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Method for detecting nitrite in cubilose based on dialysis bag purification technology

A technical detection and nitrite technology, which is applied in the field of detection of nitrite in bird's nest based on dialysis bag purification technology, can solve problems such as chromatographic column clogging and chromatographic peak interference, and achieve the effect of reducing clogging and chromatographic peak interference

Active Publication Date: 2019-04-09
厦门市仙岳医院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of this, the purpose of the present invention is to provide a new method for detecting nitrite in bird's nest, which can not only solve the problems of clogging of chromatographic column and interference of chromatographic peak, but also obtain ideal detection limit and limit of quantitation

Method used

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  • Method for detecting nitrite in cubilose based on dialysis bag purification technology
  • Method for detecting nitrite in cubilose based on dialysis bag purification technology
  • Method for detecting nitrite in cubilose based on dialysis bag purification technology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] Preparation of standard solutions

[0072] Nitrite standard stock solution (100mg / L, with NO 2 Measure) Accurately weigh 0.1500g of sodium nitrite dried at 110°C-120°C to constant weight, dissolve in water and transfer to a 1000mL volumetric flask, add water to dilute to the mark, and mix well. Accurately measure 1mL100mg / L standard NO 2 , in a 100mL volumetric flask, add ultrapure water to the mark to make a 1mg / L standard stock solution. Pipette 0.2, 0.4, 0.8, 1.2mL of standard stock solutions into 10mL volumetric flasks, add water to make up to the mark, and make a series of standard nitrite solutions with concentrations of 0.02, 0.04, 0.08, 0.1, 0.2mg / L.

[0073] A series of standard solutions are sequentially injected and analyzed according to the chromatographic conditions, and the chromatographic conditions are as follows:

[0074] The chromatographic column is a 4mm×250mm Dionex IonPacTMAS 19 anion column;

[0075] The guard column is Dionex IonPacTM AG19 of...

Embodiment 2

[0086] Weigh 5.00g (accurate to 0.01g) of the test sample and dilute it to 20mL in a 50mL colorimetric tube, ultrasonically extract for 60min, shake once every 10min to keep the solid phase completely separated, and at the same time take a glass centrifuge tube and add 20mL of water stand-by. After the ultrasound was completed, 5 mL of the solution was extracted, placed in a 44 mm dialysis bag and placed in a glass centrifuge tube filled with 20 mL of water, and extracted by ultrasound for 60 min. Take it out and let it stand at room temperature, pick up the dialysis bag, and use the filtrate for later use.

[0087] Take about 15mL of the above-mentioned filtrate, pass it through a 0.22μm aqueous filter membrane syringe filter, RP column, Ag column, and Na column in sequence at a flow rate of 2mL / min, discard 10mL of the initial eluate, collect the eluate, and inject it into the injection bottle The ion chromatography analysis was carried out directly according to the chromat...

Embodiment 3

[0094] Spike recovery

[0095] Add a certain amount of sodium nitrite to the negative bird's nest, mix well, make the standard addition content of nitrite in the sample be respectively 0.4mg / kg, 0.8mg / kg and 4mg / kg (the standard addition level is respectively 1 times quantitative limit, 2 times of quantification limit and 3 times of quantification limit) according to the conditions obtained by optimization to measure nitrite average recovery rate and relative standard deviation (n=6), the average recovery rate of sample is at 83.1-99.6%, and relative standard deviation is at 2.98- 10.16%, in line with the detection requirements, the detection results of this method are credible.

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Abstract

The invention provides a method for detecting nitrite in cubilose based on a dialysis bag purification technology, and belongs to the technical field of cubilose safety monitoring. The method for detecting the nitrite in the cubilose based on the dialysis bag purification technology comprises the following steps of dissolving the cubilose in water, and carrying out dialysis on an obtained cubilosesolution; performing microfiltration, RP column, Ag column and Na column separation on a filtrate in sequence according to a flow speed of 0.5-3 mL / min, removing 10 mL of an initial eluate, and collecting the eluate; carrying out ion chromatographic analysis on the eluate to obtain an ion chromatogram; and calculating a detection limit and a quantitation limit according to a peak response value at the acid salt retention time of ion chromatography. A detection result is consistent with that in a national standard detection method. The dialysis bag purification method is adopted, so that impurities are effectively removed; the method is simple and feasible; a chromatographic column is effectively protected; the resolution of the ion chromatography is improved; and the content of the nitrite can be rapidly, accurately and efficiently determined by the ion chromatography method.

Description

technical field [0001] The invention belongs to the technical field of bird's nest safety monitoring, and in particular relates to a method for detecting nitrite in bird's nest based on a dialysis bag purification technology. Background technique [0002] Nitrite is the general term for sodium nitrite and potassium nitrite, generally refers to sodium nitrite, is a white opaque crystal chemical product, shaped like table salt, and is widely used in chemical industry, construction and medicine. Nitrite can be used as a coloring agent and preservative in food production and processing, and the amount controlled within a safe range will not cause harm to human health. At the same time, the toxicity of nitrite is strong. The half-lethal dose (LD50) of mice is 220mg / kg body weight, the poisoning dose of human is 0.3-0.5g, and the lethal dose is 3g. Due to the poor detoxification ability of children, the organs are harmful to the body. Poison tolerance is poor, only 1 / 5 to 1 / 3 of ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/14
CPCG01N30/02G01N30/06G01N30/14
Inventor 郑慧斐赖国银徐敦明王文强章家新张志刚吴敏
Owner 厦门市仙岳医院
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