the step B, and performing regression analysis by taking the concentration of the standard working solution as an X axis and the chromatographic peak area of the standard working solution with each concentration as a Y axis to obtain a standard working curve; and C, carrying out HILIC-MS measurement on the to-be-measured substance obtained in the step B under the same condition, measuring the chromatographic peak area of the to-be-measured substance, and substituting the chromatographic peak area into a standard curve to obtain the concentration of the to-be-measured substance.
In this example, the measurement method in step F is as follows:
a) and (3) qualitative determination: b, detecting the to-be-detected product obtained in the step B, and if the retention time of the liquid chromatogram peak is consistent with that of the standard product, judging that the to-be-detected product is the target substance;
b) quantitative determination: performing HILIC-ELSD (high intensity liquid-electron scattering diffraction) determination on the standard working solution with each concentration in the step C, and performing regression analysis by taking the concentration of the standard working solution as an X axis and the chromatographic peak area of the standard working solution with each concentration as a Y axis to obtain a standard working curve; and C, carrying out HILIC-ELSD measurement on the to-be-measured substance obtained in the step B under the same condition, measuring the chromatographic peak area of the to-be-measured substance, and substituting the chromatographic peak area into a standard curve to obtain the concentration of the to-be-measured substance.
In the embodiment, the water phase pressure distillation washing temperature in the step A is set to be 80-95 ℃, and the filter membrane is an organic polytetrafluoroethylene membrane or a nylon membrane.
In this embodiment, according to the gradient selection principle in step C, the initial proportion of the mobile phase acetonitrile-water mixed solution or methanol-water mixed solution is adjusted according to the content of the hydrophilic group in the molecular chain and the strength of the hydrophilic property of the sample to be tested, and formic acid is added to adjust the pH value to optimize the peak shape.
In this embodiment, the column used in step E, F is a hydrophilic interaction chromatographic column, and includes any one of bare silica, amino silica, amide modified silica, alkyl betaine sulfonate modified silica, carboxyl betaine type silica, anionic and cationic silica, carbohydrate modified silica, cyano silica, diol silica, triazole modified silica, imidazole chimeric amino silica, and polymer-based monolithic columns.
In this embodiment, in the step E, the electrospray ion source is used for mass spectrometry, the positive ion mode and the negative ion mode are both available, the to-be-detected sample can adopt a multi-reaction monitoring mode or a full-scanning mode, and the selective ion detection can be adopted for the standard working solution, wherein the ion source temperature is 120-.
In this embodiment, the mass spectrometry detection in step E uses a first-order full scan mode.
Example (b):
fatty alcohol polyoxyethylene ether was used for analysis with chromatographic components:
10g of fatty alcohol-polyoxyethylene ether is absorbed and washed by 100g of purified water, standing and layering are carried out to remove oil phase monomers which are not completely synthesized, then a non-ionic surfactant dissolved in water is distilled under reduced pressure at 90 ℃, a stock solution of a to-be-detected product is prepared by using a liquid chromatogram initial mobile phase acetonitrile-water 5:5, and after the non-ionic surfactant is fully dissolved, a 0.45 mu m polytetrafluoroethylene needle filter is used for filtering the to-be-detected product.
Dissolving 25mg of standard substance with a certain polymerization degree by using chromatographic pure acetonitrile and ultrapure water with an initial mobile phase ratio of 5:5, fixing the volume to a 50mL volumetric flask, preparing 0.5g/l standard substance stock solution, and downwards diluting the standard substance stock solution into 5 concentration standard working solutions with 0.02g/l, 0.04g/l, 0.06g/l, 0.08g/l and 0.1g/l by using chromatographic pure acetonitrile and ultrapure water with an initial mobile phase ratio of 5: 5;
performing gradient elution on the solution to be detected in HILIC chromatographic column with initial mobile phase acetonitrile (A) -water (B)5:5, wherein gradient elution parameters are 0-5min and 50% of A; 5-10min, 70% A; 10-15min, 90% A; 15-20min, 95% A; adding 0.1% of formic acid v/v into water to adjust the pH value to optimize the peak shape;
the mass spectrometry uses an electrospray ionization source (ESI), the positive ion mode and the negative ion mode can be used, the to-be-detected article can adopt a multi-reaction monitoring mode (MRM) or a full scanning mode (SCAN), the standard working solution can adopt selective ion detection (SIM), the temperature of the ion source is 120-. And (3) performing tandem mass spectrometry on the characteristic ion peak of the liquid to be detected separated by the hydrophilic interaction chromatography, determining the ratio of the liquid-mass characteristic ion peak to the peak area of the characteristic peak of the corresponding standard substance, and calculating the content of the corresponding component in the sample to be detected according to the peak area ratio and the added standard amount.
In conclusion, the nonionic surfactant detected by the method is a temperature-sensitive surfactant with cloud point, so that the detection process can not only adjust and separate the peak condition by changing the proportion of inorganic solvent components in a mobile phase, but also adjust and separate the peak condition by adjusting the column temperature of a hydrophilic interaction chromatographic column, and the separation efficiency can be further improved by utilizing the stationary phase hydrophilic interaction chromatographic column of isopropyl acrylamide with certain temperature response capability; the invention utilizes HILIC hydrophilic interaction chromatography to separate the components of the nonionic surfactant, and the established HPLC-MS/MS detection method is successfully applied to the detection of the components of the nonionic surfactant. The newly established detection method has the advantages of no need of derivatization in sample treatment and short detection time, and has the characteristics of high accuracy, good sensitivity and the like.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A chromatographic detection method of a nonionic surfactant is characterized in that: the method comprises the following steps:
A. purifying and preparing a sample: pre-treating a to-be-detected article, weighing a certain amount of the to-be-detected article, washing the to-be-detected article with purified water which is 5-10 times the weight of the to-be-detected article, standing and layering the to-be-detected article to remove and synthesize an oil phase monomer which is not completely reacted, then carrying out reduced pressure distillation on a non-ionic surfactant dissolved in water, preparing a purified sample with a proper concentration range by using a liquid chromatogram initial flow phase as a stock solution, and filtering the sample to be detected by using a 0.45 mu m;
B. preparing a qualitative and quantitative standard working curve solution: preparing a stock solution from a standard reagent by using a liquid chromatogram initial mobile phase under a proper concentration, diluting the stock solution downwards into a series of working solutions with target concentration at equal intervals according to a mode of 'stock solution concentration taking quantity as target concentration and constant volume', and filtering the working solutions with 0.45 mu m of polytetrafluoroethylene needle type filter for later use;
C. mobile phase gradient elution: gradient eluting the solution to be detected with acetonitrile (A) -water (B) as mobile phase in HILIC chromatographic column with gradient elution parameter of 0-5min and 50% A; 5-10min, 70% A; 10-15min, 90% A; 15-20min, 95% A;
D. and (3) flow rate control: controlling the flow rate to be 0.3-1.2 mL/min;
E. performing hydrophilic chromatography-mass spectrometry;
F. hydrophilicity chromatography-evaporative light scattering assay.
2. The chromatographic detection method for the nonionic surfactant according to claim 1, characterized in that: the determination method in the step E is as follows:
a) and (3) qualitative determination: b, detecting the to-be-detected product obtained in the step A, if the retention time of the chromatographic peak of the excimer ions in the total ion flow graph is consistent with that of the standard product; and when the relative standard deviation of the mass number of the standard substance with the mass number equivalent to the concentration does not exceed a limit value, judging that the to-be-detected substance is the target substance; or judging the mass number of the product to be detected according to the mass-to-charge ratio of the molecular ion peak in the mass spectrogram;
b) quantitative determination: performing HILIC-MS measurement on the standard working solution with each concentration in the step B, and performing regression analysis by taking the concentration of the standard working solution as an X axis and the chromatographic peak area of the standard working solution with each concentration as a Y axis to obtain a standard working curve; and C, carrying out HILIC-MS measurement on the to-be-measured substance obtained in the step B under the same condition, measuring the chromatographic peak area of the to-be-measured substance, and substituting the chromatographic peak area into a standard curve to obtain the concentration of the to-be-measured substance.
3. The chromatographic detection method for the nonionic surfactant according to claim 1, characterized in that: the determination method in the step F is as follows:
a) and (3) qualitative determination: b, detecting the to-be-detected product obtained in the step B, and if the retention time of the liquid chromatogram peak is consistent with that of the standard product, judging that the to-be-detected product is the target substance;
b) quantitative determination: performing HILIC-ELSD (high intensity liquid-electron scattering diffraction) determination on the standard working solution with each concentration in the step C, and performing regression analysis by taking the concentration of the standard working solution as an X axis and the chromatographic peak area of the standard working solution with each concentration as a Y axis to obtain a standard working curve; and C, carrying out HILIC-ELSD measurement on the to-be-measured substance obtained in the step B under the same condition, measuring the chromatographic peak area of the to-be-measured substance, and substituting the chromatographic peak area into a standard curve to obtain the concentration of the to-be-measured substance.
4. The chromatographic detection method for the nonionic surfactant according to claim 1, characterized in that: in the step A, the water phase differential pressure distillation washing temperature is set to be 80-95 ℃, and the filter membrane is an organic polytetrafluoroethylene membrane or a nylon membrane.
5. The chromatographic detection method for the nonionic surfactant according to claim 1, characterized in that: and C, adjusting the initial proportion of the mobile phase acetonitrile-water mixed solution or the methanol-water mixed solution according to the gradient selection principle in the step C and the content of the hydrophilic group in the molecular chain and the strength of the hydrophilic property of the product to be detected, and adding formic acid to adjust the pH value to optimize the peak shape.
6. The chromatographic detection method for the nonionic surfactant according to claim 1, characterized in that: the column used in step E, F is a hydrophilic interaction chromatographic column, and includes any one of bare silica gel, amino silica gel, amide-modified silica gel, alkyl betaine sulfonate-modified silica gel, carboxyl betaine type silica gel, anion and cation type silica gel, carbohydrate-modified silica gel, cyano silica gel, glycol silica gel, triazole-modified silica gel, imidazole-embedded amino silica gel, and polymer-based monolithic columns.
7. The chromatographic detection method for the nonionic surfactant according to claim 1, characterized in that: in the step E, an electrospray ion source is used for mass spectrometry, the positive ion mode and the negative ion mode can be used, the to-be-detected product can adopt a multi-reaction monitoring mode or a full scanning mode, and the standard working solution can adopt selective ion detection, wherein the ion source temperature is 120-.
8. The chromatographic detection method for the nonionic surfactant according to claim 1, characterized in that: and E, performing mass spectrum detection in a first-order full scanning mode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911267080.6A CN111307963A (en) | 2019-12-11 | 2019-12-11 | Chromatographic detection method of nonionic surfactant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911267080.6A CN111307963A (en) | 2019-12-11 | 2019-12-11 | Chromatographic detection method of nonionic surfactant |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111307963A true CN111307963A (en) | 2020-06-19 |
Family
ID=71145284
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911267080.6A Withdrawn CN111307963A (en) | 2019-12-11 | 2019-12-11 | Chromatographic detection method of nonionic surfactant |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111307963A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112362768A (en) * | 2020-10-23 | 2021-02-12 | 北京民海生物科技有限公司 | Method for measuring content of Berol 185 in sample by using liquid chromatography tandem mass spectrometry |
| CN113759068A (en) * | 2021-08-24 | 2021-12-07 | 中国石油天然气股份有限公司 | Method for detecting demulsifier in oilfield sewage |
| CN115480016A (en) * | 2022-10-12 | 2022-12-16 | 中国科学院兰州化学物理研究所 | Liquid chromatography analysis and detection method of laurinol polyoxyethylene ether nonionic surfactant |
-
2019
- 2019-12-11 CN CN201911267080.6A patent/CN111307963A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112362768A (en) * | 2020-10-23 | 2021-02-12 | 北京民海生物科技有限公司 | Method for measuring content of Berol 185 in sample by using liquid chromatography tandem mass spectrometry |
| CN112362768B (en) * | 2020-10-23 | 2023-09-08 | 北京民海生物科技有限公司 | Method for measuring Berol 185 content in sample by utilizing liquid chromatography-tandem mass spectrometry |
| CN113759068A (en) * | 2021-08-24 | 2021-12-07 | 中国石油天然气股份有限公司 | Method for detecting demulsifier in oilfield sewage |
| CN113759068B (en) * | 2021-08-24 | 2022-09-13 | 中国石油天然气股份有限公司 | Method for detecting demulsifier in oilfield sewage |
| CN115480016A (en) * | 2022-10-12 | 2022-12-16 | 中国科学院兰州化学物理研究所 | Liquid chromatography analysis and detection method of laurinol polyoxyethylene ether nonionic surfactant |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111307963A (en) | Chromatographic detection method of nonionic surfactant | |
| Zuo et al. | Simultaneous determination of creatinine and uric acid in human urine by high-performance liquid chromatography | |
| CN103293243B (en) | Detection method and application of carboxy methyl lysine ingredient in food | |
| EP1962097A1 (en) | Mass spectrometric quantitative detection of methyl malonic acid and succinic acid using hilic on a zwitterionic stationary phase | |
| CN108802256B (en) | Method for detecting content of monoethanolamine | |
| CN101865886A (en) | Method for measuring residual quantity of chloramphenicol in propolis by using high performance liquid chromatography tandem mass spectrum | |
| CN103728398B (en) | A kind of Ion-pair Liquid Chromatography measures the method for dyeing and finishing auxiliaries for textile neutral line alkyl benzene sulfonate | |
| Rao et al. | Rapid separation and determination of process-related substances of paracetamol using reversed-phase HPLC with photo diode array as a detector | |
| CN102507819B (en) | Method for measuring hexabromocyclododecane in food contact material | |
| Liu et al. | Penicillin analyses by capillary electrochromatography-mass spectrometry with different charged poly (stearyl methacrylate–divinylbenzene) monoliths as stationary phases | |
| Deshmukh et al. | A review on analytical method development and validation by high performance liquid chromatography technique | |
| CN103175930B (en) | A kind of HPLC analytical method measuring sodium sulphite content | |
| Tiwari et al. | HPLC: a modern approach of development and validation | |
| CN107462643A (en) | The assay method of thiourea dioxide in a kind of food additives | |
| Salama et al. | Validated TLC and HPLC stability-indicating methods for the quantitative determination of dapsone | |
| CN110590612B (en) | Preparation method of high-purity L-PFOS and high-purity L-PFOS | |
| CN111830144A (en) | High performance liquid detection method for surfactant triton X-100 | |
| RU2653582C1 (en) | Method of high-efficient liquid chromatographic determination of concentrations of alkylphosphonic and/or o-alkylalkylphosphonic acids in aqueous solution | |
| Wang et al. | LC determination of trace short-chain organic acids in wheat root exudates under aluminum stress | |
| CN111122742B (en) | Method for detecting residual quantity of dimercaptopolyethylene glycol in sample to be detected | |
| CN111323503A (en) | Method for measuring content of compound amino acid injection | |
| Vuković et al. | One-step solid-phase UV spectrophotometric method for phenol determination in vaccines: Development and quality assessment | |
| CN112255347B (en) | Method for measuring ethirimol isomer | |
| Zaitsev et al. | A novel HPLC method for simultaneous determination of trimebutine, methylparaben and propylparaben in peroral medicines | |
| CN113484437B (en) | Method for determining ultra-trace halocarban in environmental water sample and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20200619 |
|
| WW01 | Invention patent application withdrawn after publication |