CN101692074A - Method for analyzing fatty amide compounds on basis of liquid chromatography - Google Patents
Method for analyzing fatty amide compounds on basis of liquid chromatography Download PDFInfo
- Publication number
- CN101692074A CN101692074A CN200910093228A CN200910093228A CN101692074A CN 101692074 A CN101692074 A CN 101692074A CN 200910093228 A CN200910093228 A CN 200910093228A CN 200910093228 A CN200910093228 A CN 200910093228A CN 101692074 A CN101692074 A CN 101692074A
- Authority
- CN
- China
- Prior art keywords
- chain
- long
- chromatographic column
- moving phase
- water
- 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.)
- Pending
Links
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention provides a method for determining long-chain [C8-C24] fatty amide compounds on the basis of liquid chromatography (LC). The method is characterized in that high-purity spherical silica gel particles are reverse-bonded with chromatographic column with C18 as filler; and water-organic polar solvent with the volume ratio being 80:20-50:50 is taken as a mobile phase containing organic acid. The method comprises the following steps: (1) sampling a proper amount of long-chain [C8-C24] fatty amide compounds, and dissolving the sample in water, to prepare 0.1-5mg of sample solution out of 1ml of the long-chain [C8-C24] fatty amide compounds; (2) setting the flow rate of the mobile phase as 0.5-1.5ml/min, the detection wavelength as 200-260nm and the temperature of the chromatographic column box as 25-50 DEG C; and (3) injecting 10-40 mu l of the sample solution in Step (1) into the high-performance liquid chromatograph, so as to finish the analysis of long-chain [C8-C24] fatty amide compounds.
Description
Technical field
The invention belongs to the analytical chemistry field, be specifically related to the method that a kind of liquid chromatography analysis is measured long-chain (C8～24) fatty acyl amide compound.
Background technology
The analytical approach of long chain fatty acyl amide compound mainly contains electricity spectrographic method and red, orange, green, blue, yellow (ROGBY).Electricity spectrographic method medium ultraviolet absorption spectrum, infrared absorption spectrum, nuclear magnetic resonance spectrum and mass spectrum have constituted the Spectrum Analysis of organic compound together, are the strong tool of identifying and measure organic constitution and qualitative analysis at present.Long chain fatty acyl amide compound can adopt infra-red sepectrometry that it is carried out qualitative analysis because it has the amide group structure; But, adopt infra-red sepectrometry to be difficult to it is carried out quantitative test.For convenient, efficiently long chain fatty acyl amide compound is carried out qualitative and quantitative analysis, must adopt red, orange, green, blue, yellow (ROGBY).
Red, orange, green, blue, yellow (ROGBY) comprises vapor-phase chromatography and liquid phase chromatography.The analytic target of vapor-phase chromatography is the material that has enough volatile grade and thermal stability under column temperature, and therefore, it is only limited to lower compound of analytical gas and boiling point and volatile derivatives and relative molecular mass less than 400 nonionic compound.And high performance liquid chromatography (HPLC) is wide to the applicability of sample, is not subjected to the restriction of analytic target volatility and thermal stability, can analyze relative molecular mass greater than 400 organism.
HPLC is quick, efficient, a sensitive isolation technics that grew up in recent years, it is not subjected to the restriction of sample volatility and relative molecular mass, can be used for that compartment analysis higher boiling, relative molecular mass are big, the organic compound of poor heat stability, also can be used for the compartment analysis of various ions; HPLC not only can utilize separated component polarity difference, also can utilize the difference of affinity between the difference of difference, ion-exchange capacity of component molecular dimension size and biomolecule to separate.
Summary of the invention
The object of the present invention is to provide the efficient liquid-phase chromatography method of a kind of assay determination long-chain (C8～24) fatty acyl amide compound, thereby realize the qualitative and quantitative analysis of long-chain (C8～24) fatty acyl amide compound, for long-chain (C8～24) fatty acyl amide compound provides the good detection means.
The present invention is the method that a kind of liquid chromatography analysis is measured long-chain (C8～24) fatty acyl amide compound, it is characterized in that:
With high-purity ball-type aerosil particles, inverse bonded C18 is the chromatographic column of filler, is moving phase with water-organic polar solvent, wherein comprises organic acid in the moving phase;
Chromatographic column is selected from the chromatographic column that model is ZORBAX Eclipse XDB-C18;
Described organic solvent is selected from following compound: methyl alcohol, acetonitrile, tetrahydrofuran, and wherein organic solvent is preferably methyl alcohol;
Water-organic polar solvent volume ratio is 80: 20～50: 50;
Organic acid in the described moving phase is selected from formic acid, acetate or trifluoroacetic acid;
To account for the volume ratio of water be 0.1～5% to organic acid concentration (v/v) in the described moving phase;
The method that described liquid chromatography analysis is measured long-chain (C8～24) fatty acyl amide compound comprises following steps:
(1) it is an amount of to get long-chain (C8～24) fatty acyl amide compound sample, the water sample dissolution, and be configured to the sample solution that every 1ml contains long-chain (C8～24) fatty acyl amide compound 0.1～5mg;
(2) flow velocity that moving phase is set is 0.5～1.5ml/min, and the detection wavelength is 200～260nm, and chromatographic column post oven temperature, degree is 25～50 ℃;
(3) get sample solution 10～40 μ l of (1), inject high performance liquid chromatograph, finish the analysis of long-chain (C8～24) fatty acyl amide compound.
According to method of the present invention, the flow velocity of described moving phase is preferably 1ml/min.
According to method of the present invention, described detection wavelength is preferably and is 254nm.
According to method of the present invention, described chromatographic column post oven temperature, degree is preferably 35 ℃.
The present invention adopts ZORBAX Eclipse XDB-C18 reverse-phase chromatographic column, effectively assay determination long-chain (C8～24) fatty acyl amide compound; Select the water-soluble sample of separating for use, guaranteed the stability of solution; Select sampling volume 20 μ l for use, 35 ℃ of column temperatures have improved the symmetry of chromatographic peak.The invention solves the qualitative and quantitative analysis problem of long-chain (C8～24) fatty acyl amide compound, thereby guaranteed the dose controlled in long-chain (C8～24) the fatty acyl amide compound use.
Description of drawings
The liquid chromatogram of Fig. 1 long-chain (C12) fatty acid amide standard items.
The liquid chromatogram of Fig. 2 long-chain (C24) fatty acid amide standard items.
The liquid chromatogram of Fig. 3 long-chain (C8) fatty acid amide standard items.
The liquid chromatogram of Fig. 4 long-chain (C12) fatty acid amide standard items.
Embodiment
Embodiment 1,
Instrument and condition
U.S. Agilent 1200 type high performance liquid chromatograph and workstations; Hand sampling; With ZORBAXEclipse XDB-C18 (4.6 * 150mm, 5 μ m) is chromatographic column; Ultraviolet detection wavelength 260nm; With methyl alcohol: water (0.1% formic acid)=50: 50 is moving phase; Flow velocity is l ml/min; 25 ℃ of column temperatures; Sampling volume: 40 μ l
Experimental procedure
Get the about 10mg of long-chain (C12) fatty acid amide standard items, place the 100ml volumetric flask, be dissolved in water and be diluted to scale, shake up, as solution to be measured.
Get solution to be measured, carry out liquid-phase chromatographic analysis, the results are shown in Figure 1, t by above-mentioned condition
ProtectThe pairing peak of=20.211min is long-chain (C12) fatty acid amide characteristic peak.
Instrument and condition
U.S. Agilent 1200 type high performance liquid chromatograph and workstations; Hand sampling; With ZORBAXEclipse XDB-C18 (4.6 * 150mm, 5 μ m) is chromatographic column; Ultraviolet detection wavelength 200nm; With tetrahydrofuran: water (5% acetate)=80: 20 is moving phase; Flow velocity is 1.5ml/min; 50 ℃ of column temperatures; Sampling volume: 10 μ l
Experimental procedure
Get the about 500mg of long-chain (C24) fatty acid amide standard items, put in the 100ml volumetric flask, be dissolved in water and be diluted to scale, shake up, as solution to be measured.
Get solution to be measured, carry out liquid-phase chromatographic analysis, the results are shown in as Fig. 2 t by above-mentioned condition
ProtectThe pairing peak of=17.171min is long-chain (C24) fatty acid amide characteristic peak.
Embodiment 3,
Instrument and condition
U.S. Agilent 1200 type high performance liquid chromatograph and workstations; Hand sampling; With ZORBAXEclipse XDB-C18 (4.6 * 150mm, 5 μ m) is chromatographic column; Ultraviolet detection wavelength 220nm; With acetonitrile: water (1% trifluoroacetic acid)=60: 40 is moving phase; Flow velocity is 0.5ml/min; 35 ℃ of column temperatures; Sampling volume: 25 μ l
Experimental procedure
Get the about 100mg of long-chain (C8) fatty acid amide standard items, put in the 100ml volumetric flask, be dissolved in water and be diluted to scale, shake up, as solution to be measured.
Get solution to be measured, carry out liquid-phase chromatographic analysis, the results are shown in as Fig. 3 t by above-mentioned condition
ProtectThe pairing peak of=20.232min is long-chain (C8) fatty acid amide characteristic peak.
Embodiment 4,
Instrument and condition
U.S. Agilent 1200 type high performance liquid chromatograph and workstations; Hand sampling; With ZORBAXEclipse XDB-C18 (4.6 * 150mm, 5 μ m) is chromatographic column; Ultraviolet detection wavelength 254nm; With methyl alcohol: water (0.1% formic acid)=50: 50 is moving phase; Flow velocity is 1ml/min; 35 ℃ of column temperatures; Sampling volume: 20 μ l
Experimental procedure
Get the about 10mg of long-chain (C12) fatty acid amide standard items, put in the 100ml volumetric flask, be dissolved in water and be diluted to scale, shake up, as solution to be measured.
Get solution to be measured, carry out liquid-phase chromatographic analysis, the results are shown in as Fig. 4 t by above-mentioned condition
ProtectThe pairing peak of=20.110min is long-chain (C12) fatty acid amide characteristic peak.
Claims (2)
1. a liquid chromatography analysis is measured the method for long-chain [C8～24] fatty acyl amide compound, it is characterized in that:
With high-purity ball-type aerosil particles, inverse bonded C18 is the chromatographic column of filler, is moving phase with water-organic polar solvent, wherein comprises organic acid in the moving phase;
Chromatographic column is selected from the chromatographic column that model is ZORBAX Eclipse XDB-C18;
Described organic solvent is selected from following compound: methyl alcohol, acetonitrile, tetrahydrofuran;
Water-organic polar solvent volume ratio is 80: 20～50: 50;
Organic acid in the described moving phase is selected from formic acid, acetate or trifluoroacetic acid;
To account for the volume ratio of water be 0.1～5% to organic acid concentration v/v volume ratio in the described moving phase;
The method that described liquid chromatography analysis is measured long-chain [C8～24] fatty acyl amide compound comprises following steps:
(1) it is an amount of to get long-chain [C8～24] fatty acyl amide compound sample, the water sample dissolution, and be configured to the sample solution that every 1ml contains long-chain [C8～24] fatty acyl amide compound 0.1～5mg;
(2) flow velocity that moving phase is set is 0.5～1.5ml/min, and the detection wavelength is 200～260nm, and chromatographic column post oven temperature, degree is 25～50 ℃;
(3) get sample solution 10～40 μ l of (1), inject high performance liquid chromatograph, finish the analysis of long-chain [C8～24] fatty acyl amide compound.
2. method according to claim 1, wherein said organic solvent are methyl alcohol; The flow velocity of described moving phase is 1ml/min; Described detection wavelength is 254nm; Described chromatographic column post oven temperature, degree is 35 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910093228A CN101692074A (en) | 2009-09-23 | 2009-09-23 | Method for analyzing fatty amide compounds on basis of liquid chromatography |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910093228A CN101692074A (en) | 2009-09-23 | 2009-09-23 | Method for analyzing fatty amide compounds on basis of liquid chromatography |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101692074A true CN101692074A (en) | 2010-04-07 |
Family
ID=42080782
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910093228A Pending CN101692074A (en) | 2009-09-23 | 2009-09-23 | Method for analyzing fatty amide compounds on basis of liquid chromatography |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101692074A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770762A (en) * | 2016-12-20 | 2017-05-31 | 广州天赐高新材料股份有限公司 | The detection method of free amine content in fattyamidopropyl betaine |
| CN114544802A (en) * | 2022-01-21 | 2022-05-27 | 河北科技大学 | High performance liquid chromatography analysis method of acrylamide resin monomer |
| CN114544802B (en) * | 2022-01-21 | 2024-05-31 | 河北凯诺中星科技有限公司 | High performance liquid chromatography analysis method for acrylamide resin monomer |
-
2009
- 2009-09-23 CN CN200910093228A patent/CN101692074A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770762A (en) * | 2016-12-20 | 2017-05-31 | 广州天赐高新材料股份有限公司 | The detection method of free amine content in fattyamidopropyl betaine |
| CN106770762B (en) * | 2016-12-20 | 2019-11-05 | 广州天赐高新材料股份有限公司 | The detection method of free amine content in fattyamidopropyl betaine |
| CN114544802A (en) * | 2022-01-21 | 2022-05-27 | 河北科技大学 | High performance liquid chromatography analysis method of acrylamide resin monomer |
| CN114544802B (en) * | 2022-01-21 | 2024-05-31 | 河北凯诺中星科技有限公司 | High performance liquid chromatography analysis method for acrylamide resin monomer |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Kosikowska et al. | Review of the determination of pesticide residues in ambient air | |
| Wang et al. | Magnetic solid-phase extraction and determination of puerarin in rat plasma using C18-functionalized magnetic silica nanoparticles by high performance liquid chromatography | |
| CN205374391U (en) | Toxin detects uses solid phase extraction column | |
| US10514365B2 (en) | Cooling-assisted inside needle capillary adsorption trap device for analyzing complex solid samples using nano-sorbent | |
| CN107884493A (en) | The method of short chain chlorinated paraffin in comprehensive two dimensional gas chromatography flying time mass spectrum analysis environmental sample | |
| JP2009500638A (en) | Method for analyzing pesticide residues in plant samples | |
| West et al. | Gas-liquid chromatographic analysis applied to air pollution. Sampling | |
| Chen et al. | Dynamic ultrasound-assisted extraction coupled on-line with solid support derivatization and high-performance liquid chromatography for the determination of formaldehyde in textiles | |
| Fan et al. | Design and application of Hadamard-injectors coupled with gas and supercritical fluid sample collection systems in Hadamard transform-gas chromatography/mass spectrometry | |
| Jouyban et al. | Molecularly imprinted polymer based-solid phase extraction combined with dispersive liquid–liquid microextraction using new deep eutectic solvent; selective extraction of valproic acid from exhaled breath condensate samples | |
| Yang et al. | Dynamic ultrasonic nebulisation extraction coupled with headspace ionic liquid‐based single‐drop microextraction for the analysis of the essential oil in Forsythia suspensa | |
| CN105548431B (en) | Detect the method for oxamyl and oxamyl oxime residual quantity in vegetables/fruit simultaneously | |
| Aly et al. | Green chromatography and related techniques | |
| CN102798682B (en) | Method for determination of flumethrin in garlic or garlic product | |
| CN103123345B (en) | Method for rapidly detecting phenoxyacetic acid herbicide in soil | |
| CN110057959A (en) | A kind of analysis method of the high effective liquid chromatography for measuring Febustat intermediate in relation to substance | |
| CN104897824B (en) | The gel chromatographic columns of a kind of gas chromatography mass spectrometry detection PBDE and metabolite thereof and detection method thereof | |
| Cheng et al. | Applications of Hadamard transform-gas chromatography/mass spectrometry to online detection of exhaled breath after drinking or smoking | |
| CN101692074A (en) | Method for analyzing fatty amide compounds on basis of liquid chromatography | |
| CN105823741A (en) | Air for detecting content of butyraldehyde in air | |
| CN104502486A (en) | Method for determining methyl vanillin and ethyl vanillin in milk powder by adopting headspace-solid phase microextraction technology | |
| Hackett et al. | Extraction and analysis of clonazepam and 7-aminoclonazepam in whole blood using a dual internal standard methodology | |
| Wu et al. | Solid-phase microextraction followed by gas chromatography-mass spectrometry analysis of the volatile components of Flos Chrysanthemi indici in different growing areas | |
| CN101846660B (en) | Determination method of trace furadan | |
| Li et al. | Ultrasonic nebulization extraction coupled with headspace hollow fiber microextraction of pesticides from root of Panax ginseng CA Mey. |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20100407 |