Method for measuring furosemide by high performance liquid chromatography and genetic toxic impurity in its preparation

A high-performance liquid chromatography and furosemide technology, applied in the field of analytical chemistry, can solve the problems of weak ultraviolet response and neglected control, and achieve the effect of ensuring effectiveness and safety

Inactive Publication Date: 2019-10-29
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] Impurity B has a weak UV response and will be transformed into other impurities, so it is often easily ignored or not included in the quality control project according to the research; and then the control of genotoxic impurity C is ignored
There are very few relevant literature reports on the separation and determination of this impurity C in furosemide

Method used

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  • Method for measuring furosemide by high performance liquid chromatography and genetic toxic impurity in its preparation
  • Method for measuring furosemide by high performance liquid chromatography and genetic toxic impurity in its preparation
  • Method for measuring furosemide by high performance liquid chromatography and genetic toxic impurity in its preparation

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1. Instrument

[0031] High performance liquid chromatography: Shimadzu, LC-2030C, UV detector.

[0032] Column: Ultimate AQ-C 18 (4.6mm × 250mm, 5μm).

[0033] 2. Chromatographic conditions.

[0034] Mobile phase: the aqueous phase is phosphoric acid aqueous solution; the organic phase is acetonitrile.

[0035] Elution gradient:

[0036]

[0037] Flow rate: 1.0mL / min;

[0038] Column temperature: 35°C;

[0039] Detection wavelength: 270nm;

[0040] Injection volume: 20μL;

[0041] The diluent is a mixed solution of acetonitrile and water.

[0042] 3. Experimental steps.

[0043] Weigh 20mg of the impurity C reference substance, put it in a 10mL volumetric flask, add diluent to dissolve and dilute to the mark, and then quantitatively dilute to 1μg / mL solution successively to obtain the system suitability solution.

[0044] Weigh 100mg of furosemide respectively, put it in a 10mL volumetric flask, add diluent to dilute to the mark, and use it as the test sol...

Embodiment 2

[0049] 1. Instrument

[0050] With embodiment 1;

[0051] Column: Thermo BDS C 18 (4.6mm × 250mm, 5μm).

[0052] 2. Chromatographic conditions.

[0053] Mobile phase: the aqueous phase is phosphate buffered saline; the organic phase is acetonitrile;

[0054] Elution gradient: same as Example 1;

[0055] Flow rate: with embodiment 1;

[0056] Column temperature: with embodiment 1;

[0057] Detection wavelength: 220nm, 277nm;

[0058] Injection volume: 10μL;

[0059] Diluent is with embodiment 1.

[0060] 3. Experimental steps.

[0061] System suitability solution: same as Example 1;

[0062] Weigh an appropriate amount of furosemide injection respectively, add diluent to dilute properly, and use it as the test solution.

[0063] Detection was carried out according to the chromatographic conditions mentioned above.

[0064] Under the above detection conditions, prepare impurity B and C reference substance solutions of different concentrations, and detect them respect...

Embodiment 3

[0069] 1. Instrument

[0070] With embodiment 1;

[0071] Chromatographic column: with embodiment 1.

[0072] 2. Chromatographic conditions

[0073] With embodiment 2;

[0074] Diluent is with embodiment 1.

[0075] 3. Experimental steps.

[0076] System suitability solution: same as embodiment 1

[0077] Get the furosemide tablet and grind it, accurately weigh an appropriate amount, add a diluent to dilute properly, and use it as the test solution.

[0078] Detection was carried out according to the chromatographic conditions mentioned above.

[0079] Six parts of the test solution were prepared in parallel, and the average impurity C content was determined to be 37ppm, and the RSD value of the measurement result was 1.8%.

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Abstract

The invention discloses a method for measuring genetic toxic impurity C in furosemide by high performance liquid chromatography. The method comprises using a carbon-18 chromatographic column and usinga mixed solution of phosphoric acid water and acetonitrile as a mobile phase, wherein the volume ratio of the phosphoric acid water to the acetonitrile in the mobile phase is (97 to 85): (3 to 15); and using a mixed solution of acetonitrile and water as a diluent. The invention provides a method for separating and measuring the genetic toxic impurity C in furosemide, which finally simplifies thecontrol method of the genetic toxic impurities, improves the quality control requirement of the furosemide, and ensures the effectiveness and safety of the furosemide.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for separating and measuring genotoxic impurity C in furosemide by high performance liquid chromatography. Background technique [0002] Furosemide, also known as furosemide and furosemide, is a loop diuretic widely used in the treatment of congestive heart failure and edema. The reabsorption of electrolytes by renal tubules inhibits the reabsorption of Na by proximal tubules + , Cl - reabsorption of water, Na + , Cl - Increased excretion produces a diuretic effect. It is widely used clinically to treat edema associated with heart failure, including pulmonary edema and related kidney and liver diseases, and can also be used alone or in combination with other antihypertensive drugs to treat hypertension. [0003] Because furosemide is unstable to light, especially under acidic conditions, it is extremely sensitive to light, and will degrade a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/34
CPCG01N30/34G01N30/88G01N2030/8872
Inventor 谢晓燕朱亚芳
Owner 南京科宁检测科技有限公司
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