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A method for measuring dalbavancin impurities

A dalbavancin and detection method technology, applied in the field of medical analysis, can solve problems such as poor solubility, ineffective liquid phase extraction, and ineffective free vaporization of 3-dimethylaminopropylamine, and achieve low equipment requirements, improve quality and The effect of drug safety and high recovery rate

Active Publication Date: 2019-10-15
HANGZHOU HUADONG MEDICINE GRP PHARMA RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In order to overcome the technical defects of poor solubility of dalbavancin in the prior art, 3-dimethylaminopropylamine in dalbavancin cannot be effectively free vaporized, and cannot be effectively extracted in liquid phase, the present invention provides a simple, universal, high detection sensitivity The method for the detection of 3-dimethylaminopropylamine in dalbavancin

Method used

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  • A method for measuring dalbavancin impurities
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  • A method for measuring dalbavancin impurities

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0072] Chromatographic conditions:

[0073] Column temperature: programmed temperature rise: the initial temperature was 60°C and kept for 8 minutes, then the temperature was raised to 220°C at a rate of 20°C per minute and kept for 8 minutes.

[0074] Injection port temperature: 250°C;

[0075] Flame ionization detector temperature: 300°C;

[0076] Carrier gas: nitrogen;

[0077] Carrier gas flow rate: 1.5ml / min;

[0078] Split ratio: 5:1.

[0079] 1. Detection

[0080] A. Preparation of the test solution:

[0081] Prepare 2.5mol / L sodium hydroxide solution for subsequent use;

[0082] Take about 0.1g of dalbavancin, weigh it accurately, put it in a stoppered test tube, add 1ml of prepared sodium hydroxide solution, shake to dissolve, add 1ml of acetonitrile, add 0.5g of sodium chloride, shake to mix thoroughly, Leave to stand for stratification, absorb the supernatant, and use it as the test solution for subsequent use;

[0083] B. Preparation of reference substance ...

Embodiment 2

[0132] The test sample and reference substance solutions were prepared with reference to Example 1. The difference is that the concentration of the sodium hydroxide solution in this embodiment is 2.0mol / L; the concentration of acetonitrile is 2ml; the inorganic salt is potassium chloride, and the addition amount is 2g.

[0133] Chromatographic conditions:

[0134] Column temperature: programmed temperature rise: the initial temperature was 60°C and kept for 8 minutes, then the temperature was raised to 220°C at a rate of 20°C per minute and kept for 8 minutes.

[0135] Injection port temperature: 230°C;

[0136] Flame ionization detector temperature: 280°C;

[0137] Carrier gas: nitrogen;

[0138] Carrier gas flow rate: 1.0ml / min;

[0139] Split ratio: 1:1;

[0140] The injection volume was 1 μl.

[0141] According to the above conditions, three batches of the test solution were detected, and no 3-dimethylaminopropylamine peak was detected in the chromatograms. After cal...

Embodiment 3

[0143] The test sample and reference substance solutions were prepared with reference to Example 1. The difference is that the sodium hydroxide solution in this embodiment is 10ml, the concentration is 3.0mol / L; the acetonitrile is 1ml; the inorganic salt is anhydrous sodium sulfate, and the addition amount is 1g.

[0144] Chromatographic conditions:

[0145] Column temperature: programmed temperature rise: the initial temperature was 60°C and kept for 8 minutes, then the temperature was raised to 220°C at a rate of 20°C per minute and kept for 8 minutes.

[0146] Injection port temperature: 270°C;

[0147] Flame ionization detector temperature: 320°C;

[0148] Carrier gas: nitrogen;

[0149] Carrier gas flow rate: 2.0ml / min;

[0150] Split ratio: 10:1;

[0151] The injection volume was 3 μl.

[0152] According to the above conditions, three batches of the test solution were detected, and no 3-dimethylaminopropylamine peak was detected in the chromatograms. After calcula...

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Abstract

The invention relates to the technical field of drug analysis, and discloses a method for detecting dalbavancin impurities. The present invention adopts direct sampling method to detect 3-dimethylaminopropylamine in dalbavancin. The method provided by the invention is simple and universal in operation and has low requirements on gas-phase related equipment; the assay method provided by the invention has high detection sensitivity and high recovery rate. The detection method provided by the invention improves the quality and medication safety of dalbavancin.

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. Background technique [0002] Dalbavancin (Dalbavancin, structural formula is as follows), also known as daugtomycin, is a new type of semi-synthetic glycopeptide antibiotic, which is a derivative of teicoplanin analogue A40926. Dalbavancin hydrochloride is the first and only intravenous antibiotic approved in a two-dose regimen for the treatment of ABSSSI. The mechanism of action of dalbavancin is the same as that of vancomycin and teicoplanin. It inhibits the biosynthesis of the cell wall of G+ bacteria and is widely used as a drug for the treatment of skin and soft tissue infections. Dalbavancin is a second-generation, semi-synthetic lipoglycopeptide that incorporates a lipophilic side chain into an enhanced glycopeptide backbone, and is effective in vitro against a variety of Gram-positive...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/60
Inventor 雍春
Owner HANGZHOU HUADONG MEDICINE GRP PHARMA RES INST
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