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Method for rapid detection of cadmium in rice by combination of solid phase extraction and fluorescent colorimetry

A solid-phase extraction column and fluorescence ratio technology, which is applied in fluorescence/phosphorescence, test sample preparation, material excitation analysis, etc., can solve the problems of large instruments, interference, and unsatisfactory detection sensitivity, and achieve the effect of improving sensitivity

Inactive Publication Date: 2015-06-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, many of the above-mentioned methods generally have the disadvantages of high cost, large instruments and skilled operators.
[0006] There are also some simple and fast CDs on the market 2+ Detection methods such as, Cd 2+ Detectors and test papers, etc., but generally have the disadvantages of unsatisfactory detection sensitivity and easy to be interfered by other metal ions that exist at the same time.

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  • Method for rapid detection of cadmium in rice by combination of solid phase extraction and fluorescent colorimetry
  • Method for rapid detection of cadmium in rice by combination of solid phase extraction and fluorescent colorimetry

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preparation example Construction

[0035] 1. Preparation of solid phase extraction column: weigh 0.1g-10g of Cd 2+ sulfonated porous polystyrene-divinylbenzene particles 201 with an adsorption capacity of 40 mg / g-200 mg / g, pour the weighed particles into the solid phase extraction column tube 101 with a sieve plate 301 in advance, and knock the filling After solidification, put into the upper sieve plate 302 to form Cd 2+ Solid phase extraction column.

[0036] 2. Establishment of standard color card and standard concentration curve:

[0037] ①Cd 2+ Preparation of test paper: polyvinyl butyral: trioctyl phosphate: polyethylene glycol-400 mixed in a mass ratio of 30mg-75mg: 200mg-280mg: 75mg-200mg, dissolved in 3mL-10mL absolute ethanol, at room temperature Shake for 0.5h-2h to obtain a polymer solution; mix 10mg-80mg Cd 2+ Add the fluorescent indicator to 5mL of the polymer synthesized above, stir to dissolve, and prepare the test paper by pulling at a uniform speed (pull speed=2mm / s-15mm / s), so that the di...

Embodiment 1

[0043] Take 1g of rice to digest and remove the acid and leave a total of 5mL of the metal mixed solution, and directly add it dropwise to the Cd 2+ In the solid phase extraction column (the volume of the column is 1mL, the amount of the filler is 200mg, the filler is a particle diameter of 50 μm, and a porous polystyrene-divinylbenzene particle with a cross-linking degree of 10%, which has a significant effect on Cd 2+ The adsorption capacity is 50mg / g), under the action of gravity, after the solution passes through the column completely, first drop 10mL of citric acid with a concentration of 0.003M to remove the Cu in the column 2+ 、Ni 2+ and Zn 2+ Wait until the metal ions are rinsed completely, then add 1mL of sodium phosphate solution with a concentration of 0.2M dropwise, and remove all the Cd 2+ and part of Mn 2+ And some alkali metal and alkaline earth metal ions are all eluted. Cd 2+ 400 μL of the solution was added dropwise to the fluorescence detection test pap...

Embodiment 2

[0045] Take 1g of rice to digest and remove the acid and leave a total of 5mL of the metal mixed solution, add a certain amount of standard cadmium chloride solution, so that the added Cd 2+ The concentration in the solution is 2.0 μ M, and others are the same as in Example 1, and the result is Cd 2+ The concentration was 1.93 μM.

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Abstract

The present invention relates to rapid detection of Cd<2 + > in rice, is a method for detection of Cd<2 + > in rice by combination of solid phase extraction, separation and fluorescent colorimetry, and the method is as follows: metal ions in a mixed solution obtained by digestion of rice can be enriched in filler on a sulfonated polymer filled column, Cu<2 + >, Ni<2 + >, Zn<2 + > and other heavy metal ions can be removed by stepwise elution, a mixed solution containing Cd<2 + >, Mn<2 + > and K<+ >, Na < + > ,Ca<2 + >, Mg<2 + > and other alkali metal and alkaline earth metal ions can be separated; the solution containing Cd<2 + > is added dropwise to test paper fixed with a cadmium ion fluorescence indicator; the cadmium ion fluorescence indicator is excited by light with the 365nm specific wavelength, electronic imaging equipment is used for capturing indicator fluorescent color changes before and after the addition of the Cd<2 + >. The color change values of red, green and blue (RGB) three channels in an image before and after the color change can be extracted for construction of a standard curve of Cd<2 + > and corresponding concentration gradient. In the testing process of a sample, the obtained sample change value is compared with values in the curve so as to perform quantitative analysis of Cd<2 + > in an unknown sample.

Description

technical field [0001] The present invention relates to the enrichment of metal ions in rice samples, Cd 2+ Separation and detection of metal ions in rice digested solution with a sulfonated polymer-filled extraction column to enrich metal ions and separate Cd from them 2+ and several other metal ions, and then use fluorescence colorimetry for Cd 2+ method of detection. Background technique [0002] Cadmium is a heavy metal poison, in addition to causing acute and chronic poisoning, it also has certain teratogenic, carcinogenic and mutagenic effects. People have known the existence of cadmium for more than a hundred years, but in the past only paid attention to occupational poisoning. It was not until 1934 that "cadmium rice poisoning" occurred in Fukuyama, Japan, which led to "bone pain disease", also known as "itai pain disease", did not attract more attention. In 1967, it was determined that "bone pain disease" was mainly caused by heavy metals, especially cadmium pois...

Claims

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Application Information

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IPC IPC(8): G01N21/64G01N1/28G01N1/34
Inventor 冯亮李慧张雨关亚风
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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