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A high-performance liquid chromatography analysis and detection method for 3-nitropropionic acid in food

A high-performance liquid chromatography and nitropropionic acid technology, which is applied in the detection field of 3-nitropropionic acid in food, can solve the problems of unsatisfactory solid phase extraction column purification effect and recovery rate, and achieve simple and novel processing steps , high recovery rate and good precision

Active Publication Date: 2018-08-24
GUANGZHOU PONY TESTING TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Then the purification method was further optimized. By comparing various purification methods, it was found that the purification effect and recovery rate of various solid phase extraction columns (such as neutral alumina, etc.) were not ideal

Method used

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  • A high-performance liquid chromatography analysis and detection method for 3-nitropropionic acid in food
  • A high-performance liquid chromatography analysis and detection method for 3-nitropropionic acid in food
  • A high-performance liquid chromatography analysis and detection method for 3-nitropropionic acid in food

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1. Instruments and reagents

[0034] High performance liquid chromatography: Shimadzu LC-20AT, equipped with diode array detector;

[0035] Standard substance: 3-nitropropionic acid, purity 98.0%;

[0036] Acetonitrile: chromatographically pure;

[0037] Ethyl acetate, sodium dihydrogen phosphate, disodium hydrogen phosphate, and phosphoric acid are all analytically pure;

[0038] The water used in this method is primary water.

[0039] 2. Instrument analysis conditions

[0040] Gel Permeation Chromatography Conditions:

[0041] Purification column: Bio-Rad Bio-Beads S-X3, 200-400 mesh;

[0042] Detection wavelength: 254nm;

[0043] Mobile phase: ethyl acetate + n-hexane, volume ratio 1:1;

[0044] Injection volume: 5ml;

[0045] Start collection time: 10min;

[0046] End collection time: 25min;

[0047] Liquid chromatography conditions:

[0048] Column: Agilent HC-C 18 , 4.6×250mm, 5μm;

[0049] Mobile phase: acetonitrile + 0.02mol / L KH 2 PO 4 Solution =...

Embodiment 2

[0074] 1. Instruments and reagents

[0075] High performance liquid chromatography: Shimadzu LC-20AT, equipped with diode array detector;

[0076] Standard substance: 3-nitropropionic acid, purity 98.0%;

[0077] Acetonitrile: chromatographically pure;

[0078] Ethyl acetate, sodium dihydrogen phosphate, disodium hydrogen phosphate, phosphoric acid, and n-hexane are all analytically pure;

[0079] The water used in this method is primary water.

[0080] 2. Instrument analysis conditions

[0081] Gel Permeation Chromatography Conditions:

[0082] Purification column: Bio-Rad Bio-Beads S-X3, 200-400 mesh;

[0083] Detection wavelength: 254nm;

[0084] Mobile phase: ethyl acetate + n-hexane, volume ratio 1:1;

[0085] Injection volume: 5ml;

[0086] Start collection time: 10min;

[0087] End collection time: 25min;

[0088] Liquid chromatography conditions:

[0089] Column: Agilent HC-C 18 , 4.6×250mm, 5μm;

[0090] Mobile phase: acetonitrile + 0.02mol / L KH 2 PO 4 ...

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Abstract

The invention belongs to the technical field of food safety and relates to a detecting method of 3-nitropropionic acid in foods. The method includes following steps: (1) weighing a uniform sample, and homogenizing and extracting the sample with a Na2HPO4-HaHPO4 buffer solution being 8 in pH; (2) performing high-speed freeze-centrifugation, moving the buffer solution and regulating the pH to 2 by phosphorus acid; (3) performing extraction with ethyl acetate, performing GPC purification, blowing an eluant with nitrogen to dryness, dissolving a mobile phase and diluting the mobile phase to constant volume; and (4) filtering the mobile phase through an organic filter membrane being 0.45 [um]m in mesh size for detection. The to-be-detect sample is separated through a C18 liquid phase chromatographic column and is detected in a diode array detector with a quantitative treatment through an external standard method. The detection method is simple and creative in pre-treatment, is good in impurity removal effect, is high in sensitivity and recycle rate, is high in precision of measurement result and can be used for effectively detecting the content of the 3-nitropropionic acid in various foods.

Description

1. Technical field [0001] The invention belongs to the technical field of food safety, in particular to a detection method for 3-nitropropionic acid in food. 2. Technical background [0002] 3-Nitropropionic acid is a white crystalline compound, easily soluble in polar solvents such as water, methanol, ethyl acetate, and acetonitrile. Studies have shown that 3-nitropropionic acid is a metabolite of a few species of Aspergillus and Penicillium, and the sugarcane Arthrophyllum and Arthrospora saccharomyces isolated from spoiled sugarcane in my country can also produce 3-nitropropionic acid. Nitropropionic acid. 3-Nitropropionic acid is a kind of neurotoxin, and people are prone to poisoning if they eat it by mistake, especially in children. The main manifestation of this poisoning is damage to the central nervous system. Symptoms in the acute stage include vomiting, dizziness, paroxysmal convulsions, hemigazing, coma, and even death. The sequelae are mainly damage to the extr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 宋薇邹强李庆
Owner GUANGZHOU PONY TESTING TECH