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Method for determining acetohydroxamic acid in wheat flour and wheat flour treating agent

A flour treatment agent, acetohydroxamic acid technology, applied in the field of chemical analysis, to achieve the effect of high sensitivity and simple method

Pending Publication Date: 2022-03-25
河南省食品检验研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, acetohydroxamic acid is a non-food ingredient
Currently there is no standard or method for the determination of acetohydroxamic acid in flour or flour treatment agents

Method used

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  • Method for determining acetohydroxamic acid in wheat flour and wheat flour treating agent
  • Method for determining acetohydroxamic acid in wheat flour and wheat flour treating agent
  • Method for determining acetohydroxamic acid in wheat flour and wheat flour treating agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] extract

[0057] Accurately weigh 1g (accurate to 0.01g) of the sample, place it in a 15mL stoppered centrifuge tube, add 0.4g (accurate to 0.01g) of polyethylene glycol and mix well. Accurately add 10 mL of absolute ethanol, vortex for 10 min, extract with ultrasound (power: 100 kHz) for 10 min, and centrifuge at 8000 r / min for 5 min at 4°C. The supernatant was used for later use.

[0058] purify

[0059] Pipette 5 mL of supernatant and transfer to activated C 18 In the solid-phase extraction column, discard the first 3mL of effluent, collect the effluent, pass through a 0.22μm organic filter membrane, discard 2-5 drops of the initial filtrate, and take the subsequent filtrate to be tested on the machine.

[0060] Gas Chromatography Reference Conditions

[0061] Chromatographic column: Agilent 19091N-1131 HP-INNOWAX (40~270℃), 30m×320μm×0.25μm, or equivalent;

[0062] Carrier gas: high-purity nitrogen, purity ≥ 99.9995%; column flow rate: 2.5mL / min.

[0063] Inlet ...

Embodiment 2～13

[0107] Sample testing

[0108] Select 6 batches of representative samples of wheat flour and flour treatment agent, a total of 12 batches of samples, and test according to the method specified in this standard. It is found that the residual amount of acetohydroxamic acid in the two batches of flour treatment agent samples is 38.46 ( see Figure 4 ) and 37.25mg / kg, and the residues of acetohydroxamic acid in the remaining samples were not detected.

[0109] Experimental effect

[0110] precision

[0111] The absolute difference between two independent determination results obtained under repeatability conditions shall not exceed 10% of the arithmetic mean.

[0112] Weigh 1g of blank matrix sample, add acetohydroxamic acid standard (n=6) at different levels, the addition level is 50mg / kg and 100mg / kg, process according to the proposed sample pretreatment method, test on the machine, investigate The precision of the method. The results are shown in Tables 5 and 6. The relat...

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Abstract

The invention discloses wheat flour and a method for determining acetohydroxamic acid in a flour treating agent of the wheat flour. Belongs to the technical field of chemical analysis. Comprising the following steps: sample extraction; purifying and analyzing; drawing a standard curve; and qualitatively and quantitatively identifying the sample. According to the method, acetohydroxamic acid is detected based on a gas chromatography technology, ethanol extraction and C18 solid-phase extraction column purification are carried out, a gas chromatograph provided with a nitrogen and phosphorus detector is adopted for detection after filtration, the retention time of a gas chromatography is used for qualitative determination, and an external standard method is used for quantification. The method is simple and convenient, has high sensitivity, and is very suitable for determining acetohydroxamic acid in wheat flour and a flour treating agent thereof. The detection limit is 10 mg / kg; the quantification limit is 30 mg / kg.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a method for determining acetohydroxamic acid in wheat flour and a flour treatment agent thereof. Background technique [0002] Acetohydroxamic acid (AHA), also known as acetohydroxamic acid, Junshitong, etc., is a hydroxamic acid compound with a CAS number of 546-88-3 and a molecular formula of C 2 h 5 NO 2 , the molecular weight is 75.0666. The -CONHOH functional group in the structure of acetohydroxamic acid is an excellent organic ligand and a very important beneficiation agent; in the 1990s, acetohydroxamic acid was widely used in animal husbandry as a good urease inhibitor of rumen microorganisms application. [0003] Flour is one of the most commonly eaten staple foods for people in northern my country, and it is also the main raw material for many baked and other processed foods. Acetohydroxamic acid is added to flour and flour treatment agents to prevent th...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8679G01N2030/062
Inventor 袁利杰张培毅毛景袁阳蕾刘璐凡猛石璐武文凯周楠
Owner 河南省食品检验研究院
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