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A method for quantitatively detecting the valence state and content of chromium in chromium-containing substances

A technology for quantitative determination of chromium content, applied in the field of analysis, can solve the problem of inability to accurately measure the content of chromium elements in different valence states of chromium-enriched yeast cells, and achieve the effects of shortening measurement time, fast speed, and avoiding reduction.

Active Publication Date: 2017-03-15
INST OF MICROBIOLOGY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims to solve the problem that it is impossible to accurately measure the content of chromium elements in different valence states in chromium-rich yeast cells

Method used

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  • A method for quantitatively detecting the valence state and content of chromium in chromium-containing substances
  • A method for quantitatively detecting the valence state and content of chromium in chromium-containing substances
  • A method for quantitatively detecting the valence state and content of chromium in chromium-containing substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Example 1. Separation of Cr(III) and Cr(VI) in liquid samples and optimization of detection methods.

[0043] 1) Make the standard curve of total chromium:

[0044]With the concentrations of Cr(III) and Cr(VI) being 0.1, 0.5, 1, 5, 10, 50 and 100 μg / l respectively, and the molar ratio of Cr(III) and Cr(VI) being 1 as the standard sample, the The standard sample is quantitatively determined by ICP-MS to obtain chromatograms corresponding to different total chromium contents, with the total chromium content as the independent variable and the corresponding peak area as the dependent variable to obtain the standard curve of the total chromium content in the standard sample;

[0045] 2) Make Cr(III) and Cr(VI) standard curves:

[0046] The aforementioned standard samples were treated with EDTA Na at a concentration of 5 mM and pH 7.0 2 The aqueous solution is used as a chelating agent for chelation, the chelation temperature is 75°C, and the chelation time is 3h, and then...

Embodiment 2

[0051] Embodiment 2, establishment of valence state analysis method of solid sample chromium element

[0052] Since solid samples need to be digested by alkaline method before separation and determination, it is necessary to detect the influence of alkaline digestion and chelation treatment on sample separation and detection.

[0053] 1. The effect of alkaline digestion on the separation and determination of Cr(VI) in the sample.

[0054] Draw 20μg / l Cr(III) standard solution and 1μg / l Cr(VI) standard solution into a clean Erlenmeyer flask, accurately measure 5ml digestion solution, 0.04g MgCl 2 and 0.05ml of phosphate buffer solution with a concentration of 1.0M and a pH value of 7.0, continuously stirred the sample at room temperature for 5 minutes, then heated the sample to 95°C and maintained it for 60 minutes, then gradually cooled to room temperature, and continued to stir the sample during the process. Centrifuge at 4000g for 5 minutes to take the supernatant, wash the...

Embodiment 3

[0068] Embodiment 3, the determination of chromium element valence state in chromium-enriched yeast cell

[0069] 1) A Saccharomyces cerevisiae strain containing 0 μg / ml, 200 μg / ml, 400 μg / ml and 600 μg / ml Cr respectively 3+ (Chromium acetate) YEPD medium (glucose 20g / l, yeast powder 10g / l, peptone 20g / l) at 200rpm, 30°C for 24hr. Yeast cells were collected by centrifugation at 3000 g for 10 min, washed with deionized water until no chromium ions were detected in the eluate, and dried in an oven at 60°C to constant weight. Weigh 0.03g yeast stem cells, accurately measure 5ml alkaline digestion solution, 0.04g MgCl 2 and 0.05ml of phosphate buffer solution with a concentration of 1.0M and a pH value of 7.0. Stir the sample continuously at room temperature for 5 minutes, then heat the sample to 95°C and maintain it for 60 minutes, then gradually cool to room temperature. During the process, the sample is continuously stirred, and the supernatant is taken by centrifugation at 40...

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Abstract

The invention discloses a method for quantitative detection of chromium element valence and content in a chromium-containing substance. The method includes: adding a chromium-enriched yeast stem cell sample into an alkali digestive juice to conduct treatment, then performing centrifugation, adjusting the pH of conditioning fluid to obtain a to-be-detected solution; preparing a chromium standard solution, performing testing, and establishing a chromium stand solution standard curve; subjecting the to-be-detected solution to high performance liquid phase separation, using an inductively coupled plasma mass spectrometry to analyze the Cr(VI) content, conducting acid digestion, and directly using inductively coupled plasma mass spectrometry to analyze the total chromium content of the sample, calculating the Cr(III) content through the difference of the total chromium content and the Cr(VI) content of the sample. The method provided by the invention improves the accuracy of sample measurement, has the characteristics of small sample size and short detection time, saves the sample preparation amount and measurement time, can accurately and quantitatively measure chromium-enriched yeasts with different chromium enrichment amounts.

Description

technical field [0001] The invention belongs to the field of analysis, and relates to a method for detecting the valence state and content of chromium element in a sample, in particular to a method for quantitatively detecting the valence state and content of chromium element in chromium-containing substances. Background technique [0002] In the natural environment, chromium mainly exists stably in two valence states, namely Cr(III) and Cr(VI). The physiological functions of these two chromium ions are completely opposite. Cr(III) is an essential nutrient element for organisms, affecting the normal metabolism of glucose, lipids and proteins in organisms; while Cr(VI) is a recognized carcinogen and mutagen . Organisms deficient in Cr(III) can lead to diabetes-like symptoms. There are various forms of Cr(III) supplements, among which chromium-enriched yeast is considered to be a Cr(III) supplement with naturally occurring, high organic chromium content and high bioavailabil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 郭雪娜何秀萍张博润
Owner INST OF MICROBIOLOGY - CHINESE ACAD OF SCI
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