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Analysis of Amino Compounds by Precolumn Derivatization with Dimethoxybenzenesulfonyl Chloride

A technology of dimethoxybenzenesulfonyl chloride and amino compounds, applied in the field of analytical chemistry, can solve the problems of easy decomposition of derivatives, inability to detect secondary amino acids, unstable derivatives, etc., and achieve stable derivative products and high sensitivity , the effect of short reaction time

Inactive Publication Date: 2011-12-21
NANJING TECH UNIV
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0002] Pre-column derivatization reversed-phase high-performance liquid chromatography (RP-HPLC) is a common method to improve the sensitivity of the analysis of some amino compounds without chromophores, such as amino acids, and the reagents used for pre-column derivatization of amino acids have been reported so far. There are many, but there are some problems to some extent, such as: o-phthalaldehyde (OPA) can only react with primary amino acids, cannot detect secondary amino acids, and the derivatives are unstable; benzyl isothiocyanate (PITC) derivative operation Complicated, it is necessary to vacuum the excess solvent after derivatization; fluorenylmethyl chloroformate (FMOC-Cl) needs to extract the remaining derivatization reagent in the reaction process to terminate the derivatization reaction, and the derivatives are prone to decomposition; dansyl chloride ( Dansyl-Cl) reacts with all amino acids including imino groups, which affects quantification; after derivatization of dinitrofluorobenzene (FDNB), interference by-products are generated, and the reactant needs to be removed by pumping dry method [Mou Shifen, in Hong. Research progress of amino acid analysis methods. [J] Review and Progress of Analytical Chemistry, 2005, 3(33): 398-404]

Method used

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  • Analysis of Amino Compounds by Precolumn Derivatization with Dimethoxybenzenesulfonyl Chloride
  • Analysis of Amino Compounds by Precolumn Derivatization with Dimethoxybenzenesulfonyl Chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Experimental steps:

[0013] Use borax buffer solution (0.35M, pH 8.1) to prepare a glyphosate solution with a concentration of 0.31mg / mL, take 1mL of this solution and 0.5mL concentration of 3.47mg / mL 2,5-dimethoxybenzenesulfonyl chloride solution ( dissolved in ethanol) and mixed, derivatized at 45°C for 10 minutes, cooled in an ice-water bath, referring to the instrument and chromatographic conditions, mobile phase methanol, acetonitrile and phosphate buffer solution (pH=5.8, 0.05mol / L) volume ratio 15:5:80; flow rate 1.0mL / min; column temperature 25°C; detection wavelength 235nm.

Embodiment 2

[0015] Experimental steps:

[0016] Use borax buffer solution (0.20M, pH10.7) to prepare a glycine solution with a concentration of 1.0 mg / mL, take 3 mL of this solution and 1.5 mL of a 18.92 mg / mL 2,5-dimethoxybenzenesulfonyl chloride solution (methanol dissolved) and mixed, derivatized at 35°C for 15 minutes, then cooled in an ice-water bath. Referring to the instrument and chromatographic conditions, the volume ratio of the mobile phase methanol, acetonitrile and phosphate buffer solution (pH=5.5, 0.02mol / L) was 20:10:70; flow rate 1.0mL / min; column temperature 30°C; detection wavelength 230nm.

Embodiment 3

[0018] Experimental steps:

[0019] Use borax buffer solution (0.30M, pH 10) to prepare a proline solution with a concentration of 0.23 mg / mL, take 1 mL of this solution and 0.5 mL of a 4.72 mg / mL 2,5-dimethoxybenzenesulfonyl chloride solution ( dissolved in ethanol) mixed, derivatized at 28°C for 15 minutes, cooled in an ice-water bath, referring to the instrument and chromatographic conditions, the mobile phase methanol, acetonitrile and phosphate buffer solution (pH=6.9, 0.02mol / L) volume ratio 18:15:67; flow rate 0.9mL / min; column temperature 35°C; detection wavelength 220nm.

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Abstract

The invention discloses a pre-column derivatization method for high-performance liquid chromatography for analyzing amino compounds, and belongs to the technical field of analytical chemistry. The process is as follows: prepare the sample solution with a borax buffer solution with a pH of 8.0 to 11.5 and a concentration of 0.05 to 0.35M for the primary or secondary or primary and secondary amino compound samples, and add dimethoxybenzenesulfonyl chloride Methanol or ethanol or acetonitrile solution, mix well, conduct derivatization reaction at 25-45°C for 10-40 minutes, cool in ice-water bath, filter and inject samples into full-performance liquid chromatography, use ultraviolet detector to detect the derivatization of amino compounds Derivatives were analyzed quantitatively. The invention has the advantages of simple derivation reaction operation, short reaction time, high sensitivity, simultaneous derivation of primary and secondary amine compounds, no need to remove excess reagents after derivation, stable derivatized products, low derivatization reaction temperature, and is especially suitable for the analysis of biological samples.

Description

technical field [0001] The invention relates to a pre-column derivatization method of amino compounds, belonging to the technical field of analytical chemistry. Background technique [0002] Pre-column derivatization reversed-phase high-performance liquid chromatography (RP-HPLC) is a common method to improve the sensitivity of the analysis of some amino compounds without chromophores, such as amino acids, and the reagents used for pre-column derivatization of amino acids have been reported so far. There are many, but there are some problems to some extent, such as: o-phthalaldehyde (OPA) can only react with primary amino acids, cannot detect secondary amino acids, and the derivatives are unstable; benzyl isothiocyanate (PITC) derivative operation Complicated, it is necessary to vacuum the excess solvent after derivatization; fluorenylmethyl chloroformate (FMOC-Cl) needs to extract the remaining derivatization reagent in the reaction process to terminate the derivatization r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06
Inventor 刘晓宁李寿椿方芳魏荣卿
Owner NANJING TECH UNIV
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