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Method for measuring urotropine content of rice and flour and rice-flour product

A technology of hexamethamine and products, which is applied in the field of detecting the content of hexamethamine in rice noodles and products, can solve the problems of poor repeatability, low accuracy of detection results, poor recovery rate of hexamethamine, etc., and achieve high recovery rate , the extraction effect is good, and the effect of increasing the ammonia content

Inactive Publication Date: 2018-11-13
GUANGZHOU INST FOR FOOD INSPECTION(GUANGZHOU INSPECTION CENT FOR WINE & SPIRITS)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the high-performance liquid chromatography in these methods, the test is carried out according to the conditions of the chromatographic column and extract in the literature. After the food is placed in water, its pH value is mostly between 5.0-6.5, which is weakly acidic. The product will be partially decomposed into formaldehyde and ammonia in the acidic solution, so the existing extracts generally have the defects of poor recovery rate of urotropine, low accuracy and poor repeatability of test results
However, the liquid chromatography-mass spectrometry method in the industry standard method is not suitable for the determination of rice flour and its products, and is only limited to the determination of urotropine in food of animal origin

Method used

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  • Method for measuring urotropine content of rice and flour and rice-flour product
  • Method for measuring urotropine content of rice and flour and rice-flour product
  • Method for measuring urotropine content of rice and flour and rice-flour product

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Embodiment 1

[0031] A method for measuring the content of urotropine in rice noodles and products, comprising the following steps.

[0032] Step 1. Make a sample of the food to be tested. The food to be tested in this embodiment is a solid food made of rice noodles. The solid food to be tested is crushed until the particle diameter is not greater than 0.3mm as a sample; the sample of this embodiment No urotropine was detected in the sample, so 1 kg of the sample was weighed first, 4 mg of urotropine was added, and mixed to obtain sample P1, the spiked value of the urotropine content was 4 mg / kg.

[0033] Carry out 6 groups of parallel tests starting from step 2, that is, weigh 2.5g of 6 parts of sample P1 in step 1, place them in 6 different centrifuge tubes respectively, and form 6 groups of parallel tests, and each group of parallel tests proceeds from steps 2 to 1 in turn. 4.

[0034] Step 2. Weigh 2.5g of the sample P1 of step 1 into a centrifuge tube, add 5mL of ammonium acetate with...

Embodiment 2

[0043] The method for measuring urotropine content in rice noodles and products of the present embodiment, it may further comprise the steps:

[0044] Step 1. Crush the product to be tested into a sample with a particle diameter of not more than 0.3 mm. In this example, the product to be tested was not detected to contain urotropine, so first weigh 1 kg of the sample, add 8 mg of urotropine, and mix well Obtained sample P2, the spiked value of its urotropine content is 8mg / kg.

[0045] Carry out 6 groups of parallel tests starting from step 2, that is, weigh 2.5g of 6 parts of the sample P2 in step 1, place them in 6 different centrifuge tubes respectively, and form 6 groups of parallel tests, and each group of parallel tests will carry out steps 2 to 1 in turn. 4.

[0046] Step 2. Weigh 2.5g of the sample P2 of step 1 into a centrifuge tube, add 5mL ammonium acetate with a concentration of 20mmol / L to the centrifuge tube, adjust the pH value of the ammonium acetate solution ...

Embodiment 3

[0050] The method for measuring urotropine content in rice noodles and products of the present embodiment, it may further comprise the steps:

[0051] Step 1. Crush the product to be tested into a sample with a particle diameter not greater than 0.3mm. In this example, the product to be tested was not detected to contain urotropine, so first weigh 1 kg of the sample, add 40 mg of urotropine, and mix well , to obtain sample P3, the spiked value of its urotropine content was 40mg / kg.

[0052] Carry out 6 groups of parallel tests starting from step 2, that is, weigh 2.5g of 6 parts of the sample P3 in step 1, place them in 6 different centrifuge tubes respectively, and form 6 groups of parallel tests, and each group of parallel tests proceeds from steps 2 to 1 in turn. 4.

[0053] Step 2. Weigh 2.5g of sample P3 from step 1 into a centrifuge tube, add 5mL of ammonium acetate with a concentration of 20mmol / L to the centrifuge tube, adjust the pH value of the ammonium acetate solu...

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Abstract

The invention provides a method for measuring urotropine content of rice and flour and a rice-flour product. The method comprises the following steps: 1, making a product to be measured into a sample;2, weighing the sample to a centrifuging tube, adding ammonium acetate for performing ultrasonic extraction and centrifuging, and placing supernatant into a volumetric flask; 3, continuously adding the ammonium acetate into the centrifuging tube, performing ultrasonic extraction and centrifuging, placing the supernatant into the volumetric flask used in step 2, and metering the volume of the supernatant to 10 mL with the ammonium acetate to obtain a clear sample liquid; 4, performing filtering with a water-phase microfiltration membrane to obtain a sample liquid to be measured; 5, measuring peak areas of a urotropine standard working liquid and the sample liquid to be measured with an efficient liquid phase chromatograph to obtain a standard curve equation; 6, calculating the urotropine content in the product to be measured. The method has the characteristics of high urotropine extraction efficiency, easiness in operation, high accuracy, high stability and high repeatability, so thata stable and reliable method for detecting urotropine in the rice-flour product is provided.

Description

technical field [0001] The invention relates to the technical field of detection in rice noodles and products, in particular to a method for detecting the content of urotropine in rice noodles and products. Background technique [0002] Methenamine is a white fine granular crystal, also known as hexamethylenetetramine, soluble in water, ethanol, chloroform, insoluble in carbon tetrachloride, ether, petroleum ether. Hexatropine is used in industrial production as curing agent, catalyst and foaming agent for resins and plastics, accelerator for rubber vulcanization, anti-shrinkage agent for textiles, etc. In the field of military industry, the action of urotropine and fuming nitric acid can be made into extremely explosive cyclone dynamite. The product is flammable and corrosive, and contact can cause dermatitis and eczema, and is harmful to the kidney, liver, central nervous system, immune function and digestive system of the human body. In recent years, the supervisory dep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 彭名军宋安华毛新武刘冬豪李慧琴林子豪黄秋婷王宇姚子升胡雯艳周庆琼江程明陈楷漆亚乔钟玉心王成龙汪宁赵金利曾豪威吴嘉文
Owner GUANGZHOU INST FOR FOOD INSPECTION(GUANGZHOU INSPECTION CENT FOR WINE & SPIRITS)
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