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Method for measuring selenium in food through combination of double cloud point extraction and hydride generation-atomic fluorescence spectroscopy

A technology of atomic fluorescence spectroscopy and hydride generation, which is applied in the directions of fluorescence/phosphorescence, food testing, material inspection, etc., can solve the problems of undetectable, solution entering, and low measurement results, and achieve good accuracy, detection precision and The effect of high enrichment factor and low detection limit

Inactive Publication Date: 2015-11-04
GUANGDONG PHARMA UNIV
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0004] The difficulty encountered in the combination of CPE and HG-AFS is that the surfactant introduced into HG-AFS after a cloud point extraction will generate a lot of foam during the HG process, which will cause the solution to enter the atomizer, so that it cannot be detected
Adding defoamer can eliminate the influence of surfactant, but the stability of selenium complex after extraction is high, and it cannot completely react with potassium borohydride to form H 2 Se, the measured result is low

Method used

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  • Method for measuring selenium in food through combination of double cloud point extraction and hydride generation-atomic fluorescence spectroscopy

Examples

Experimental program
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Effect test

Embodiment 1

[0046] Sample digestion:

[0047] Accurately weigh 0.5g sample into a 50ml conical flask, add 15ml HNO 3 -HClO 4 (4:1) Mix acid for wet digestion. When the solution becomes clear and colorless with white smoke, continue to heat until it is dried. After cooling, add 5mL of 6mol / L HCL, heat on an electric furnace to drive the acid to about 1mL, transfer to a 50ml centrifuge tube with stopper, and dilute with three distilled water.

[0048] Enriching selenium by double cloud point extraction operation:

[0049] Take the sample solution after the above treatment in a 50ml centrifuge tube with a stopper, add 1ml of pH 4.0 HCl-NaAc buffer solution, 1g / L APDC 1.2ml and 5% Triton X-114 solution 1.1ml, and dilute to volume with three-distilled water To 50ml, shake well, place in a constant temperature water bath at 51℃, heat for 15min, take it out and centrifuge for 10min (3500r / min) while it is hot, then cool in an ice water bath for 10min, discard the water phase, add 16%HCl+20%H 2 O 2 (...

Embodiment 2

[0053] Refer to the method in Example 1, the difference is that the pH of the HCl-NaAc buffer solution added to S22 is 1.0, the dosage is 1ml, 1g / L APDC 0.6ml and 5% (m / v) Triton X-114 solution 0.8ml , The temperature of the water bath is 40℃.

Embodiment 3

[0055] Refer to the method in Example 1, the difference is that the pH of the HCl-NaAc buffer solution added to S22 is 5.0, the amount is 3ml, 1g / L APDC 1.4ml and 5% Triton X-114 solution 1.2ml, the water bath temperature is 70℃ .

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Abstract

The invention provides a method for measuring selenium in food through combination of double cloud point extraction and hydride generation (GG)-atomic fluorescence spectroscopy (AFS). The method comprises the following steps that firstly, a sample is digested through a wet method; secondly, primary cloud point extraction is carried out on the digested object obtained in the first step, then a mixed solution of HC1 and H2O2 is adopted as back-extractant, and secondary extraction is carried out to concentrate selenium; thirdly, the content of selenium in the sample is measured through the HG-AFS method. It is achieved for the first time that double cloud point extraction and the HG-AFS are applied to detection of the selenium in food in a combination mode, according to the method, the detection limit is 0.16 microgram / L, RSD is 4.04%, the method is high in accuracy and precision, the detection limit is low, and the method is especially suitable for measuring the trace selenium in the food such as spiral seaweeds, kelp and tea.

Description

technical field [0001] The invention belongs to the technical field of food detection, and more specifically relates to a method for determining selenium in food by means of double cloud point extraction-hydride generation-atomic fluorescence spectroscopy. Background technique [0002] Selenium (Selenium) is one of the essential trace elements for life, and is an essential component of the 21st amino acid selenocysteine, selenomethionine and selenium-containing enzymes. Selenium plays an important role in the human immune system, anti-cancer, anti-oxidation and other aspects. However, the safety threshold of selenium in the body is very narrow. Selenium deficiency will occur if the daily selenium intake is less than 50 μg; poisoning may occur if the selenium intake is greater than 200 μg. It is necessary to establish an accurate and sensitive analysis method for selenium content in food. Due to the complex sample matrix and low selenium content, certain pre-enrichment and s...

Claims

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Application Information

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IPC IPC(8): G01N33/02G01N21/64
Inventor 王梅杨冰仪钟怡洲王美霞张泽华
Owner GUANGDONG PHARMA UNIV
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