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HPLC determination method for detecting impurities in zanamivir and zanamivir-containing preparation

A zanamivir and preparation technology, applied in the field of drug impurity analysis and detection, can solve the problems of unsuitable quantitative and qualitative use, unstable chromatographic separation, long analysis time, etc., achieve excellent retention capacity, appropriate analysis time, and stable analysis method Effect

Active Publication Date: 2014-08-27
NANJING SIMCERE DONGYUAN PHARM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reversed-phase system, represented by C18 chromatographic column, does not retain zanamivir. Although the retention of zanamivir can be appropriately increased by selecting ion-pairing reagents, the analysis time is too long and it is not suitable as an analysis method for quality control of impurities.
On the other hand, because zanamivir is weakly acidic, it is easy to bind and adsorb in the amino column, resulting in unstable chromatographic separation, so the amino chromatographic column is not suitable for quantitative and qualitative purposes.

Method used

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  • HPLC determination method for detecting impurities in zanamivir and zanamivir-containing preparation
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  • HPLC determination method for detecting impurities in zanamivir and zanamivir-containing preparation

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Experimental program
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Effect test

Embodiment 1

[0037] Embodiment 1: 1.1 Preparation of sample solution: take an appropriate amount of inhaled powder mist, accurately weighed, add an appropriate amount of water for ultrasonic dissolution, add mobile phase dilution to make a solution containing 20 mg of zanamivir in every 1 ml, as the test sample solution.

[0038] 1.2 Instrument and chromatographic conditions:

[0039] Instrument: Agilent 1200 high performance liquid chromatography;

[0040] Chromatographic column: Waters HILIC Silica (4.6*150mm, 3μm);

[0041] Mobile phase: acetonitrile: 10mM ammonium formate (pH6.5) = 65:35;

[0042] Flow rate: 0.5ml / min;

[0043] Column temperature: 25°C;

[0044] Detection wavelength: 210nm and 234nm;

[0045] 1.3 Determination: Take 5 μl and inject it into the high-performance liquid chromatograph, and record the spectrum (attached figure 1 , figure 2 ).

Embodiment 2

[0047] 2.1 Preparation of sample solution: Take about 10 mg of inhalation powder, add mobile phase to prepare 0.5 mg / ml test solution, add 2 ml of 0.1 mol / L hydrochloric acid solution, let it stand, add 0.1 mol / L sodium hydroxide solution in 2 ml and, as an acid-destroyed sample solution.

[0048] 2.2 Instrument and chromatographic conditions:

[0049] Instrument: Agilent 1200 high performance liquid chromatography;

[0050] Chromatographic column: Waters HILIC Silica (4.6*150mm, 3μm);

[0051] Mobile phase: acetonitrile: 10mM ammonium formate (pH6.5) = 65:35;

[0052] Flow rate: 0.5ml / min;

[0053] Column temperature: 25°C;

[0054] Detection wavelength: 210nm and 234nm;

[0055] 2.3 Determination: Take 5 μl and inject it into the high-performance liquid chromatograph, and record the spectrum (attached image 3 , Figure 4 ).

Embodiment 3

[0057] 3.1 Preparation of sample solution: Take about 10 mg of inhalation powder, add mobile phase to prepare 0.5 mg / ml test solution, add 2 ml of 0.1 mol / L sodium hydroxide solution, let it stand, add 0.1 mol / L hydrochloric acid solution in 2 ml and, as a solution of alkali-destroyed samples.

[0058] 3.2 Instrument and chromatographic conditions:

[0059] Instrument: Agilent 1200 high performance liquid chromatography;

[0060] Chromatographic column: Waters HILIC Silica (4.6*150mm, 3μm);

[0061] Mobile phase: acetonitrile: 10mM ammonium formate (pH6.5) = 65:35;

[0062] Flow rate: 0.5ml / min;

[0063] Column temperature: 25°C;

[0064] Detection wavelength: 210nm and 234nm;

[0065] 3.3 Determination: Take 5 μl and inject it into the high-performance liquid chromatograph, and record the spectrum (attached Figure 5 , Figure 6 ).

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Abstract

The invention discloses an HPLC determination method for detecting impurities in zanamivir and a zanamivir-containing preparation. Hydrophilic interaction liquid chromatography (HILIC) is selected to separate zanamivir and its relevant substances, and the determination method for detecting impurities in zanamivir and the zanamivir-containing relevant preparation is concretely characterized in that a chromatographic column is an HILIC column, a mobile phase selects a polar organic solvent-buffer salt solution, a polar organic solvent-weak acid solution or an aqueous solution of a polar organic solvent, and the detection wavelength is 200-240nm. The determination method enables process impurities and degraded products of zanamivir to be rapidly and accurately detected, and has the characteristics of simple operation, high sensitivity, good repeatability and reliable result.

Description

technical field [0001] The invention relates to an HPLC assay method for detecting impurities in zanamivir and zanamivir-containing preparations, belonging to the field of drug impurity analysis and detection. Background technique [0002] Zanamivir was developed by GlaxoSmithKline and approved by the US FDA in August 1999. It is mainly used to treat influenza A and B. Philippine) is currently an internationally recognized drug for treating influenza. Zanamivir is the first approved influenza treatment drug since rimantadine went on the market in 1993, and it is also the first neuraminidase inhibitor influenza-like virus treatment drug. Its chemical name is: 5-acetylamino-4-[(aminoiminomethyl)-amino]-2,6-hydro-3,4,5-trideoxy-D-glycerol-D-semi Lactose-2-enoic acid. Molecular formula C 12 h 20 N 4 o 7 , relative molecular weight 332.3. This product is white or off-white powder, the solubility in water is about 18mg / ml at 20℃. [0003] There are mainly two types of chr...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 冯慧敏张斐许向阳檀爱民
Owner NANJING SIMCERE DONGYUAN PHARM CO LTD
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