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Method for determining 2,4-dinitrophenol in dry food wrapper based on derivatization

A technology of dinitrophenol and food wrapping paper, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effects of reducing errors, fast methods, and high sensitivity

Active Publication Date: 2013-08-14
CHINA TOBACCO JIANGSU INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, for samples with complex matrices, the accurate characterization of the target needs to be further improved

Method used

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  • Method for determining 2,4-dinitrophenol in dry food wrapper based on derivatization
  • Method for determining 2,4-dinitrophenol in dry food wrapper based on derivatization
  • Method for determining 2,4-dinitrophenol in dry food wrapper based on derivatization

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Experimental program
Comparison scheme
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Embodiment 1

[0031] A method for determining 2,4-dinitrophenol in dry food wrapping paper based on derivatization, the specific process is as follows:

[0032] (1) Preparation of standard working solution

[0033] Accurately weigh 0.2g of the standard 2,4-dinitrophenol, disperse and dissolve it with ethyl acetate, and then use ethyl acetate as a solvent to dilute it into a 100mL volumetric flask to obtain a standard stock solution with a concentration of 2000mg / L . Accurately pipette a certain volume of standard stock solution, and use ethyl acetate as solvent to prepare standard working solutions with concentrations of 20mg / L, 50mg / L, 100mg / L, 500mg / L and 1000mg / L respectively.

[0034] (2) Preparation of standard extraction solution

[0035] Draw 1mL of the above series of standard working solutions, accurately add 1mL of ethyl acetate internal standard solution with a concentration of 10mg / L of phenylethyl propionate, then add 0.1mL of pyridine and acetic anhydride, and finally add 7....

Embodiment 2

[0049] The present embodiment is as follows to the detection method of the precision of the present invention and the standard addition recovery rate:

[0050] Detection of precision: 6 parallel determinations of the content of 2,4-dinitrophenol in the spiked sample (the spiked level is 50mg / kg), calculate the relative standard deviation, and investigate the precision of the method. The results are shown in Table 2 below . It shows that the method has good repeatability.

[0051] Table 2 Precision of the method (n=6)

[0052]

[0053] Detection of recovery rate: Select two representative samples (instant food wrapping paper and candy paper) as spiked sample matrix, and make spiked samples with low, medium, and high concentration levels respectively. The recovery rate is shown in Table 3. The recovery rate of instant food packaging paper is 87.30-105.00%, and the recovery rate of candy paper is 89.32-104.29%, which shows that the recovery rate of this method is better.

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Abstract

The invention discloses a method for determining 2,4-dinitrophenol in a dry food wrapper based on derivatization. The method comprises the steps of: (1) preparing a plurality of ethyl acetate series standard working solutions with concentration of 2,4-dinitrophenol being 20-1000mg / L; (2) preparing a standard extract solution; (3) preparing a sample solution; (4) detecting and analyzing the standard working solutions and the sample solution by a gas chromatography-mass spectrometer; and (5) making a standard curve and calculating the result. According to the method, the phenomenon of peak tailing of 2,4-dinitrophenol caused by direct sampling is avoided; an internal standard method is utilized for quantification, volume fixing can be omitted and the errors caused by the reproducibility of a pretreatment method and the problem related to instrument precision can be reduced; and the method is rapid, correct, high in sensitivity and suitable for determining the content of the 2,4-dinitrophenol in the dry food wrapper.

Description

technical field [0001] The invention belongs to the technical field of physical and chemical index detection of packaging materials, and specifically relates to a derivatization-based determination of 2,4-dinitrophenol in dry food packaging paper (mainly including instant food packaging paper, candy paper, pasta paper, etc.) Methods. Background technique [0002] 2,4-Dinitrophenol (2,4-dinitrophenol, referred to as DNP), slightly soluble in water, soluble in organic solvents such as ethanol, ether, benzene and chloroform. 2,4-Dinitrophenol belongs to the protoplasmic poison and is highly toxic. The lowest oral lethal dose (LDLo) for humans is 36 mg / kg, and the oral half-lethal dose (LD50) for rats is 30 mg / kg. The poisoning mechanism is mainly Act directly on energy metabolism, stimulate oxidation process, inhibit phosphorylation process. Mainly used in industries such as dyes, developers, drugs, indicators, pesticides and wood preservation. [0003] Dry food packaging pa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 廖惠云朱龙杰庄亚东张映熊晓敏王珂清曹毅张媛
Owner CHINA TOBACCO JIANGSU INDAL