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Determination method of free amine content in fatty amidopropyl betaine

A fatty amidopropyl beet, detection method technology, applied in the field of chemical analysis, can solve problems such as long retention time, poor repeatability, complex sample extraction, etc.

Active Publication Date: 2019-11-05
GUANGZHOU TINCI MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these two methods have the problems of complex sample extraction, low accuracy and poor repeatability of the analysis results after extraction.
There is a method for analyzing fatty amide compounds by liquid chromatography, but when analyzing long-chain fatty amide samples, the sample retention time is longer and requires 20 minutes, which is not conducive to the improvement of sample detection efficiency

Method used

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  • Determination method of free amine content in fatty amidopropyl betaine
  • Determination method of free amine content in fatty amidopropyl betaine
  • Determination method of free amine content in fatty amidopropyl betaine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Instruments and experimental drugs: Shimadzu LC-10AT high performance liquid chromatography, SPD-20A detector (ultraviolet detector, quantitative loop 20μL), ultrasonic cleaner, electronic balance with a precision of 0.0001g, pH meter, pipette , graduated cylinder, volumetric flask, 0.45μm organic and aqueous filter membrane, solvent filter, chromatographic column with reverse bonded C18 filler, acetonitrile (HPLC), phosphoric acid (AR), sodium dihydrogen phosphate (AR) , triethylamine (AR), C12-C18 free amine standard sample (98.5%), self-made ultrapure water (18.2MΩ).

[0035] Mobile phase A: Accurately weigh 1.56g of sodium dihydrogen phosphate (accurate to 0.0001g) into a 1000mL beaker, add 1000mL of ultrapure water, stir well until the solid is completely dissolved to prepare a 0.01mol / L solution, add 1mL of triethylamine solution , and then use phosphoric acid to adjust the pH of the solution to 2.3, and filter it with a 0.45 μm water filter membrane for later use...

Embodiment 2

[0041] Mobile phase: add the mobile phase B in Example 1 to the mobile phase A according to the ratio of mobile phase B:A=50:50, shake well and degas it by ultrasonic for 20 minutes for later use.

[0042] Accurately weigh C12 free amine (RCONHCH 2 CH 2 CH 2 N(CH 3 ) 2 , R is a C11 alkyl) standard sample 0.50g (accurate to 0.0001g) is placed in a 50mL volumetric flask, and the mobile phase is used to prepare a 10mg / mL standard solution for later use, and then 500μL of the standard solution is placed in a 25mL volumetric flask , dilute to the mark with mobile phase, and shake well as the standard solution to be tested.

[0043] Set the detection conditions of liquid chromatography: the chromatographic column is a chromatographic column with reverse bonded C18 as filler, the detection wavelength is 210nm, the flow rate is 1.2mL / min, the column temperature is 30°C, and the injection volume is 20 μL. After the instrument is stable, inject the standard solution of C12 free ami...

Embodiment 3

[0045] Mobile phase: add the mobile phase B in Example 1 to the mobile phase A according to the ratio of mobile phase B:A=50:50, shake well and degas it by ultrasonic for 20 minutes for later use.

[0046] Accurately weigh C18 free amine (RCONHCH 2 CH 2 CH 2 N(CH 3 ) 2 , R is a C17 alkyl) standard sample 0.50g (accurate to 0.0001g) is placed in a 50mL volumetric flask, and the mobile phase is used to prepare a 10mg / mL standard solution after constant volume, and then 500μL of the standard solution is placed in a 25mL volumetric flask , dilute to the mark with mobile phase, and shake well as the standard solution to be tested.

[0047] Set the detection conditions of liquid chromatography: the chromatographic column is a chromatographic column with reverse bonded C18 as filler, the detection wavelength is 210 nm, the flow rate is 0.6 mL / min, the column temperature is 50 ° C, and the injection volume is 20 μL. After the instrument is stable, inject the standard solution of ...

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Abstract

The invention relates to a method for detecting the content of free amine in fattyamidopropyl betaine. Detection is conducted by means of the high performance liquid chromatography. The method comprises the following steps that firstly, a standard solution is prepared; secondly, a to-be-detected solution is prepared; thirdly, determination is conducted, wherein the standard solution is drawn precisely and determined by means of the high performance liquid chromatography, and a standard curve is plotted according to a detection result; the to-be-detected solution is drawn precisely and determined by means of the high performance liquid chromatography, and according to a detection result and the standard curve, the free amine residue in the sample is calculated. When the content of the free amine in fattyamidopropyl betaine is detected by means of the detection method, the content of the C12-C18 free amine can be determined, and the method has the advantages that quick determination is achieved, the simple is easy to prepare, and the detection results are stable and high in repeatability.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a method for detecting free amine content in fatty amidopropyl betaine. Background technique [0002] C12-C18 fatty amidopropyl dimethyl tertiary amine is mainly used in the production of amphoteric surfactants, amine oxides, betaines and quaternary ammonium salts. It is a chemical raw material used in large quantities, but there are often a small amount of it in the products produced Unreacted free amine. Free amines are allowed to exist within a safe range (<0.5%) in general products. [0003] At present, the methods for detecting free amine mainly include chemical titration and gas chromatography. The chemical titration method mainly uses the acid standard solution to titrate the free amine components in the sample to achieve the purpose of quantitative determination. Gas chromatography is to separate the free amine from other components by using a gas chromato...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 钟国祯吴海龙孙伏恩罗海英户献雷
Owner GUANGZHOU TINCI MATERIALS TECH