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Method for efficiently detecting aliphatic diamine

An aliphatic diamine, high-efficiency technology, applied in the biological field, can solve the problems of poor repeatability, weak sensitivity, cumbersome process, etc., and achieve the effect of improving detection efficiency and accuracy, sensitivity and stability, and fewer by-products

Inactive Publication Date: 2021-10-22
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the detection method of pentamethylenediamine mainly consists of 2,4-dinitrofluorobenzene (1-Fluoro-2,4-dinitrobenzene) (CN105316270B), dansyl chloride (Dansyl chloride) (CN106011216A) as pre-column derivatizers, respectively by Detect by HPLC and HPLC-MS, these two derivatizing agents have problems such as strong background interference, weak sensitivity and poor repeatability; Or derivatize by benzoyl chloride (Benzoyl Chloride) (CN102424811A), extract with ether, detect through HPLC; Or derivatize by trinitrobenzenesulfonic acid (Picrylsulfonic acid solution) (CN107177641A), extract with toluene, and read the absorbance value at 340nm by microplate reader, these two methods need to go through extraction, the process is loaded down with trivial details, and detection is not sensitive enough

Method used

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  • Method for efficiently detecting aliphatic diamine
  • Method for efficiently detecting aliphatic diamine
  • Method for efficiently detecting aliphatic diamine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 600 μL 50 mM pH=9 borate buffer, 200 μL methanol, 60 μL 0.0001 / 0.3125 / 0.625 / 1.25 / 2.5 / 5 / 10 / 20 mM 1,5-pentanediamine, 130 μL ultrapure water and 10 μL 1M ethoxylate to the reaction system Diethyl methylene malonate (DEEMM) was reacted at room temperature for 10 minutes, and transferred to 70°C for 2 hours to complete the reaction of DEEMM. The derivatized product was detected by reversed-phase high performance liquid chromatography with an ultraviolet (nm) detector. Wherein mobile phase A: 100% acetonitrile; mobile phase B: 25mMpH=4.8 sodium acetate buffer solution; flow rate 0.5mL / min, using gradient elution 0min A:B is 20:80; 2min A:B is 25:75; 27min A:B is 62.5:37.5; 27.01min A:B is 20:80; 37min A:B is 20:80; 37.01min ends the test. Detection column: C18 column (Shim-pack GIST-HP-C18 column, 2.1×100mm, 3m particle size); detection temperature: 35°C; injection volume: 5μL, detector: SPD-20A diode array detector; wavelength: 284nm. Calculate the standard curve by 1...

Embodiment 2

[0036] Add 600 μL 50 mM pH=9 boric acid buffer, 200 μL methanol, 60 μL 0.0001 / 0.3125 / 0.625 / 1.25 / 2.5 / 5 / 10 / 20 mM 1,4-butanediamine, 130 μL ultrapure water and 10 μL 1M ethoxylate to the reaction system Diethyl methylene malonate (DEEMM) was reacted at room temperature for 10 minutes, and transferred to 70°C for 2 hours to complete the reaction of DEEMM. The derivatized product was detected by reversed-phase high performance liquid chromatography with an ultraviolet (nm) detector. Wherein mobile phase A: 100% acetonitrile; mobile phase B: 25mMpH=4.8 sodium acetate buffer solution; flow rate 0.5mL / min, using gradient elution 0min A:B is 20:80; 2min A:B is 25:75; 27min A:B is 62.5:37.5; 27.01min A:B is 20:80; 37min A:B is 20:80; 37.01min ends the test. Detection column: C18 column (Shim-pack GIST-HP-C18 column, 2.1×100mm, 3m particle size); detection temperature: 35°C; injection volume: 5μL, detector: SPD-20A diode array detector; wavelength: 284nm. By 1,4-butanediamine peak area...

Embodiment 3

[0038]Add 600 μL 50 mM pH=9 borate buffer, 200 μL methanol, 60 μL 0.0001 / 0.3125 / 0.625 / 1.25 / 2.5 / 5 / 10 / 20 mM 1,6-hexanediamine, 130 μL ultrapure water and 10 μL 1M ethoxylate to the reaction system Diethyl methylene malonate (DEEMM) was reacted at room temperature for 10 minutes, and transferred to 70°C for 2 hours to complete the reaction of DEEMM. The derivatized product was detected by reversed-phase high performance liquid chromatography with an ultraviolet (nm) detector. Wherein mobile phase A: 100% acetonitrile; mobile phase B: 25mMpH=4.8 sodium acetate buffer solution; flow rate 0.5mL / min, using gradient elution 0min A:B is 20:80; 2min A:B is 25:75; 27min A:B is 62.5:37.5; 27.01min A:B is 20:80; 37min A:B is 20:80; 37.01min ends the test. Detection column: C18 column (Shim-pack GIST-HP-C18 column, 2.1×100mm, 3m particle size); detection temperature: 35°C; injection volume: 5μL, detector: SPD-20A diode array detector; wavelength: 284nm. By 1,6-hexamethylenediamine peak ar...

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Abstract

The invention relates to a method for efficiently detecting aliphatic diamine, and belongs to the technical field of biology. According to the detection method, pre-column derivatization is carried out on an aliphatic diamine standard substance or an experimental sample by virtue of a derivatization agent, and the content of derived aliphatic diamine is detected by virtue of a high performance liquid chromatography ultraviolet detector. The derivatization agent is diethyl ethoxy methylene malonate (DEEMM), aliphatic diamine is derived from the derivatization agent through a condensation reaction, and the derivatization agent mainly comprises 1, 4-butanediamine, 1, 5-pentamethylene diamine, 1, 6-hexamethylenediamine, 1, 7-heptyl diamine and other diamine containing ammonium ions, monoamine, amino acid and the like. The content of the aliphatic diamine is detected through the high performance liquid chromatography ultraviolet detector, the method is simple, rapid, high in sensitivity, few in by-product and high and stable in derivatization product detection sensitivity; and aliphatic diamine and amino acid can be analyzed at the same time, the detection efficiency and accuracy are improved, and the detection limit reaches 100 nM.

Description

technical field [0001] The invention relates to a method for efficiently detecting aliphatic diamines, belonging to the field of biotechnology. Background technique [0002] Nylon, that is, polyamide (nylon), has excellent comprehensive properties in many fields such as fiber spinning (such as cord fabrics, airbag fabrics and clothing, etc.) and engineering plastics (such as automobiles, machinery, cable ties and electrical appliances). Significant application value, the market size reaches 7 million tons per year, of which nylon 66 is one of the important varieties. Nylon 66, which is polymerized from hexamethylenediamine and adipic acid, mainly relies on petroleum as a raw material, and foreign companies INVISTA, Ascend, Solvay and Asahi Kasei have monopolized the core technology of hexamethylenediamine synthesis. Therefore, my country urgently needs to develop alternatives to hexamethylenediamine. The production of bio-based nylon not only replaces petroleum-based raw m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/74
CPCG01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N2030/027G01N2030/067
Inventor 黄玉红赵永亮薛雅鞠张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI