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Method for detecting free and bound trace cyanide

A cyanide, free state technology, applied in the field of analysis and detection, can solve the problems of low detection sensitivity, easy interference, high detection limit, complicated operation, etc., and achieve the effect of reducing detection inaccuracy, easy operation, and simplified operation.

Active Publication Date: 2017-05-31
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The first object of the present invention is to provide a method for detecting trace cyanide in free state and bound state, which solves the problems of high detection limit, cumbersome operation, low detection sensitivity and easy interference of the prior art free state and bound state cyanide determination method

Method used

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  • Method for detecting free and bound trace cyanide
  • Method for detecting free and bound trace cyanide
  • Method for detecting free and bound trace cyanide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1: the mensuration of free state and combined state cyanide in yellow rice wine

[0041] (1) Pretreatment and derivatization of rice wine samples:

[0042] a. Sample pretreatment and derivatization for the determination of free cyanide: Add 2 mL of rice wine sample to the sample reaction bottle of the pretreatment and derivatization device, add 1 mL of lactic acid, and convert cyanide into hydrocyanic acid. Under the condition of blowing nitrogen, transfer the hydrocyanic acid to the derivatization receiving bottle. Pre-accurately add 2mL of derivatizer and 10μL of internal standard with a concentration of 1mg / L in the derivatization receiving bottle 13 C 15 N-cyanide standard solution. The derivatization reaction between the derivatizing agent and hydrocyanic acid takes place at room temperature for 20 minutes. The derivatized product was obtained, and the content of free cyanide was detected by sample injection.

[0043] b. Sample pretreatment and deri...

Embodiment 2

[0050] Embodiment 2: the mensuration of total cyanide in water

[0051] (1) Sample pretreatment and derivatization:

[0052] Sample pretreatment and derivatization for the determination of total cyanide: add 2 mL of water sample to the sample reaction bottle of the pretreatment and derivatization device, add about 10 mL of distilled water, quickly add 1 g of tartaric acid and 2 mL of 100 g / L zinc acetate, and conduct boiling water The bath is heated and distilled, and the distillate is received by a derivation receiving bottle. Pre-accurately add 2mL of derivatizer and 100μL of internal standard with a concentration of 5mg / L in the derivatization receiving bottle 13 C 15 N-cyanide standard solution. Distillation was stopped when the distillate was close to 10 mL. The distillate was fixed to volume, and the sample was injected to detect the total cyanide content.

[0053] (2) Using Thermo Fisher TSQ Quantum Ultra EMR Triple Quadrupole Liquid Mass Spectrometry to Cyanide De...

Embodiment 3

[0058] Embodiment 3: Evaluation of cyanide detection method

[0059] (1) Repeatability - precision test

[0060] Six standard solutions with a concentration of 10 μg / L were tested respectively, and the final results are shown in Table 1. The test results show that this method has good reproducibility.

[0061] Table 1 Precision

[0062]

[0063] (2) Recovery rate - accuracy test

[0064] Take 6 samples of yellow rice wine with a free cyanide concentration of 4.71 μg / L, add standard substances with a concentration of 2.5 and 10 μg / L accurately, and measure according to the above steps. The recoveries were 93.8% and 106%, respectively. See Table 2 for details.

[0065] Table 2. Recovery rates

[0066]

[0067] (3) Limit of detection and limit of quantitation

[0068] When the injection volume is 2 μL and S / N=3, the LOD of cyanide determination is 0.01 μg / L; when the injection volume is 2 μL and S / N=10, the LOQ is 0.05 μg / L.

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Abstract

The invention discloses a method for detecting free and bound trace cyanide and belongs to the technical field of analysis and detection. The method is mainly used for beverage wine and its raw material analysis. The method utilizes a specific pretreatment and derivatization device to respectively treat the free or bound cyanide samples. Aiming at a free cyanide, the hydrocyanic acid is released and the cyanide group is directly derived. Aiming at the bound cyanide, the bound cyanide is converted into free hydrocyanic acid and the free hydrocyanic acid is derived through a derivatization reagent. The derivative is subjected to qualitative and quantitative analysis based on the liquid chromatography-mass spectrometry combined technology. A standard curve is built by an internal standard method. The contents of the free and bound cyanides are respectively calculated. The detection method has a detection limit of 0.01 micrograms per liter, a quantification limit of 0.05 micrograms per liter, a linear correlation coefficient of more than 0.99, an adding standard recovery rate of 93.8% to 106% and relative standard deviation of less than 10%. The method has the advantages of high detection sensitivity, short time and small interference, and can meet the requirements on free and bound cyanide determination.

Description

technical field [0001] The invention relates to a method for detecting trace cyanide in a free state and a combined state, and belongs to the technical field of analysis and detection. It is mainly used for the analysis of drinking wine and its raw materials. Background technique [0002] Cyanide is a highly toxic substance, which can enter the human body through the respiratory tract, digestive tract and skin, and binds to the ferric iron of the oxidative cytochrome oxidase in the mitochondria of the cell, preventing the reduction of the ferric iron in the oxidase and hindering the normal respiration of the cells. Causes hypoxia in the body resulting in a toxic effect. In addition, cyanide may form other harmful compounds under certain conditions, which poses a safety risk in food and beverages. Naturally occurring cyanide includes free and bound states. Bound cyanide, usually in the form of cyanogenic glucosides, forms free cyanide by hydrolysis and is therefore an impo...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 王栋徐岩邹伟
Owner JIANGNAN UNIV
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