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Method of determining selenium shape of honey and fruit juice by solid phase extraction-atomic fluorescence spectrometry

An atomic fluorescence spectroscopy, honey technology, applied in the field of fluorescence spectroscopy detection, can solve the problems affecting the accuracy of selenium speciation, honey cannot be digested, and it is difficult to extract organic selenium, etc., achieves significant separation effect, avoids extremely low extraction efficiency, The effect of saving processing time and costs

Active Publication Date: 2017-05-31
安徽出入境检验检疫局检验检疫技术中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the viscous tissue state of honey, it is difficult to extract organic selenium with organic reagents, which affects the accuracy of selenium speciation determination.
When using chromatography-spectral detection combined technology, honey cannot be digested, and can only be injected after simple dissolution and dilution.
A large number of sugars and proteins in honey enter the instrument together during sample injection, which will seriously pollute the sample injection system of the instrument. Therefore, this method has not been applied to the determination of selenium in honey.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The determination operation steps of inorganic selenium and organic selenium in honey are as follows:

[0034] (1) Extraction of inorganic selenium in honey

[0035] Add 20 mL of distilled water to 2 g of the honey sample to be tested (accurate to 0.01 g), and vortex to mix;

[0036] Adjust the pH value to 3 with hydrochloric acid solution with a concentration of 1 mol / L, and add water to make up to 10 mL;

[0037] Then super strong cation exchange column (SCX column) (activated with 3 mL methanol and 3 mL water before use), the separation condition of solid phase extraction is hydrochloric acid solution with a pH value of 3; the filtrate is collected under negative pressure to obtain inorganic selenium. Extract;

[0038] Add 20 mL of mixed acid (concentrated nitric acid: hydrogen peroxide = 4:2) to the extract, and heat to a slight boil; when the solution becomes clear and colorless with white smoke, it means that the organic matter has been completely removed by dig...

Embodiment 2

[0054] The determination method steps of inorganic selenium and organic selenium in fruit juice are as follows:

[0055] (1) Extraction of inorganic selenium in fruit juice

[0056] Add 20 mL of distilled water to 5 g of apple juice sample (accurate to 0.01 g), and vortex to mix;

[0057] Adjust the pH value to 3 with hydrochloric acid solution with a concentration of 1 mol / L, and add water to make up to 25 mL;

[0058] Under the condition of 4000 r / min, centrifuge for 10 min, take 5 mL supernatant and put it on a strong cation exchange column (SCX column) (activated with 3 mL methanol and 3 mL water before use), collect the filtrate under negative pressure, Obtain the extract of inorganic selenium;

[0059] Add 10 mL of mixed acid (concentrated nitric acid: hydrogen peroxide = 4:2) to the extract, and heat to a slight boil; when the solution becomes clear and colorless with white smoke, it means that the organic matter has been completely removed by digestion, and then cont...

Embodiment 3

[0075] This example is a method for the determination of inorganic selenium and organic selenium in fruit and vegetable juice beverages. The fruit and vegetable juice beverages used are clarified beverages prepared by mixing concentrated fruit juices such as apples, tomatoes, and grapes, and adding water and other ingredients. The specific determination steps are as follows:

[0076] (1) Extraction of inorganic selenium

[0077] Add a little distilled water to 5 g of fruit and vegetable juice beverage samples (accurate to 0.01 g);

[0078] Adjust the pH value to 3 with hydrochloric acid solution with a concentration of 1 mol / L, and add water to make up to 10 mL;

[0079] Pass the constant volume solution over a strong cation exchange column (SCX column) (activated by rinsing with 3 mL methanol, 3 mL water, and 3 mL 0.001mol / L hydrochloric acid solution before use), and collect the filtrate under negative pressure to obtain inorganic selenium of the extract;

[0080] Add 20 m...

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Abstract

The invention discloses a method of determining selenium shape of honey and fruit juice by solid phase extraction-atomic fluorescence spectrometry. The method comprises the following steps: separating organic selenium and inorganic selenium in honey or fruit juice under a condition of pH being 3 by means of an SCX solid phase extraction column; then adding a mixed acid to digest and separate to obtain an inorganic selenium extraction liquid; then determining the selenium element by means of atomic fluorescence spectrometry; determining the content of total selenium by means of wet digestion; and finally obtaining the content of the organic selenium by means of a minusing method. The method of determining the shape of selenium separates and determines inorganic selenium and organic selenium accurately and effectively by combining technologies of ionic adsorption exchange, acid digestion and atomic fluorescence spectrometry and the like. The method is simple, environmentally friendly and efficient, thereby providing a powerful technical support for evaluating the functionality and safety of selenium-enriched honey and juice.

Description

technical field [0001] The invention belongs to the technical field of fluorescence spectrum detection, and in particular relates to a method for determining the form of selenium in honey and fruit juice by solid-phase extraction-atomic fluorescence spectrometry. Background technique [0002] Selenium is an essential trace element to maintain the normal life activities of humans and animals. The biological activity of selenium has an important relationship with its chemical form. It has the effect of delaying aging. The form of selenium is divided into organic selenium and inorganic selenium, of which inorganic selenium includes selenous acid and selenic acid, organic selenium includes selenocystine, selenomethionine, selenosulfur protein and other forms. Organic selenium in honey is mainly in the form of selenomethionine (SeMet), selenocysteine ​​(SeCys), selenosaccharides, etc., while the inorganic selenium is mainly selenous acid (SeO 3 2- ), selenic acid (SeO 4 2- )...

Claims

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Application Information

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IPC IPC(8): G01N21/64G01N1/34
CPCG01N1/34G01N21/6404
Inventor 吕亚宁胡艳云韩芳宋伟沈贵兰丁磊周典兵郑平盛旋
Owner 安徽出入境检验检疫局检验检疫技术中心
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