Measurement method of content of cyanide in drugs

A method of determination and technology of drugs, which is applied in the detection of drug components and the determination of cyanide content in drugs, can solve the problems of high detection limit, damage to instruments, failure to meet quality control and environmental protection, and achieve optimal detection limits, The effect of less precision

Inactive Publication Date: 2019-03-15
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, for drugs with complex matrices such as high chlorine and high organic matter, directly using ion chromatography to detect the cyanide content in them, the baseline noise is very loud, the instrument is damaged, and the detection limit is high, which cannot meet the requirements of quality control and environmental protection.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A method for assaying cyanide content in medicine, comprising the following steps:

[0021] (1) Pretreatment of drug samples by acid steaming method

[0022] The drug sample is compound drug or synthetic drug with complex matrix (1701).

[0023] Accurately weigh 0.5g (accurate to 0.0001g) of drug sample 1701, put it in a 250mL three-neck flask, add 50mL of ultrapure water, then quickly add 1mL of phosphoric acid, immediately cover the bottle stopper, and directly use an acid steamer for heating and acid steaming. Treatment, the cyanide (CN - ) is completely converted and separated from the drug sample, and absorbed with the absorption liquid to obtain the absorption liquid to be tested for cyanide.

[0024] (2) Determination of cyanide by ion chromatography

[0025] CN in the absorption liquid to be measured that step (1) obtains with ion chromatography analysis - content, the chromatographic conditions adopted are: amperometric detector;

[0026] Ag working electr...

Embodiment 2

[0052] A kind of assay method of cyanide content in medicine, basic steps are the same as embodiment 1.

[0053] The difference is:

[0054] The drug sample is compound drug or synthetic drug containing high salt.

[0055] Accurately weigh 1.0g (accurate to 0.0001g) of the drug sample, place it in a 250mL three-neck flask, add 50mL of ultrapure water, then quickly add 2mL of sulfuric acid, immediately cover the bottle stopper, and use a round-bottomed flask for heating and acid steaming. Cyanide (CN - ) is completely converted and separated from the drug sample, and absorbed with the absorption liquid to obtain the absorption liquid to be tested for cyanide.

Embodiment 3

[0057] A kind of assay method of cyanide content in medicine, basic steps are the same as embodiment 1.

[0058] The difference is:

[0059] The drug samples are compound drugs or synthetic drugs containing high organic matter.

[0060] Accurately weigh 0.8g (accurate to 0.0001g) of the drug sample, put it in a 250mL three-neck flask, add 50mL of ultrapure water, then quickly add 1.6mL of oxalic acid and phosphoric acid, immediately cover the bottle stopper, and directly heat it with an acid steamer Acid steam treatment, the cyanide (CN - ) is completely converted and separated from the drug sample, and absorbed with the absorption liquid to obtain the absorption liquid to be tested for cyanide.

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Abstract

The invention discloses a measurement method of the content of cyanide in drugs. The method comprises the following steps: (1), performing pretreatment on a drug sample through an acid distilling method: performing heating distilling through an acid distiller or a round-bottom flask, completely converting and separating out cyanide from the drug sample, and absorbing the cyanide through sodium hydroxide, so as to obtain a cyanide absorption liquid to be tested; (2), measuring the cyanide through an ion chromatography method: ensuring that the adopted chromatographic conditions are as follows:an ampere detector, an Ag working electrode, an Ag/AgCl reference electrode, an anion separating column, an anion protective column, injection volume of 25 micro liters, flow rate of 1.0 mL/min, temperature of 30 DEG C, and a NaOH solution with the flowing phase being 4mmol/L. The method has the advantages that the concentration of CN- presents a good linear relation within a measurement range, the detection limit is 0.0103 microgram/g, the sample adding standard recovery is 96.0 to 101.1 percent, and the degree of precision is 1.01 to 2.07 percent; the chromatographic conditions can obtain the superior detection limit and precision degree and smaller leaching time, the cyanide retention time can reach 7.78 min, and the lowest detection limit is 0.004 gm/L.

Description

technical field [0001] The invention relates to the technical field of detection methods of chemistry and medicine, in particular to a detection method of pharmaceutical ingredients, which is a kind of cyanide (CN) in medicine - ) content determination method. Background technique [0002] Most people know that cyanide is a highly toxic substance, which can produce extreme toxicity to the human physiological system. Murder or suicide with cyanide is not uncommon in previous novels or films. But now, in metallurgy, medicine, electroplating, rubber, pesticide production and other industrial fields, the environmental problems caused by cyanide are becoming more and more serious, which will have a serious impact on residents and human living environment. Therefore, it is very necessary to have a quick and easy detection method or detection means for cyanide. [0003] At present, the quantitative detection methods for cyanide mainly include: isonicotinic acid-pyrazolone spectr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/96
CPCG01N30/96
Inventor 栾绍嵘张芳芳倪力军
Owner EAST CHINA UNIV OF SCI & TECH
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