HPLC analysis method for hydroxychloroquine sulfate and related substances thereof

A technology for hydroxychloroquine sulfate and related substances, which is applied in the field of HPLC analysis of hydroxychloroquine sulfate and related substances, can solve the problems of small amount of impurities, complex mobile phase system, damage to instruments or chromatographic columns, etc., and achieves high accuracy and sensitivity. High, low cost effect

Pending Publication Date: 2022-02-18
SHANGHAI ZHONGXI PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The present invention is in order to solve the analysis method for hydroxychloroquine sulfate and related substances in the prior art, there is the impurity amount that can be detected at the same time is few, mobile phase system is complex and may bring irreversible damage to instrument or chromatographic column etc. problem, And provide a kind of HPLC analysis method of hydroxychloroquine sulfate and its related substances

Method used

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  • HPLC analysis method for hydroxychloroquine sulfate and related substances thereof
  • HPLC analysis method for hydroxychloroquine sulfate and related substances thereof
  • HPLC analysis method for hydroxychloroquine sulfate and related substances thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Investigate the effect of different filter membranes on the test results

[0052] Prepare the solution of the hydroxychloroquine sulfate of 0.2mg / mL, centrifuge and get the supernatant (5000 rpm, centrifugal 5 minutes) and the microporous filter membrane of 0.45 μ m different materials (the size and pore diameter of polyvinylidene fluoride membrane PVDF) with centrifuge 25mm*0.45μm, the size and pore diameter of polytetrafluoroethylene membrane PTFE is 25mm*0.45μm, the size and pore diameter of polyamide Nylon is 25mm*0.45μm) filter. The solvent for dissolving hydroxychloroquine sulfate here is a solution containing perchloric acid (perchloric acid: acetonitrile; water=0.05:10:90; v / v / v).

[0053] Use YMC-Triart Phenyl 150*4.6mm ID S-3um, 12nm as the chromatographic column, the mobile phase is: 0.1% perchloric acid-acetonitrile for gradient elution, the elution program is:

[0054] time (min) A(％) B(％) 0.00 88.0 12.0 6.00 88.0 12.0 26.00 80...

Embodiment 2

[0061] Investigate the influence of solvent on the separation of hydroxychloroquine sulfate and its related substances.

[0062] Prepare a solution of 0.2 mg / mL hydroxychloroquine sulfate and related substances (concentration of impurity solution is 20 μg / mL), dissolve with different solvents a~d, and centrifuge to get the supernatant (5000 rpm, centrifuge for 5 minutes) ,carry out testing.

[0063] Solvent: a) H 2 O:ACN:HClO 4 =80:20:0.05(v / v / v); b) H 2 O:ACN:HClO 4 =90:10:0.05 (v / v / v); c) H 2 O: ACN=90:10 (v / v); d) H 2 O:ACN:HClO 4 =70:30:0.05 (v / v / v).

[0064] Use YMC-Triart Phenyl 150*4.6mm ID S-3um, 12nm as the chromatographic column, the mobile phase is: 0.1% perchloric acid-acetonitrile for gradient elution, the elution program is:

[0065] time (min) A(％) B(％) 0.00 88.0 12.0 6.00 88.0 12.0 26.00 80.0 20.0 31.00 65.0 35.0 36.00 65.0 35.0 37.00 50.0 50.0 40.00 50.0 50.0 40.10 88.0 12.0 45.00 88.0 1...

Embodiment 3

[0073] Investigate the influence of hydroxychloroquine sulfate concentration on the separation of hydroxychloroquine sulfate and its related substances

[0074] The hydroxychloroquine sulfate solution of preparation 0.5mg / mL (in the hydroxychloroquine sulfate crude drug that adopts in the embodiment all contains impurity 6 in table 1, namely hydroxychloroquine sulfate impurity D in the European Pharmacopoeia), centrifuge and get supernatant with centrifuge ( 5000 rpm, centrifuge for 5 minutes). The solvent dissolved here is a solution containing perchloric acid (perchloric acid:acetonitrile; water=0.05:10:90; v / v / v).

[0075] Use YMC-Triart Phenyl 150*4.6mm ID S-3um, 12nm as the chromatographic column, the mobile phase is: 0.1% perchloric acid-acetonitrile for gradient elution, the elution program is:

[0076]

[0077]

[0078] The detection wavelength is 220nm, the flow rate is 1mL / min, the column temperature is 25°C, and the injection volume is 10μL, and the chromatog...

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Abstract

The invention discloses an HPLC analysis method for hydroxychloroquine sulfate and related substances thereof, which comprises the steps of dissolving a tested substance in a solution containing perchloric acid, and carrying out HPLC detection, wherein the chromatographic conditions are as follows: a mobile phase comprises a mobile phase A and a mobile phase B; the mobile phase A is a perchloric acid solution; the mobile phase B is acetonitrile; and the chromatographic column is a phenyl column. According to the method, hydroxychloroquine sulfate, 12 related substances and contents thereof can be detected at the same time, and effective separation of hydroxychloroquine sulfate and related substances thereof is realized; and the mobile phase system is simple and does not cause damage to an instrument or a chromatographic column, and the method is simple to operate, high in precision, good in reproducibility, high in sensitivity, high in accuracy and low in cost.

Description

technical field [0001] The invention relates to an HPLC analysis method for hydroxychloroquine sulfate and related substances thereof. Background technique [0002] Hydroxychloroquine sulfate, chemical name: 2-[[4-[(7-chloro-4-quinolyl)amino]pentyl]ethylamino]-ethanol sulfate, is an antimalarial agent, usually used to treat Rheumatoid arthritis, systemic erythema lupus, sarcoidosis and other diseases. Hydroxychloroquine sulfate has a good oral effect and can be quickly and completely absorbed by the human body. Therefore, hydroxychloroquine sulfate is a chloroquine-like antimalarial drug widely used in clinical practice. [0003] At present, although some documents and pharmacopoeias have reported the analytical methods about hydroxychloroquine sulfate and related substances, there are some defects in them. Specifically as follows: European Pharmacopoeia (EP) adopts UPLC liquid phase method to measure impurity content in hydroxychloroquine sulfate, and it adopts sodium hep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/74
CPCG01N30/02G01N30/06G01N30/74
Inventor 徐洪鸿刘莉周敏张婷
Owner SHANGHAI ZHONGXI PHARMA
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