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A method capable of simultaneously detecting mercuric chloride and mercuric bromide

A technology of mercuric bromide and mercuric chloride, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high quantitative limit, cumbersome procedures, and long time consumption, so as to save time and cost, simplify detection steps, and improve sensitivity Effect

Inactive Publication Date: 2019-10-11
中国医科大学
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Conventional methods for the determination of mercuric chloride are mostly atomic fluorescence spectrometry and cold atomic absorption spectrometry to determine the content of total mercury in biological samples, which require high-pressure digestion or microwave digestion steps, which usually take 3-4 hours, which are time-consuming and complicated. Complicated, not suitable for clinical first aid testing
[0004] The inventor found in the research that mercuric chloride in biological samples can be detected by gas chromatography-mass spectrometry ("Detection of mercuric chloride in biological samples by gas chromatography-mass spectrometry", Chinese Journal of Health Inspection, 2016, Vo.l26, No.17), but this method has great limitations: 1. It only detects mercuric chloride in the sample, and cannot detect mercuric bromide at the same time; 2. The limit of quantification is high and the lowest quantification The limit is 5 μg / g, and the sensitivity needs to be further improved; 3. The separation degree of mercuric chloride and mercuric bromide does not meet the requirements, and the two cannot be separated, so they cannot be detected separately; 4. It is not suitable for detecting mercuric chloride in plasma samples and mercuric bromide

Method used

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  • A method capable of simultaneously detecting mercuric chloride and mercuric bromide
  • A method capable of simultaneously detecting mercuric chloride and mercuric bromide
  • A method capable of simultaneously detecting mercuric chloride and mercuric bromide

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Embodiment 1

[0037] 1. Screening of different extraction solvents.

[0038] In order to improve the extraction recovery rate of mercuric chloride and mercuric bromide, the present invention investigates the influence of extraction solvents with different polarities on the extraction recovery rate of mercuric chloride and mercuric bromide.

[0039] The experimental process is as follows: take 0.5 g each of three blank urines, add the same amount of mercuric chloride and mercuric bromide standard stock solution, add 500 ng of skf-525a internal standard, add 0.01mol / L hydrochloric acid solution 1 ml, Use 2 ml ethyl acetate, 2 ml dichloromethane, and 2 ml cyclohexane to vortex and extract, centrifuge at 3 500 r / min for 10 min, absorb the supernatant, blow dry with nitrogen at room temperature, and reconstitute with 20 μl ethyl acetate. dissolved, and 1 μl was injected for analysis. The extraction recoveries of mercuric chloride and mercuric bromide were calculated respectively.

[0040] The ...

Embodiment 2

[0056] (1) Detection conditions.

[0057] Gas spectrometer: 7890B-5977A mass spectrometer produced by Aglient Company was used.

[0058] Chromatographic column: HP-5ms capillary column, specification: 30 m×0.25 mm, 0.25 μm;

[0059] Electronic ion bombardment source (EI source, 70 eV), full ion scanning, scanning mass range of 40 amu ~ 600 amu.

[0060] The carrier gas was high-purity helium (99.9%) at a flow rate of 1.0 ml / min.

[0061] Temperature program: initial column temperature is 60°C, keep for 1 min, raise temperature to 180°C at 15°C / min, hold for 8 min, then raise temperature to 260°C at 30°C / min, inlet temperature is 265°C, ion source temperature is 230°C.

[0062] (2) Sample processing.

[0063] Take 0.5 g of human urine, add 500 ng of skf-525a internal standard, add 1 ml of 0.01mol / L hydrochloric acid solution, vortex and extract with 2 ml of ethyl acetate, centrifuge at 3 500 r / min for 10 min, and absorb the supernatant solution, dried under nitrogen at roo...

Embodiment 3

[0074] Take 0.5 g of the plasma to be tested, and determine the content of mercuric chloride and mercuric bromide in plasma as 1.34 μg / g and 2.76 μg / g according to the above method.

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Abstract

A method for detecting mercury chloride and mercury bromide at same time comprises the steps of (1) setting detection conditions; (2) treating samples; (3) preparing mercury chloride and mercury bromide stock solutions; (4) performing spectral analysis; (5) calculating contents. By using gas chromatography-mass spectrometry, it is possible to specifically detect mercury chloride and mercury bromide in a biological sample rather than detect only the content of total mercury in the biological sample; detection sensitivity is improved, detection steps are greatly simplified, and time and cost are saved.

Description

technical field [0001] The invention belongs to the field of biological material detection, in particular to a method capable of simultaneously detecting mercuric chloride and mercuric bromide. Background technique [0002] Halogenated high-mercury compounds, including mercuric chloride and mercuric bromide, are highly toxic inorganic substances with similar chemical structures and physical and chemical properties. Among them, mercuric chloride, commonly known as mercuric chloride, is an important reagent in analytical chemistry. It can also be used for the preservation of wood and anatomical specimens, leather tanning and steel engraving, etc. It is widely used in the field of industrial production. Mercury bromide is also a commonly used chemical reagent in drug analysis tests. Both mercury chloride and mercury bromide belong to the category of inorganic highly toxic substances, which can be absorbed through the respiratory tract, digestive tract or skin. In actual produ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
Inventor 袁慧雅刘俊亭
Owner 中国医科大学
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