CN112098541A - Chromatographic analysis method for unsaturated fatty primary amine component - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000004587 chromatography analysis Methods 0.000 title claims abstract description 23
- 125000002924 primary amino group Chemical class [H]N([H])* 0.000 title claims description 12
- 238000004458 analytical method Methods 0.000 claims abstract description 38
- 238000001212 derivatisation Methods 0.000 claims abstract description 38
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 17
- 230000010933 acylation Effects 0.000 claims abstract description 6
- 238000005917 acylation reaction Methods 0.000 claims abstract description 6
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical group CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 33
- -1 polysiloxane Polymers 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 125000002668 chloroacetyl group Chemical group ClCC(=O)* 0.000 claims description 4
- 238000004817 gas chromatography Methods 0.000 claims description 3
- 238000002309 gasification Methods 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000001514 detection method Methods 0.000 claims description 2
- 150000003141 primary amines Chemical class 0.000 abstract description 31
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 abstract description 20
- 125000000217 alkyl group Chemical group 0.000 abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 abstract description 5
- 150000003139 primary aliphatic amines Chemical class 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 18
- 238000012360 testing method Methods 0.000 description 17
- 239000000126 substance Substances 0.000 description 6
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011981 development test Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 208000010727 head pressing Diseases 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000003760 tallow Substances 0.000 description 1
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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
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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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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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
- G01N2030/067—Preparation by reaction, e.g. derivatising the sample
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a chromatographic analysis method for unsaturated fatty primary amine components, which comprises the following steps: firstly, performing derivatization pretreatment on a sample, namely adding a proper amount of acylating reagent into an unsaturated fatty primary amine sample to perform acylation derivatization treatment; analyzing by a gas chromatograph, namely analyzing the prepared derivative by adopting a gas chromatograph analysis method; compared with the prior art, the method has the advantages that an unsaturated primary aliphatic amine sample is added with a proper amount of acylating reagent for acylation and derivatization, primary aliphatic amine is converted into acetamide with corresponding alkyl, and then the acetamide is analyzed by a gas chromatograph, so that the separation efficiency of chromatographic components is greatly improved, all unsaturated components with the same carbon chain can be effectively separated, such as C18:0, C18:1 and C18:2, can be accurately and quantitatively separated, the production control can be effectively guided, and the product quality is improved.
Description
Technical Field
The invention relates to the technical field of chromatographic analysis, in particular to a chromatographic analysis method for unsaturated fatty primary amine components.
Background
The components with the same carbon chain length in the higher unsaturated primary aliphatic amine products (such as tallow primary amine, oleic acid primary amine and the like) may contain a plurality of unsaturated components (such as C18:1 and C18:2 unsaturated components contained in C18 carbon chain components in oleic acid primary amine), and as the alkalinity and polarity of amino functional groups in primary amine molecules are very strong, chromatographic peaks are seriously trailing when chromatographic analysis is directly carried out on chromatographic columns with various polarities, so that the chromatographic column has extremely low separation efficiency and is difficult to accurately carry out quantification, namely, the primary amine is not suitable for being directly analyzed on the polar chromatographic columns.
Although a good chromatographic peak can be obtained by adopting a low-polarity or non-polar chromatographic column to directly analyze unsaturated primary amine, unsaturated components of the same carbon chain cannot be separated, a peak or a chromatographic peak with serious overlap is often formed, the distribution of the unsaturated components cannot be quantitatively obtained, and the development test and factory production are difficult to guide.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a chromatographic analysis method for an unsaturated fatty primary amine component, so as to solve the problem that the unsaturated fatty primary amine cannot be accurately quantitatively analyzed in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme: a chromatographic analysis method for unsaturated fatty primary amine components comprising the steps of:
firstly, performing derivatization pretreatment on a sample, namely adding a proper amount of acylating reagent into an unsaturated fatty primary amine sample to perform acylation derivatization treatment;
and step two, analyzing by using a gas chromatograph, wherein the prepared derivative is analyzed by using a gas chromatograph analysis method.
Compared with the prior art, the invention has the following beneficial effects:
according to the analysis method, an unsaturated primary aliphatic amine sample is added with a proper amount of acylation reagent for acylation derivatization, primary aliphatic amine is converted into acetamide with corresponding alkyl, and then the acetamide is analyzed by a gas chromatograph, so that the separation efficiency of chromatographic components is greatly improved, all unsaturated components with the same carbon chain can be effectively separated, such as C18:0, C18:1 and C18:2, can be accurately and quantitatively separated, the production control can be effectively guided, and the product quality is improved.
Further, in the first step, the prepared derivative is placed in a water bath environment for heating, and then gas chromatography analysis is performed.
Further, the temperature of the water bath environment is 78-83 ℃, and the heating time is 5-10 min.
Further, in the second step, the chromatographic column used in the gas chromatograph analysis method is a nitrile propyl polysiloxane column.
Further, in the second step, the detector adopted in the gas chromatograph analysis method is an FID detector, and the detection temperature is 290-300 ℃.
Further, in the second step, the temperature of the gasification chamber used in the gas chromatograph analysis method is 275-285 ℃.
Further, the column head pressure of the chromatographic column is 115-120 kPa.
Further, in the second step, the initial temperature of a column box adopted in the analysis method of the gas chromatograph is 150-155 ℃, the temperature is increased to 190-200 ℃ at the heating rate of 10-15 ℃/min, and then the temperature is increased to 235-240 ℃ at the heating rate of 5-8 ℃/min and is kept for about 25 min.
Further, the acylating agent is acetic anhydride or chloroacetyl.
Drawings
FIG. 1 is a chromatogram obtained by a prior art method;
FIG. 2 is a chromatogram obtained in the present method.
Detailed Description
The present invention will be described in further detail below by way of specific embodiments:
example 1
A chromatographic analysis method for unsaturated fatty primary amine components comprises the following specific test steps:
firstly, derivatization pretreatment of sample
Taking about 0.3g of unsaturated aliphatic primary amine sample, adding 2mL of acetic anhydride into a 15mL test tube, heating in a 78 ℃ water bath to melt the sample, heating for 5 min-10 min, and taking about 0.4 mu L of solution by a micro-injector to enter a gas chromatograph for analysis.
Selecting chemical reaction of derivatization treatment according to chemical properties of a sample and possible reactions, comprehensively considering factors such as derivatization reaction degree, influence of derivatization reagent on analysis, chromatographic column analysis and the like, selecting acetic anhydride as the derivatization reagent, converting unsaturated fatty primary amine into acetamide with corresponding alkyl, separating and analyzing derivatives by using a polar chromatographic column capable of separating unsaturated components, and indirectly analyzing the content of each unsaturated component in an unsaturated fatty primary amine sample by separating the derivatives.
Example 2
A chromatographic analysis method for unsaturated fatty primary amine components comprises the following specific test steps:
firstly, derivatization pretreatment of sample
About 0.3g of unsaturated aliphatic primary amine sample is added with 2mL of chloroacetyl in a 15mL test tube, the test tube is placed in a 78 ℃ water bath to be heated and melted, then the sample is heated for 5min, and about 0.4 mu L of solution is taken by a micro-syringe to enter a gas chromatograph for analysis.
Selecting chemical reaction of derivatization treatment according to chemical properties of a sample and possible reactions, comprehensively considering factors such as derivatization reaction degree, influence of derivatization reagent on analysis, chromatographic column analysis and the like, selecting acetic anhydride as the derivatization reagent, converting unsaturated fatty primary amine into acetamide with corresponding alkyl, separating and analyzing derivatives by using a polar chromatographic column capable of separating unsaturated components, and indirectly analyzing the content of each unsaturated component in an unsaturated fatty primary amine sample by separating the derivatives.
Example 3
A chromatographic analysis method for unsaturated fatty primary amine components comprises the following specific test steps:
firstly, derivatization pretreatment of sample
About 0.3g of unsaturated aliphatic primary amine sample is added with 1.5mL of acetic anhydride in a 20mL test tube, the test tube is placed in a water bath at 83 ℃ to be heated and melted, then the sample is heated for 10min, and about 0.4 mu L of solution is taken by a micro-syringe to enter a gas chromatograph for analysis.
Selecting chemical reaction of derivatization treatment according to chemical properties of a sample and possible reactions, comprehensively considering factors such as derivatization reaction degree, influence of derivatization reagent on analysis, chromatographic column analysis and the like, selecting acetic anhydride as the derivatization reagent, converting unsaturated fatty primary amine into acetamide with corresponding alkyl, separating and analyzing derivatives by using a polar chromatographic column capable of separating unsaturated components, and indirectly analyzing the content of each unsaturated component in an unsaturated fatty primary amine sample by separating the derivatives.
Example 4
A chromatographic analysis method for unsaturated fatty primary amine components comprises the following specific test steps:
firstly, derivatization pretreatment of sample
About 0.3g of unsaturated aliphatic primary amine sample is added with 1.5mL of chloracetyl in a 20mL test tube, the test tube is placed in a water bath at 83 ℃ to be heated and melted, then the sample is heated for 10min, and about 0.4 mu L of solution is taken by a micro-syringe to enter a gas chromatograph for analysis.
Selecting chemical reaction of derivatization treatment according to chemical properties of a sample and possible reactions, comprehensively considering factors such as derivatization reaction degree, influence of derivatization reagent on analysis, chromatographic column analysis and the like, selecting acetic anhydride as the derivatization reagent, converting unsaturated fatty primary amine into acetamide with corresponding alkyl, separating and analyzing derivatives by using a polar chromatographic column capable of separating unsaturated components, and indirectly analyzing the content of each unsaturated component in an unsaturated fatty primary amine sample by separating the derivatives.
Example 5
A chromatographic analysis method for unsaturated fatty primary amine components comprises the following specific test steps:
firstly, derivatization pretreatment of sample
About 0.3g of unsaturated aliphatic primary amine sample is added with 1.8mL of acetic anhydride into an 18mL test tube, the test tube is placed in a water bath at 80 ℃ to be heated and melted, then the sample is heated for 8min, and about 0.4 mu L of solution is taken by a micro-syringe to enter a gas chromatograph for analysis.
Selecting chemical reaction of derivatization treatment according to chemical properties of a sample and possible reactions, comprehensively considering factors such as derivatization reaction degree, influence of derivatization reagent on analysis, chromatographic column analysis and the like, selecting acetic anhydride as the derivatization reagent, converting unsaturated fatty primary amine into acetamide with corresponding alkyl, separating and analyzing derivatives by using a polar chromatographic column capable of separating unsaturated components, and indirectly analyzing the content of each unsaturated component in an unsaturated fatty primary amine sample by separating the derivatives.
Example 6
A chromatographic analysis method for unsaturated fatty primary amine components comprises the following specific test steps:
firstly, derivatization pretreatment of sample
About 0.3g of unsaturated aliphatic primary amine sample is added with 1.8mL of chloroacetyl in an 18mL test tube, the test tube is placed in a water bath at 80 ℃ to be heated and melted, then the sample is heated for 8min, and about 0.4 mu L of solution is taken by a micro-syringe to enter a gas chromatograph for analysis.
Selecting chemical reaction of derivatization treatment according to chemical properties of a sample and possible reactions, comprehensively considering factors such as derivatization reaction degree, influence of derivatization reagent on analysis, chromatographic column analysis and the like, selecting acetic anhydride as the derivatization reagent, converting unsaturated fatty primary amine into acetamide with corresponding alkyl, separating and analyzing derivatives by using a polar chromatographic column capable of separating unsaturated components, and indirectly analyzing the content of each unsaturated component in an unsaturated fatty primary amine sample by separating the derivatives.
Gas chromatography analysis of derivatives
Among them, the gas chromatograph analysis is the existing analysis technology, but the following reasonable adjustment is made to the chromatographic conditions of the gas chromatograph analysis in the process of the gas chromatograph analysis aiming at the performance of the primary amine derivative:
chromatographic conditions
1. A detector: FID, temperature 290-300 ℃.
2. A gasification chamber: the temperature is 275-285 ℃.
3. A chromatographic column: nitrile propyl polysiloxane column, 30 m.times.0.25 mm.times.0.25. mu.m.
4. Column head pressing: 115-120 kPa.
5. Temperature program: initial temperature of 150-155 deg.c, raising the temperature to 190-200 deg.c at 10 deg.c/min, raising the temperature to 235-240 deg.c at 5 deg.c/min and maintaining for 25 min.
Wherein, the qualitative analysis of the sample is carried out by a standard sample control method, and the quantitative analysis of the components is carried out by an area normalization method.
All of the unsaturated components with the same carbon chain in the chromatogram obtained by the analysis of the gas chromatograph can be effectively and independently presented by adjusting the previous data in the embodiments 1 to 6, so that the production control can be effectively guided, and the product quality can be improved. As is apparent from the comparison between FIG. 1 and FIG. 2, the component A in FIG. 1 is the unsaturated component C18:1, C18:2, etc. in the sample, and the chromatographic peaks thereof are overlapped; in fig. 2, B indicates unsaturated components such as C18:1 and C18:2 in the sample, and chromatographic peaks of the components are clearly separated.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (9)
1. A method for chromatographic analysis of an unsaturated fatty primary amine component comprising the steps of:
firstly, performing derivatization pretreatment on a sample, namely adding a proper amount of acylating reagent into an unsaturated fatty primary amine sample to perform acylation derivatization treatment;
and step two, analyzing by using a gas chromatograph, wherein the prepared derivative is analyzed by using a gas chromatograph analysis method.
2. A method according to claim 1 for chromatographic analysis of unsaturated fatty primary amine components characterized in that: in the first step, the prepared derivative is placed in a water bath environment for heating, and then gas chromatography analysis is performed.
3. A method according to claim 2 for chromatographic analysis of unsaturated fatty primary amine components characterized in that: the temperature of the water bath environment is 78-83 ℃, and the heating time is 5-10 min.
4. A method for the chromatographic analysis of an unsaturated fatty primary amine component according to any one of claims 1-3, characterized in that: in the second step, the chromatographic column adopted in the gas chromatograph analysis method is a nitrile propyl polysiloxane column.
5. A method for the chromatographic analysis of an unsaturated fatty primary amine component according to any one of claims 1-3, characterized in that: in the second step, the detector adopted in the gas chromatograph analysis method is an FID detector, and the detection temperature is 290-300 ℃.
6. A method for the chromatographic analysis of an unsaturated fatty primary amine component according to any one of claims 1-3, characterized in that: in the second step, the temperature of the gasification chamber adopted in the gas chromatograph analysis method is 275-285 ℃.
7. A method according to claim 4 for the chromatographic analysis of unsaturated fatty primary amine components characterized in that: the column head pressure of the chromatographic column is 115-120 kPa.
8. A method for the chromatographic analysis of an unsaturated fatty primary amine component according to any one of claims 1-3, characterized in that: in the second step, the initial temperature of a column box adopted in the analysis method of the gas chromatograph is 150-155 ℃, the temperature is increased to 190-200 ℃ at the heating rate of 10-15 ℃/min, and then the temperature is increased to 235-240 ℃ at the heating rate of 5-8 ℃/min and is kept for about 25 min.
9. A method according to claim 1 for chromatographic analysis of unsaturated fatty primary amine components characterized in that: the acylating agent is acetic anhydride or chloroacetyl.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331414A (en) * | 2000-06-28 | 2002-01-16 | 中国科学院大连化学物理研究所 | Method for analyzing resultants in reaction process for preparing low-grade lipoamine by liquefied ammonia catalysis |
| WO2016204854A1 (en) * | 2015-06-16 | 2016-12-22 | Agilent Technologies, Inc. | Compositions and methods for analytical sample preparation |
| CN110687235A (en) * | 2019-10-18 | 2020-01-14 | 贵州省烟草科学研究院 | Derivatization and back-extraction method for removing interference of primary amine and secondary amine in tertiary amine chiral chromatographic analysis |
-
2020
- 2020-08-31 CN CN202010900294.9A patent/CN112098541A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1331414A (en) * | 2000-06-28 | 2002-01-16 | 中国科学院大连化学物理研究所 | Method for analyzing resultants in reaction process for preparing low-grade lipoamine by liquefied ammonia catalysis |
| WO2016204854A1 (en) * | 2015-06-16 | 2016-12-22 | Agilent Technologies, Inc. | Compositions and methods for analytical sample preparation |
| CN110687235A (en) * | 2019-10-18 | 2020-01-14 | 贵州省烟草科学研究院 | Derivatization and back-extraction method for removing interference of primary amine and secondary amine in tertiary amine chiral chromatographic analysis |
Non-Patent Citations (3)
| Title |
|---|
| CHOU SL 等: "Gas chromatography-isotope dilution mass spectrometry preceded by liquid-liquid extraction and chemical derivatization for the determination of ketamine and norketamine in urine", 《JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES》 * |
| 彭万平 等: "不饱和脂肪伯胺酰化衍生法色谱分析初探", 《泸天化科技》 * |
| 肖道清 等: "固相萃取/气相色谱-质谱法对接触食品的塑料制品中24种芳香族伯胺迁移量的同时测定", 《分析测试学报》 * |
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Application publication date: 20201218 |