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Control method for determining content of furfurylamine in furosemide

A technology of furosemide and medium furfurylamine, which is applied in the field of analytical chemistry, can solve the problems of increasing the risk of furosemide precipitation and blockage of instruments, and achieve the effects of ensuring effectiveness and safety, accurate quantification, and strong specificity

Inactive Publication Date: 2020-04-03
南京科宁检测科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Furosemide has a high solubility in sodium hydroxide solution, but directly entering the acidic mobile phase will increase the risk of furosemide precipitation and even block the instrument

Method used

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  • Control method for determining content of furfurylamine in furosemide
  • Control method for determining content of furfurylamine in furosemide
  • Control method for determining content of furfurylamine in furosemide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Instrument High performance liquid chromatograph: Shimadzu, LC-2030C, UV detector.

[0046] Column: Ultimate AQ-C 18 (4.6mm × 250mm, 5μm).

[0047] Mobile phase: the aqueous phase is phosphate buffer (0.5 g of sodium heptanesulfonate is dissolved in 1000 ml of water, and the pH is adjusted to 2.6 with phosphoric acid); the organic phase is acetonitrile.

[0048] Elution gradient:

[0049] time (min) Mobile phase A (%) Mobile phase B (%) 0 95 5 20 95 5 23 30 70 29 30 70 30 95 5 45 95 5

[0050] The flow rate is 1.0ml / min

[0051] The column temperature is 35°C

[0052] Detection wavelength: 210nm

[0053] Injection volume: 50μl

[0054] Diluent: 0.1mol / L hydrochloric acid solution

[0055] Sample processing: Take 20mg of this product, accurately weigh it, put it in a 10ml measuring bottle, add 0.5ml of 0.2M sodium hydroxide solution to dissolve it, and then quantitatively dilute it with a diluent (0.1mol / L hyd...

Embodiment 2

[0059] The equipment is the same as in Example 1.

[0060] Column: Thermo Hypersil BDS C 18 4.6mm×250mm, 5μm is applicable).

[0061] The diluent is the same as in Example 1

[0062]Mobile phase: the aqueous phase is phosphate buffer (0.3 g of sodium octane sulfonate is dissolved in 1000 ml of water, and the pH is adjusted to 2.8 with phosphoric acid); the organic phase is methanol. Aqueous phase: organic phase = 90:10.

[0063] The flow rate is 1.5ml / min

[0064] The column temperature is 40°C

[0065] Detection wavelength: 210nm

[0066] Injection volume: 10μl

[0067] Diluent: 0.05mol / L hydrochloric acid solution

[0068] Sample processing: 2ml of furosemide injection, placed in a 10ml volumetric bottle, quantitatively diluted with diluent to the mark, shaken well, centrifuged, and the supernatant was taken as the test solution; an appropriate amount of the impurity furfuramide reference substance was taken and dissolved in the diluent And quantitatively diluted to...

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PUM

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Abstract

The invention discloses an analysis method for determining the content of furfurylamine in furosemide, which comprises the following steps: dissolving furosemide with sodium hydroxide, neutralizing furosemide with hydrochloric acid, determining furosemide by high performance liquid chromatography, and taking a mixed solution of phosphate buffer salt and acetonitrile as a mobile phase by using a C18 chromatographic column. The invention provides a method for quickly determining furfurylamine in furosemide, which is strong in specificity, high in sensitivity, high in accuracy, simple and convenient to operate and capable of more effectively controlling the quality of furosemide.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, in particular to an analytical method for determining furosemide content in furosemide by high performance liquid chromatography. Background technique [0002] Furosemide, chemical name Furosemide. It is widely used clinically to treat edema associated with heart failure, and can also be used alone or in combination with other antihypertensive drugs to treat hypertension. Its structural formula is as follows: [0003] [0004] The synthesis of furosemide mostly uses furfurylamine and 2,4-dichloro-5-sulfonamidobenzoic acid as starting materials, and furosemide is obtained through the steps of substitution reaction and purification. The content of chloro-5-sulfonamidobenzoic acid was used to monitor the end point of the reaction, and the residual amount of furfurylamine was easily ignored. The structural formula of furfurylamine is as follows: [0005] The rapid and accurate det...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 朱亚芳陈迅
Owner 南京科宁检测科技有限公司
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