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Method for determining relevant substances in citalopram or salt thereof and preparation thereof

A technology of citalopram and related substances, which is applied in the field of analytical chemistry and can solve the problems of small amount of separated impurities and poor separation effect

Pending Publication Date: 2019-12-24
SUZHOU KELUN PHARMA RES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] Aiming at the shortcomings of the prior art detection citalopram hydrobromide and related substances in its preparations, the separation effect is not good, the number of separated impurities is small, etc., the invention provides a new method for the determination of citalopram or its salts and its preparations method of matter

Method used

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  • Method for determining relevant substances in citalopram or salt thereof and preparation thereof
  • Method for determining relevant substances in citalopram or salt thereof and preparation thereof
  • Method for determining relevant substances in citalopram or salt thereof and preparation thereof

Examples

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Effect test

Embodiment 1

[0057] Diluent: Phosphate buffer and organic mixed solution mixed at 80:20 (v / v); among them, phosphate buffer: take 6.6g of diammonium hydrogen phosphate, add 1000mL of water to dissolve, add 2mL of triethylamine, Shake well, and adjust the pH value to 6.1 with phosphoric acid; organic mixed solution: methanol-acetonitrile=40:60 (v / v).

[0058] Mixed impurity stock solution: Accurately weigh about 2.5mg of each of the 12 impurity reference substances of impurities Z2-Z13, place them in 10mL volumetric flasks, add diluent to dissolve and constant volume, shake well, and use as each impurity stock solution; Accurately measure 0.5 mL of each impurity stock solution, add it to a 10 mL volumetric flask, add diluent to constant volume, shake well, and use it as a mixed impurity stock solution.

[0059] The first system suitability solution: Accurately weigh 25 mg of citalopram hydrobromide raw material (source: Qionglai Branch of Sichuan Kelun Pharmaceutical Co., Ltd., batch 1), pu...

Embodiment 2

[0073] Except mobile phase A is 0.66% phosphate buffer saline, pH is 7.0, other chromatographic conditions are the same as embodiment 1. The first system suitability solution is tested and analyzed, and the test results are shown in Table 4 and figure 2 .

[0074] Table 4

[0075]

[0076]

[0077] Combining Table 4 and figure 2 Visible, the inventive method detects the first system suitability solution of citalopram hydrobromide, detects 12 kinds of known impurities and 3 kinds of unknown impurities altogether, and peak shape is good, between all impurities and between impurity and citalopram. Reach the baseline separation, the separation degree reaches above 1.5, and the separation effect is good.

Embodiment 3

[0079] The second system suitability solution: Accurately weigh 25 mg of citalopram hydrobromide raw material (source: Qionglai Branch of Sichuan Kelun Pharmaceutical Co., Ltd., batch 2), put it in a 20mL volumetric flask, and then precisely measure 2mL The mixed impurity stock solution in Example 1 was dissolved with the diluent in Example 1, fixed to volume, and shaken to obtain the second system suitability solution.

[0080] Except that the column temperature is 28° C., other chromatographic conditions are the same as in Example 1. The second system suitability solution is tested and analyzed, and the test results are shown in Table 5 and image 3 .

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Abstract

The invention belongs to the field of analytical chemistry, and specifically relates to a method for determining related substances in citalopram or salt thereof and a preparation thereof. According to the method, citalopram is detected by using HPLC, wherein the mobile phase A is a phosphate buffer solution with the mass volume ratio of 0.6-0.7% and the pH value of 6.0-7.0; and the mobile phase Bis a mixed solution consisting of methanol and acetonitrile in a volume ratio of (30-50): (70-50). According to the method, at least twelve known impurities in citalopram can be detected, even threeunknown impurities can be detected, the peak shape is good, the separation degree is good, the repeatability is good, and effective separation and quantitative determination of citalopram can be realized.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a method for determining related substances in citalopram or its salts and preparations thereof. Background technique [0002] Citalopram hydrobromide, its chemical name is (±)-1-[3-(dimethylamino)propyl]-1-(4-fluorophenyl)-1,3-dihydro- 5-isobenzofurancarbonitrile hydrobromide, with a structural formula such as formula I, is a serotonin reuptake inhibitor used for conventional treatment of depression and anxiety. [0003] [0004] In 1989, Citalopram Hydrobromide Tablets, an oral 5-HT reuptake inhibitor (SSRI) jointly developed by Lundbeck Pharmaceuticals and FOREST LABS, was approved for marketing in Denmark for the first time, and then in Germany, the UK, the US and other EU countries. . In June 2003, Citalopram Hydrobromide Tablets produced by the Danish Lundbeck Pharmaceutical Factory was approved in China, and the trade name was Xipumi Used to treat depression. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 李明肖子康赖婷婷郭仁平吴灵静王琦王利春王晶翼
Owner SUZHOU KELUN PHARMA RES CO LTD