CN110763781A - High performance liquid chromatography detection method of 2-benzyl-2-dimethylamino-1- (4-morpholinylphenyl) butanone - Google Patents
High performance liquid chromatography detection method of 2-benzyl-2-dimethylamino-1- (4-morpholinylphenyl) butanone Download PDFInfo
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- CN110763781A CN110763781A CN201911078777.9A CN201911078777A CN110763781A CN 110763781 A CN110763781 A CN 110763781A CN 201911078777 A CN201911078777 A CN 201911078777A CN 110763781 A CN110763781 A CN 110763781A
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- benzyl
- dimethylamino
- butanone
- morpholinylphenyl
- performance liquid
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
- B01J20/286—Phases chemically bonded to a substrate, e.g. to silica or to polymers
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/047—Standards external
Abstract
The invention belongs to the technical field of analytical chemistry, and relates to a high performance liquid chromatography detection method of 2-benzyl-2-dimethylamino-1- (4-morpholinylphenyl) butanone. Separating by octadecyl bonded phase chromatographic column, isocratic eluting with acetonitrile and water, and detecting with ultraviolet detector. The method is simple and convenient, can quickly determine the content of the 2-benzyl-2-dimethylamino-1- (4-morpholinylphenyl) butanone, and has higher accuracy, stability and separation degree.
Description
Technical Field
The invention belongs to the technical field of analytical chemistry, and relates to a high performance liquid chromatography detection method of 2-benzyl-2-dimethylamino-1- (4-morpholinylphenyl) butanone, in particular to a high performance liquid chromatography detection method of 2-benzyl-2-dimethylamino-1- (4-morpholinylphenyl) butanone, which has high accuracy, stability and separation degree of chromatographic column separation of octadecyl bonding phase and detection of an ultraviolet detector.
Background
2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) butanone, 2-benzyl-2-dimethyllamino-4' -mor pholinothyropenone, CAS 119313-12-1, molecular formula C23H30N2O2The compound has a relative molecular weight of 366.5, is light yellow powder crystal, is dissolved in organic solvents such as toluene, acetone and the like, has a melting point of 110-115 ℃ and a boiling point of 528.8 ℃, is used for initiating the photopolymerization of free radicals, can be compounded with a proper coinitiator and is used for UV curing ink and coating.
At present, the detection standard of 2-benzyl-2-dimethylamino-1- (4-morpholinyl phenyl) butanone is not available at home and abroad. Therefore, a method for detecting the content of 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) butanone, which is simple to operate, high in sensitivity and accurate in quantification, is urgently needed to be established.
Disclosure of Invention
The invention aims to provide a high performance liquid chromatography detection method of 2-benzyl-2-dimethylamino-1- (4-morpholinylphenyl) butanone, which has high accuracy, stability and separation degree of octadecyl bonding phase chromatographic column separation and ultraviolet detector detection.
In order to realize the purpose of the invention, the technical scheme of the invention is as follows: injecting the standard solution into a high performance liquid chromatograph, collecting a chromatogram under the condition of setting an instrument, and quantifying by an external standard method; separating octadecyl bonding phase by chromatographic column, eluting with acetonitrile and water as mobile phase at 40 deg.C and 6: 4 volume ratio, detecting with ultraviolet detector at detection wavelength of 350nm, collecting spectrogram, and quantifying by external standard method, wherein the column flow is 1.0mL/min, the sample injection volume is 5 μ L.
Has the advantages that: the method can quickly determine the content of the 2-benzyl-2-dimethylamino-1- (4-morpholinylphenyl) butanone by adopting chromatographic column separation of an octadecyl bonding phase and ultraviolet detector detection, has the characteristic of high efficiency compared with the prior art (comparison documents: CN 102818874B, 2014.07.16) by optimizing the analysis conditions of an instrument, and realizes the detection of the 2-benzyl-2-dimethylamino-1- (4-morpholinylphenyl) butanone within 5 minutes. Has higher accuracy, stability and separation degree, and the method is simple and convenient.
Drawings
FIG. 12 high performance liquid chromatogram of benzyl-2-dimethylamino-1- (4-morpholinophenyl) butanone standard solution
Detailed Description
The present invention is further illustrated by the following examples, but is not limited thereto in any way, and any variations or modifications based on the teachings of the present invention are within the scope of the present invention.
Example one
The high performance liquid chromatograph is used in conjunction with ultraviolet detector.
Accurately weighing appropriate amount of standard substance (2-benzyl-2-dimethylamino-1- (4-morpholine benzene)Methyl ethyl ketone, CAS: 119313-12-1), dissolving acetonitrile and fixing volume to prepare a standard solution with the concentration of 5.0 mu g/mL. The chromatographic conditions employed were: inertsustain C18A chromatographic column; column temperature of 40 ℃; acetonitrile and water are used as mobile phases and are eluted isocratically according to the volume ratio of 6: 4; flow rate of 1.0 mL/min; 5 microliter sample injection volume; detecting by an ultraviolet detector, and detecting the wavelength by 350 nm. And injecting the standard solution into a high performance liquid chromatograph, and recording the chromatogram. As shown in figure 1, 2.008 min is the peak of 2-benzyl-2-dimethylamino-1- (4-morpholinylphenyl) butanone spectrum, the retention time is appropriate, and the peak shape symmetry is good.
Claims (1)
1. A high performance liquid chromatography detection method of 2-benzyl-2-dimethylamino-1- (4-morpholine phenyl) butanone is characterized in that octadecyl bonding phase chromatography column separation is carried out, the column temperature is 40 ℃, acetonitrile and water are used as mobile phases, isocratic elution is carried out according to the volume ratio of 6: 4, the column flow is 1.0mL/min, the sample injection volume is 5 mu L, an ultraviolet detector detects the sample injection volume, the detection wavelength is 350nm, a spectrogram is acquired, and the quantification is carried out by an external standard method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911078777.9A CN110763781A (en) | 2019-11-02 | 2019-11-02 | High performance liquid chromatography detection method of 2-benzyl-2-dimethylamino-1- (4-morpholinylphenyl) butanone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911078777.9A CN110763781A (en) | 2019-11-02 | 2019-11-02 | High performance liquid chromatography detection method of 2-benzyl-2-dimethylamino-1- (4-morpholinylphenyl) butanone |
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| CN110763781A true CN110763781A (en) | 2020-02-07 |
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| CN201911078777.9A Pending CN110763781A (en) | 2019-11-02 | 2019-11-02 | High performance liquid chromatography detection method of 2-benzyl-2-dimethylamino-1- (4-morpholinylphenyl) butanone |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2447715A1 (en) * | 2010-11-01 | 2012-05-02 | Agilent Technologies, Inc. | Method for forming polymeric porous layer open tubular columns by photopolymerisation with visible light |
| CN102818874A (en) * | 2012-08-31 | 2012-12-12 | 国家烟草质量监督检验中心 | Detection method of determining 16 types of photoinitiators in paper printing and packaging material |
| CN103837617A (en) * | 2014-03-16 | 2014-06-04 | 国家烟草质量监督检验中心 | Method for analyzing migration volume from photoinitiator to modified polyphenylene oxide (MPPO) in printed wrapping paper based on liquid chromatograph-tandem mass spectrometer (LC-MS/MS) technology |
| CN108358871A (en) * | 2018-02-01 | 2018-08-03 | 浙江扬帆新材料股份有限公司 | A kind of 2- benzyls -2- dimethylaminos -1-（4- morpholinyl phenyls）The synthetic method of butanone |
-
2019
- 2019-11-02 CN CN201911078777.9A patent/CN110763781A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2447715A1 (en) * | 2010-11-01 | 2012-05-02 | Agilent Technologies, Inc. | Method for forming polymeric porous layer open tubular columns by photopolymerisation with visible light |
| CN102818874A (en) * | 2012-08-31 | 2012-12-12 | 国家烟草质量监督检验中心 | Detection method of determining 16 types of photoinitiators in paper printing and packaging material |
| CN103837617A (en) * | 2014-03-16 | 2014-06-04 | 国家烟草质量监督检验中心 | Method for analyzing migration volume from photoinitiator to modified polyphenylene oxide (MPPO) in printed wrapping paper based on liquid chromatograph-tandem mass spectrometer (LC-MS/MS) technology |
| CN108358871A (en) * | 2018-02-01 | 2018-08-03 | 浙江扬帆新材料股份有限公司 | A kind of 2- benzyls -2- dimethylaminos -1-（4- morpholinyl phenyls）The synthetic method of butanone |
Non-Patent Citations (2)
| Title |
|---|
| T. JUNG等: "Multi-analyte methods for the detection of photoinitiators and amine synergists in food contact materials and foodstuffs – Part I: HPLC-DAD screening of materials", 《FOOD ADDITIVES & CONTAMINANTS: PART A》 * |
| 张建莹等: "液相色谱－串联质谱法测定牛奶中11种光引发剂残留量", 《江西农业学报》 * |
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