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A method for detecting ethylenediamine in lipoic acid injection

A technology of ethylenediamine and lipoic acid, applied in the field of detection, can solve the problems of easy tailing and peak bifurcation of the chromatographic column, high corrosion of the sampling system, and poor sampling accuracy.

Active Publication Date: 2021-09-10
CHENGDU BRILLIANT PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, gas chromatography is used to measure ethylenediamine, but it is very corrosive to the sampling system, and it is easy to tail and peak bifurcation in the chromatographic column, resulting in poor sampling accuracy and unable to meet the limit of ±5% of the labeled amount Require

Method used

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  • A method for detecting ethylenediamine in lipoic acid injection
  • A method for detecting ethylenediamine in lipoic acid injection
  • A method for detecting ethylenediamine in lipoic acid injection

Examples

Experimental program
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Effect test

Embodiment 1

[0053] Detection of ethylenediamine content in lipoic acid injection:

[0054] Chromatographic column: RFIC IonPac CG17, 4mm*50mm, CS17, 4mm*250mm;

[0055] Mobile phase: 15mmol / L methanesulfonic acid is mobile phase A, acetonitrile is mobile phase B, and the volume ratio is 9:1;

[0056] Detector: The detector is a conductivity detector with a suppressor CERS500, 4mm;

[0057] Feed volume: 10 μl;

[0058] Column temperature: 30°C;

[0059] Flow rate: 0.8ml / min;

[0060] Detection steps:

[0061] Accurately measure 1ml of this product, put it in a 100ml measuring bottle, add water to dissolve and dilute to the mark, shake well, and use it as the test solution; take another ethylenediamine reference substance, accurately weigh it, add water to dissolve and quantitatively dilute to 66.7μg / ml solution, as the reference solution. Precisely measure 10 μl each of the test solution and the reference solution, inject them into the ion chromatograph, record the chromatogram, and ...

Embodiment 2

[0068] The applicant fully considered the chemical properties of ethylenediamine, and used a conductivity detector to perform the measurement. Due to the material characteristics of ethylenediamine, there is still obvious tailing on the chromatographic column. Therefore, the asymmetry is used as an index to further screen the mobile phase and injection volume. The screening conditions are shown in Table 2.

[0069] Table 2IC chromatographic condition screening

[0070]

[0071] When the applicant investigates the amount of acetonitrile added, when the volume percentage is greater than 10%, the retention time of ethylenediamine will be less than 5min, which is not conducive to detection, and with the increase of the added amount of acetonitrile, the inhibitory signal is enhanced, so it is determined that methyl sulfonate The volume ratio of acid:acetonitrile is 90:10.

[0072] Research finds that with methanesulfonic acid as mobile phase, as the concentration of methanesulf...

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Abstract

The present invention specifically relates to a method for detecting ethylenediamine in lipoic acid injection, comprising the following contents: 1) taking ethylenediamine to prepare a reference substance solution; 2) taking zinc sulfate injection to prepare a test solution; 3) using ion Chromatography detects reference substance solution and need testing solution respectively, calculates ethylenediamine content; Wherein the chromatographic condition of ion chromatography comprises the following content: Chromatographic column: stationary phase is cation exchange resin or chemically bonded ion exchanger; Mobile phase: mobile phase Phase A is methanesulfonic acid, mobile phase B is methanol or acetonitrile; the volume ratio of mobile phase A and mobile phase B is 90-98:10-2. The ion chromatography method of the invention is used to detect ethylenediamine, which can effectively detect ethylenediamine, and the detection result is accurate, the baseline is flat, the peak shape is symmetrical, the stability is high, the repeatability is good, and the sensitivity is high.

Description

technical field [0001] The invention relates to the field of detection methods, in particular to a method for detecting ethylenediamine. Background technique [0002] Ethylenediamine, colorless or yellowish oily or watery liquid, has an odor similar to ammonia, and has a boiling point of 116-117.2°C. It is strongly alkaline and corrosive. It is mainly used as a solvent and analytical reagent. [0003] [0004] Ethylenediamine is a commonly used pH adjuster and co-solvent in drugs. The Food and Drug Administration requires a special method to control the content of ethylenediamine in drug approval, and tighten the limit. In the prior art, gas chromatography is used to measure ethylenediamine, but it is very corrosive to the sampling system, and it is easy to tail and peak bifurcation in the chromatographic column, resulting in poor sampling accuracy and unable to meet the limit of ±5% of the labeled amount Require. Contents of the invention [0005] At present, there i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 童庆国徐立宁罗鸣李英富苏忠海
Owner CHENGDU BRILLIANT PHARMA CO LTD
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