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Method for determining impurities in dalbavancin hydrochloride

A dalbavancin hydrochloride, quantitative dilution technology, applied in the field of pharmaceutical analysis, can solve problems such as residues, titration sensitivity and accuracy not meeting requirements, poisoning, etc.

Pending Publication Date: 2021-09-28
CHONGQING QIANTAI BIOLOGICAL MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 3-Dimethylaminopropylamine is used as a starting material in the synthesis of dalbavancin, and there may be some residues in the final product
3-Dimethylaminopropylamine is a highly toxic compound that has a strong irritating effect on the skin and can cause severe poisoning if inhaled or taken orally
[0008] Due to the high requirements of the purity of the final product, the residual content of 3-dimethylaminopropylamine is very low. When the conventional analysis method is used to determine the acid-base titration method, the sensitivity and accuracy of the general titration method cannot meet the requirements.

Method used

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  • Method for determining impurities in dalbavancin hydrochloride
  • Method for determining impurities in dalbavancin hydrochloride
  • Method for determining impurities in dalbavancin hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] High performance liquid chromatography: LC-2030C

[0046] Chromatographic column: Octadecylsilane bonded silica gel column (Ultimate ® C18, 4.6mm×250mm, 5 µm)

[0047] Mobile phase: 0.02mol / L sodium dihydrogen phosphate dihydrate aqueous solution is mobile phase A; acetonitrile is mobile phase B

[0048] The elution procedure of mobile phase A and B is:

[0049] time (min) Mobile phase A (%) Mobile phase B (%) 0 90 10 5 85 15 15 20 80 20 20 80 21 90 10 25 90 10

[0050] Flow rate: 1.0ml / min

[0051] Wavelength: 210nm

[0052] Injection volume: 50ul

[0053] Column temperature: 40°C

[0054] Implementation steps:

[0055] Boric acid-borax buffer: 0.05mol / L borax aqueous solution-0.2mol / L boric acid aqueous solution = 55:45 (v / v) Derivative reagent: 5mg / ml fluorenylmethoxycarbonyl chloride acetonitrile solution

[0056] Control solution: Accurately weigh about 50 mg of 3-dimethylaminopropylamine in a 10ml measur...

Embodiment 2

[0061] High performance liquid chromatography: Agilent1260

[0062] Derivatization reagent: 2.5mg / ml benzoyl chloride acetonitrile solution;

[0063] All the other conditions are with embodiment 1;

[0064] Implementation steps:

[0065] Take each 50 μl of the blank, the reference substance and the derivative solution of the test substance and inject them into the liquid chromatograph, and record the chromatograms. see attached results figure 2 .

Embodiment 3

[0067] High performance liquid chromatography: Agilent 1260

[0068] Chromatographic column: Octadecylsilane bonded silica gel column (Ultimate ® C18, 4.6mm×250mm, 5 µm) Mobile phase: 0.02mol / L aqueous solution of sodium dihydrogen phosphate dihydrate as mobile phase A; acetonitrile as mobile phase B. The elution procedure of mobile phase A and B is:

[0069] time (min) Mobile phase A (%) Mobile phase B (%) 0 90 10 5 85 15 15 20 80 20 20 80 21 90 10 25 90 10

[0070] Flow rate: 1.0ml / min

[0071] Wavelength: 265nm

[0072] Injection volume: 50ul

[0073] Column temperature: 40°C

[0074] Implementation steps:

[0075] Boric acid-borax buffer solution: 0.05mol / L borax aqueous solution-0.2mol / L boric acid aqueous solution=55:45 (v / v)

[0076] Derivatization reagent: 2.5mg / ml benzoyl chloride acetonitrile solution

[0077] Control solution: Accurately weigh about 50 mg of 3-dimethylaminopropylamine in a 10ml measuring b...

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Abstract

The invention discloses a method for detecting impurities in dalbavancin hydrochloride. According to the method, the 3-dimethylaminopropylamine in the dalbavancin hydrochloride is detected by adopting a pre-column derivatization reverse high-performance liquid chromatography. The detection method is suitable for detecting the content of 3-dimethylaminopropylamine in the acid compound dalbavancin, and is high in universality, good in system durability, good in stability and low in detection cost.

Description

technical field [0001] The invention belongs to the technical field of medical analysis, in particular to an analysis method for determining 3-dimethylaminopropylamine in dalbavancin hydrochloride. Background technique [0002] Dalbavancin Hydrochloride is Dalbavancin A 0 、A 1 , B 0 , B 1 and B 2 The hydrochloride salt of a mixture of equal components, in which dalbavancin B 0 The main component, these five components have the same core structure, its structural formula is as follows, the chemical formula and molecular weight of each component are shown in Table 1: [0003] [0004] Darbavansing R 1 R 2 molecular formula molecular weight A 0 CH(CH 3 ) 2 H C 87 h 98 N 10 o 28 Cl 2 1802.7 A 1 CH 2 CH 2 CH 3 H C 87 h 98 N 10 o 28 Cl 2 1802.7 B 0 CH 2 CH(CH 3 ) 2 H C 88 h 100 N 10 o 28 Cl 2 1816.7 B 1 CH 2 CH 2 CH 2 CH 3 H C 88 h 1...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/74
CPCG01N30/02G01N30/06G01N30/30G01N30/32G01N30/34G01N30/74
Inventor 周莹岳崇斌易中宏吴禄春奚萍英袁建栋
Owner CHONGQING QIANTAI BIOLOGICAL MEDICINE
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