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Method for detecting residues 1, 2-dibromoethane and 1, 3-dibromopropane in homopiperazine

A detection method, the technology of dibromoethane, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve high accuracy, good detection effect, good precision and durability

Active Publication Date: 2021-10-19
KPC PHARM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis of homopiperazine uses ethylenediamine as a starting material, and is prepared through three steps of sulfonylation, cyclization, and desulfonylation; however, the homopiperazine obtained by the above synthesis method may contain 1, 2-dibromoethane (introduced from synthetic raw material 1,3-dibromopropane), 1,3-dibromopropane (synthetic raw material residue) remains; homopiperazine is one of the starting materials of Fasudil hydrochloride, Therefore, it is necessary to detect and control the residues of 1,2-dibromoethane and 1,3-dibromopropane in quality control

Method used

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  • Method for detecting residues 1, 2-dibromoethane and 1, 3-dibromopropane in homopiperazine
  • Method for detecting residues 1, 2-dibromoethane and 1, 3-dibromopropane in homopiperazine
  • Method for detecting residues 1, 2-dibromoethane and 1, 3-dibromopropane in homopiperazine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0201] Adopt gas chromatograph to measure according to gas chromatography (Chinese Pharmacopoeia 2015 edition four general rules 0521), chromatographic condition is as follows:

[0202] Adopt capillary chromatographic column DB-624UI (30m×320μm×1.8μm); column temperature: start at 120°C, keep for 2min, raise the temperature to 180°C at a rate of 5°C / min, keep for 3min, then increase the temperature at 20°C / min Raise the temperature to 220°C and keep it for 0min;

[0203] The inlet temperature is 220°C, and the split ratio is 30:1;

[0204] The makeup gas flow rate is 30mL / min, and the detector (μECD) temperature is 260°C;

[0205] The carrier gas is nitrogen, and the flow rate of the carrier gas is 1mL / min;

[0206] The injection volume of the sample to be tested is 1μL, and the column flow rate is 1.5mL / min;

[0207] Obtain the chromatogram of 1,2-dibromoethane and 1,3-dibromopropane mixed standard control solution see Figure 15 shown.

[0208] Depend on Figure 15 It ...

Embodiment 2

[0210] Adopt gas chromatograph to measure according to gas chromatography (Chinese Pharmacopoeia 2015 edition four general rules 0521), chromatographic condition is as follows:

[0211] Adopt capillary chromatographic column DB-624UI (30m×320μm×1.8μm); column temperature: initial temperature is 120°C, keep for 2min, raise the temperature to 130°C at a rate of 5°C / min, keep for 6min;

[0212] The inlet temperature is 220°C, and the split ratio is 30:1;

[0213] The makeup gas flow rate is 30mL / min, and the detector (μECD) temperature is 260°C;

[0214] The carrier gas is nitrogen, and the flow rate of the carrier gas is 1mL / min;

[0215] The injection volume of the sample to be tested is 1μL, and the column flow rate is 1.5mL / min;

[0216] Obtain the chromatogram of 1,2-dibromoethane and 1,3-dibromopropane mixed standard control solution see Figure 16 shown.

[0217] Depend on Figure 16 It can be seen that under the chromatographic conditions of Example 2, the target pea...

Embodiment 3

[0219] Adopt gas chromatograph to measure according to gas chromatography (Chinese Pharmacopoeia 2015 edition four general rules 0521), chromatographic condition is as follows:

[0220] Adopt capillary chromatographic column DB-624UI (30m×320μm×1.8μm); column temperature: the initial temperature is 120°C, keep it for 2min, raise the temperature to 130°C at the rate of 5°C / min, keep it for 6min, then increase the temperature at 20°C / min Raise the temperature to 220°C and keep it for 1min;

[0221] The inlet temperature is 220°C, and the split ratio is 30:1;

[0222] The makeup gas flow rate is 30mL / min, and the detector (μECD) temperature is 260°C;

[0223] The carrier gas is nitrogen, and the flow rate of the carrier gas is 1mL / min;

[0224] The injection volume of the sample to be tested is 1μL, and the column flow rate is 1.5mL / min;

[0225] Obtain the chromatogram of 1,2-dibromoethane and 1,3-dibromopropane mixed standard control solution see Figure 17 shown.

[0226]...

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Abstract

The invention provides a method for detecting residues 1, 2-dibromoethane and 1, 3-dibromopropane in homopiperazine, which comprises the following steps of a) carrying out gas chromatography detection on a sample to be detected, and calculating the content of the residues 1, 2-dibromoethane and 1, 3-dibromopropane in homopiperazine according to the detection result and an established standard curve. A chromatographic column for gas chromatography detection is a capillary chromatographic column DB-624UI, the temperature of a sample inlet is 210-230 DEG C, and a detector is an electron capture detector. Compared with the prior art, the detection method provided by the invention has the advantages that optimized chromatographic conditions are adopted, and the detection effect on 1, 2-dibromoethane and 1, 3-dibromopropane is good; the detection method is high in accuracy, good in sensitivity, precision and durability, and suitable for detection of residues 1, 2-dibromoethane and 1, 3-dibromopropane in homopiperazine.

Description

technical field [0001] The invention relates to the technical field of drug quality control, in particular to a method for detecting residues 1,2-dibromoethane and 1,3-dibromopropane in homopiperazine. Background technique [0002] Homopiperazine is a nitrogen-containing hetero seven-membered ring compound. It is an important pharmaceutical intermediate and an important product connecting the chemical industry and the pharmaceutical industry. It is widely used in medicine, pesticides, surfactants, energetic materials and other fields. . [0003] At present, the synthesis of homopiperazine uses ethylenediamine as a starting material, and is prepared through three steps of sulfonylation, cyclization, and desulfonylation; however, the homopiperazine obtained by the above synthesis method may contain 1, 2-dibromoethane (introduced from synthetic raw material 1,3-dibromopropane), 1,3-dibromopropane (synthetic raw material residue) remains; homopiperazine is one of the starting m...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/54G01N30/60G01N30/70G01N30/86
CPCG01N30/02G01N30/06G01N30/6078G01N30/54G01N30/70G01N30/8679
Inventor 陈云建杨建玲
Owner KPC PHARM INC
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