A method for derivatization-chromatographic analysis of residual semicarbazide in flour and flour products

A chromatographic analysis and semicarbazide technology, which is applied in the field of derivatization-chromatographic analysis of residual semicarbazides in flour and flour products, can solve the problems of expensive isotope internal standards, complicated processing procedures, and expensive instruments, etc. Detection, enhancement of UV absorption, and low detection cost

Active Publication Date: 2018-05-18
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

High-performance liquid chromatography tandem mass spectrometry is used to detect semicarbazide, the equipment used is expensive, and the price of isotope internal standard is also expensive, the sample pretreatment process is complicated, the instrument operation is highly professional, and the method is not easy to popularize

Method used

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  • A method for derivatization-chromatographic analysis of residual semicarbazide in flour and flour products
  • A method for derivatization-chromatographic analysis of residual semicarbazide in flour and flour products
  • A method for derivatization-chromatographic analysis of residual semicarbazide in flour and flour products

Examples

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Effect test

Embodiment 1

[0035] In this embodiment, the fried dough stick sample is used as the sample to be tested, and the specific analysis method of the residual semicarbazide in the fried dough stick is as follows.

[0036](1) Drawing of standard curve: Accurately weigh 0.0500 g of semicarbazide, dilute it in a 50 mL volumetric flask with ultrapure water, and prepare a 1000 mg / L semicarbazide stock solution. A series of semicarbazide standard solutions of 0.01mg / L, 0.05mg / L, 0.1mg / L, 0.5mg / L, 1mg / L, and 2mg / L were prepared by serially diluting with ultrapure water. Accurately weigh 0.0500g of 4-nitrobenzoyl chloride, dilute it in a 50mL volumetric flask with acetonitrile, prepare a 1000mg / L stock solution of 4-nitrobenzoyl chloride, dilute step by step with acetonitrile to prepare 5mg / L, 25mg / L, 50mg / L, 250mg / L, 500mg / L, 1000mg / L series of 4-nitrobenzoyl chloride standard solutions. Take 1mL of semicarbazide standard solution and add it to a 2mL sampling bottle, correspondingly add 100μL of 4-n...

Embodiment 2

[0044] This example is roughly the same as Example 1, except that the samples to be tested are different. In this example, the sample to be tested is cow ears, and the specific analysis method for residual semicarbazide in the cow ears is as follows.

[0045] (1) Drawing of standard curve: Accurately weigh 0.0500 g of semicarbazide, dilute it in a 50 mL volumetric flask with ultrapure water, and prepare a 1000 mg / L semicarbazide stock solution. A series of semicarbazide standard solutions of 0.01mg / L, 0.05mg / L, 0.1mg / L, 0.5mg / L, 1mg / L, and 2mg / L were prepared by serially diluting with ultrapure water. Accurately weigh 0.0500g of 4-nitrobenzoyl chloride, dilute it in a 50mL volumetric flask with acetonitrile, prepare a 1000mg / L stock solution of 4-nitrobenzoyl chloride, dilute step by step with acetonitrile to prepare 5mg / L, 25mg / L, 50mg / L, 250mg / L, 500mg / L, 1000mg / L series of 4-nitrobenzoyl chloride standard solutions. Take 1mL of semicarbazide standard solution and add it t...

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Abstract

The invention discloses a method for derivatization chromatographic analysis of residue semicarbazide in flour and a flour product. The method comprises the following steps: (1) enabling semicarbazide and a derivatization reagent to react, using HPLC / UV (High Performance Liquid Chromatography / Ultra Violet) to detect, and drawing to obtain a standard curve, wherein the standard curve takes the concentration of semicarbazideas an x-coordinate and takes the characteristic peak area of a derivatization product as a y-coordinate; (2) taking a to-be-detected sample, implementing ultrasonic extraction by using an extraction agent, centrifuging to obtain a supernate, adding the derivatization reagent and a precipitator into the supernate, centrifuging to obtain a supernate, filtering the supernate through an organic filter membrane to obtain a filtrate; (3) detecting the filtrate obtained in the step (2) through HPLC / UV, reading the characteristic peak area of the derivatization product, and contrasting with the standard curve to obtain the content of the semicarbazide in the to-be-detected sample. Compared with the prior art, the derivatization reagent strengthens the ultraviolet absorption of the derivatization product, and the detection is facilitated; in addition, a detection instrument is simple and common, the detection cost is low, the rapid detection of the semicarbazide is facilitated, and the method is applicable to large-scale sample detection and is suitable for standardization.

Description

technical field [0001] The invention relates to the field of food safety monitoring, in particular to a derivatization-chromatographic analysis method for residual semicarbazide in flour and flour products, which can accurately detect residual semicarbazide in flour or flour products. Background technique [0002] Semicarbazide belongs to the hydrazide series compound, and is usually used as a marker to detect illegally used contraband nitrofurazone antibiotics. Recent studies have found that semicarbazide is contained in rubber gaskets that use azodicarbonamide as a plasticizer for sealing in glass bottle caps, and the process of processing flour with azodicarbonamide as a glutenizer into flour products semicarbazides are also produced. [0003] Semicarbazide (SEM) is a high-risk substance that has attracted much food safety attention due to its carcinogenicity, mutagenicity and possible genotoxicity. There are three main sources of semicarbazides in food, one is animal-d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 李攻科韦天富张卓旻
Owner SUN YAT SEN UNIV
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