Method for detecting formic acid, acetic acid and acetone in ipratropium bromide solution for inhalation

A technology of ipratropium bromide and detection method is applied in the field of drug analysis and achieves the effects of accurate results, guaranteed product quality and simple method

Active Publication Date: 2019-12-31
SICHUAN PURITY PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The technical problem solved by the present invention is: provide the detection method of formic acid, acetic acid and acetone in the ipratropium bromide solution for inhalation, easy and simple to operate, accurate result, solve the problem that there is not yet a method in the prior art that can simultaneously measure the ipratropium for inhalation Ammonium bromide solution formic acid, acetic acid and acetone problem

Method used

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  • Method for detecting formic acid, acetic acid and acetone in ipratropium bromide solution for inhalation
  • Method for detecting formic acid, acetic acid and acetone in ipratropium bromide solution for inhalation
  • Method for detecting formic acid, acetic acid and acetone in ipratropium bromide solution for inhalation

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Embodiment 1

[0045] The present embodiment discloses the method of adopting high performance liquid chromatography of the present invention to measure formic acid, acetic acid and acetone in the ipratropium bromide solution for inhalation, specifically:

[0046] Instrument and chromatographic conditions:

[0047] Shimadzu LC-2010AHT liquid chromatograph; chromatographic column: Agilent ZORBAX SB-Aq 4.6×250mm, 5μm; chromatographic column temperature is 30°C; 2 PO 4 Buffer solution (adjust the pH to 2.7 with phosphoric acid) as mobile phase A, acetonitrile as mobile phase B for gradient elution, the flow rate is 1.0ml / min; detection wavelength: using variable wavelength detection, the retention time is 215nm at 0-6min , when the retention time is 6-15min, it is 265nm; the gradient elution procedure is as follows:

[0048] time (min) Mobile phase A(%) Mobile phase B(%) 0 100 0 10 90 10 12 100 0 15 100 0

[0049] .

[0050] Specific detection steps:...

Embodiment 2

[0057] This embodiment discloses the accuracy test of the detection method of the present invention.

[0058] Adopt the method of embodiment 1 to carry out accuracy test, if as shown in the table below:

[0059] Extract name Recovery rate RSD formic acid 98.6％～104.7％ 2.1％ Acetic acid 99.8％～101.8％ 0.7％ acetone 98.7％～101.4.0％ 0.9％

[0060] As can be seen from the above table, the recovery rates of formic acid, acetic acid, and acetone are all between 95.0%~105.0%, and the RSDs of each recovery rate are all less than 5%, showing that the accuracy of the inventive method is good.

[0061] The method for examining the accuracy in this embodiment belongs to the prior art.

Embodiment 3

[0063] This embodiment discloses the detection limit and quantitative limit test of the detection method of the present invention.

[0064] Adopt the method of embodiment 1 to carry out detection limit test, if as shown in the table below:

[0065] Detection limit test result table

[0066] Extract name Detection limit (ng) S / N formic acid 5.61 ＞3 Acetic acid 21.03 ＞3 acetone 36.27 ＞3

[0067] .

[0068] Adopt the method of embodiment 1 to carry out quantitative limit test, if as shown in the following table:

[0069] Quantitative limit test result table

[0070] Extract name Quantitation limit (ng) S / N Peak area RSD formic acid 18.7 ＞10 ＜5.0％ Acetic acid 70.1 ＞10 ＜5.0％ acetone 120.9 ＞10 ＜5.0％

[0071] .

[0072] The results show that when the signal-to-noise ratio S / N>3, the detection limits of formic acid, acetic acid and acetone in the detection method of the present invention are 5.61ng...

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Abstract

The invention discloses a method for detecting formic acid, acetic acid and acetone in an ipratropium bromide solution for inhalation, and solves the problem that a method for simultaneously determining formic acid, acetic acid and acetone in the ipratropium bromide solution for inhalation is unavailable in the prior art. According to the detection method disclosed by the invention, reversed-phasehigh-performance liquid chromatography is adopted for detection, diisopropyl substituted octadecylsilane bonded silica is used as a filler, a buffer salt solution with the pH value of 2.0-3.3 is usedas a mobile phase A, and an organic solvent is used as a mobile phase B, formic acid and acetic acid are eluted according to a ratio of A to B being (90-100):(0-10) to generate peaks, and then acetone is eluted according to a ratio of A to B being (75-100):(0-25) to generate peaks; the organic solvent is selected from one or more than two of acetonitrile, isopropanol, ethanol, tetrahydrofuran andmethanol. According to the method, the formic acid, the acetic acid and the acetone in the ipratropium bromide solution for inhalation can be rapidly and accurately measured, the product quality of the ipratropium bromide solution for inhalation is effectively guaranteed, and the medication safety is guaranteed.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a detection method for formic acid, acetic acid and acetone in ipratropium bromide solution for inhalation. Background technique [0002] Ipratropium bromide solution for inhalation is used as a bronchodilator for the maintenance treatment of bronchospasm caused by chronic obstructive pulmonary disease, including chronic bronchitis and emphysema. Clinically, it is often used in combination with inhaled β-receptor agonists to treat chronic obstructive pulmonary diseases, including chronic bronchitis and acute bronchospasm caused by asthma. [0003] Formic acid, acetic acid and acetone are the extracts of the ipratropium bromide solution for inhalation. In order to ensure the safety of the drug, it is necessary to control the content of formic acid, acetic acid and acetone. Formic acid and acetic acid are strong organic acids, and methods for determining organic acids in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/34G01N30/89G01N30/86
CPCG01N30/34G01N30/89G01N30/8679G01N2030/047
Inventor 韩佳朱柯武李丛菊赵聪燕鞠悦杨丽吴林侯曙光吴君张宾郭城
Owner SICHUAN PURITY PHARM CO LTD
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