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Analytical reagent for heavy metal measurement as well as preparation method and application thereof

An analytical reagent and diazotization technology, which is applied in the field of analytical chemistry, can solve problems such as low sensitivity, practical application limitations, and insufficient stability of the generated complex, and achieve the effects of improved detection sensitivity, improved sensitivity, and reliable measurement results

Inactive Publication Date: 2011-04-13
YUNNAN RES INST OF TOBACCO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some of these reagents generate complexes that are not stable enough, some have low sensitivity, and their practical applications are limited; Sensitivity can not meet the requirements of the determination

Method used

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  • Analytical reagent for heavy metal measurement as well as preparation method and application thereof
  • Analytical reagent for heavy metal measurement as well as preparation method and application thereof
  • Analytical reagent for heavy metal measurement as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] - Synthesis of analytical reagents

[0034] (1) Diazotization——mix 0.1 mol of aniline, 2.5 mL of concentrated hydrochloric acid and 3 mL of water, heat to dissolve, cool to below 5°C in an ice bath, and add 10 mL of 10% sodium nitrite aqueous solution dropwise under low temperature stirring. Continue to react for 30 minutes, add a small amount of urea to remove unreacted sodium nitrite. Dissolve 0.1moL of 8-aminoquinaridine in 20mL of 1:1 acetic acid, drop the above-mentioned diazonium salt into it under low temperature stirring, and add dilute sodium hydroxide at any time to control the pH value between 5-6, After coupling at low temperature for 2 hours, the crude product was obtained by filtration, and the low melting point part of the product was removed by sublimation to obtain a pure yellow product (5-phenylazo-8-aminoquinaridine), with a yield of 72%.

[0035] (2) Condensation——Dissolve 0.05mol of 5-phenylazo-8-aminoquinaridine in 6mL of absolute ethanol, heat to d...

Embodiment 2

[0037] - Chromatographic conditions used

[0038] The column is Waters Xterra TM RP 18 (5μm, 3.9×150), the mobile phase is: A 0.05moL / L pH=10.0 tetrahydropyrrole-acetic acid buffer solution, B acetonitrile (containing 0.05moL / LpH=10.0 tetrahydropyrrole-acetic acid buffer solution) and The volume ratio is changed according to: 0min (A 70%+B 30%), 10min (A 40%+B 60%) linearly increasing gradient, the injection volume is 20μL, under this condition, the standard sample and the actual sample are at a wavelength of 510nm , see chromatographic comparison figure 1 .

Embodiment 3

[0040] ——Determination of lead, cadmium and mercury in tobacco

[0041] Accurately weigh 0.5 g of the tobacco sample into a polytetrafluoroethylene microwave digestion tank, add 5 mL of concentrated nitric acid and 8 mL of 30% H 2 o 2 , digested in a microwave digestion furnace for 20min; after digestion, heated and evaporated on a hot plate until nearly dry, dissolved the residue with 20mL of 5% nitric acid, and transferred it to a 50mL volumetric flask. Add 5 mL of 0.1% 5-phenylazo-8-(2,4-dihydroxybenzaldehyde)-aminoquinaridine ethanol solution to the sample digestion solution, adjust the pH value to nearly neutral, and then add pH=10.0 Dilute 10 mL of borax-sodium hydroxide buffer solution with water to near the mark, and dilute to 50 mL. The solution is passed through the activated Waters Xterra at a flow rate of 10ml / min TM RP 18 After enrichment, the solid-phase extraction column was eluted with 1.0mL ethanol at a flow rate of 10ml / min. The volume of the eluent was a...

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Abstract

The invention discloses an analytical reagent for heavy metal measurement as well as a preparation method and application thereof. The heavy metal refers to lead, cadmium and mercury, in particular to a trace amount of lead, cadmium and mercury. The new analytical reagent provided in the invention has the chemical structure of the general formula (I) in the specification. The synthesis of the analytical reagent is synthesized through two steps of: coupling diazotized aniline with 8-aminoquinaldine to obtain 5-phenylazo-8-aminoquinaldine, and then condensing the 5-phenylazo-8-aminoquinaldine with 2,4-dyhydroxylbenzaldehyde to obtain a product of 5-phenylazo-8-(2,4-dyhydroxylbenzaldehyde)-condensed aminoquinaldine. In the invention, based on the newly synthesized analytical reagent, a new method for measuring the trace amount of lead, cadmium and mercury with high performance liquid chromatography is established and has the detection limit up to a mu g / L level, and a measurement result of the method is provided to be identical to a result of an inductive coupling plasma mass spectrum (ICP-MS) method through contrast.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, more specifically, the invention relates to an analytical reagent for determining lead, cadmium and mercury by high performance liquid chromatography. At the same time, the invention also relates to the preparation method of the agent and the application in the tobacco industry. Background technique [0002] Lead, cadmium, and mercury are important harmful elements in tobacco. Lead can damage the blood and decompose red blood cells. At the same time, it spreads to the organs and tissues of the whole body through the blood and enters the bones, causing radial nerve paralysis and finger tremors. Cadmium poisoning can cause muscle atrophy, joint deformation, unbearable bone pain, inability to sleep, and pathological fractures. Mercury can damage the nerve center and lead to nervous disorders, restlessness, and extreme pain. Therefore, the accurate determination of lead, cadmium and mercury in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D215/40G01N30/02G01N30/06
Inventor 杨光宇贺兵金永灿刘巍孔维松崔柱文
Owner YUNNAN RES INST OF TOBACCO SCI
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