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High performance liquid chromatography-time-of-flight mass spectrometry method for identifying degradation product in compound cold treatment medicine based on heart-cutting technology

A high-performance liquid chromatography and time-of-flight mass spectrometry technology, applied in the field of analytical chemistry, can solve problems such as interference and pollution, and achieve the effect of improving accuracy and reliability

Active Publication Date: 2017-01-11
SHENZHEN NEPTUNUS PHARMA RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the problem of pollution and interference caused by the use of non-volatile buffer salt system flow relative to impurities when using liquid quality to identify impurities, and relates to a method for identifying degradation products in compound cold medicine based on two-dimensional heart-cutting technology High Performance Liquid Chromatography-Time-of-Flight Mass Spectrometry Method

Method used

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  • High performance liquid chromatography-time-of-flight mass spectrometry method for identifying degradation product in compound cold treatment medicine based on heart-cutting technology
  • High performance liquid chromatography-time-of-flight mass spectrometry method for identifying degradation product in compound cold treatment medicine based on heart-cutting technology
  • High performance liquid chromatography-time-of-flight mass spectrometry method for identifying degradation product in compound cold treatment medicine based on heart-cutting technology

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0077] a. Preparation of ibuprofen oxidation sample: take an appropriate amount of compound cold medicine (approximately equivalent to 200 mg of ibuprofen), add 10 ml of acetonitrile, dissolve it by ultrasonic, filter, add 10 ml of 30% hydrogen peroxide, put in a water bath at 80 ° C for 1 hour, Take it out, let it cool, transfer it to a 100ml measuring bottle, make it to volume, shake it up, filter it, and wait for sample injection.

[0078] b. Preparation of oxidized samples of phenylephrine hydrochloride and chlorpheniramine maleate: take an appropriate amount of compound cold medicine (approximately equivalent to 10 mg of phenylephrine hydrochloride and 4 mg of chlorpheniramine maleate), add 20% acetonitrile -Water solvent 10ml, ultrasonic to dissolve, shake well, add 5ml of 30% hydrogen peroxide, put in 80°C water bath for 30 minutes, take it out, let cool, transfer to 25ml measuring bottle, constant volume, shake well, filter, wait for sample injection .

Embodiment 1

[0079] Example 1 Analysis of chlorpheniramine maleate and phenylephrine hydrochloride forced degradation products, cut as figure 1 When the middle retention time is 12.80 minutes, the instrument configuration and analysis conditions are:

[0080] One-dimensional:

[0081] High performance liquid chromatography: HPLC, Agilent 1260;

[0082] Chromatographic column: Waters spherisorb 5um SCX, 4.6*150mm;

[0083] Mobile phase A: 0.075mol / L disodium hydrogen phosphate (containing 0.1% triethylamine, adjust pH to 2.4 with phosphoric acid);

[0084] Mobile phase B: acetonitrile;

[0085] Linear Gradient:

[0086]

[0087] Detection wavelength: 215nm;

[0088] Flow rate: 1.0ml / min;

[0089] Column temperature: 35°C;

[0090] Injection volume: 20ul;

[0091] The valve switching time is 12.75-12.85min.

[0092]

[0093] Cut 1D chromatograms (eg figure 1 ) when the retention time is a component of 12.80 minutes, the two-dimensional test conditions are as follows:

[0094...

Embodiment 2

[0113] Example 2 Analysis of ibuprofen forced degradation products, cut as figure 2 When the middle component is 13.55 minutes, the instrument configuration and analysis conditions are:

[0114] One-dimensional:

[0115] High performance liquid chromatography: HPLC, Agilent 1260;

[0116] Chromatographic column: Waters BEH C18 3.5um 4.6*150mm;

[0117] Gradient elution conditions:

[0118] Mobile phase A: 0.02mol / L sodium dihydrogen phosphate (adjust the pH to 3.0 with phosphoric acid)-acetonitrile (83.5:16.5);

[0119] Mobile phase B: 0.02mol / L sodium dihydrogen phosphate (adjust the pH to 3.0 with phosphoric acid)-acetonitrile (16.5:83.5);

[0120] Linear Gradient:

[0121]

[0122] Detection wavelength: 214nm;

[0123] Flow rate: 1.4ml / min;

[0124] Column temperature: 35°C;

[0125] Injection volume: 20ul;

[0126] The valve switching time is 13.50-13.60min.

[0127]

[0128] Cut 1D chromatograms (eg figure 2 ), the two-dimensional test conditions are as...

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Abstract

The invention relates to a high performance liquid chromatography-time-of-flight mass spectrometry method for identifying a degradation product in a compound cold treatment medicine based on a heart-cutting technology. The method comprises the following steps: separating a sample by using a mass spectrum incompatible mobile phase in a first-dimensional chromatograph; acquiring ultraviolet data through a one-dimensional detector; determining a target peak, and carrying out heart-cutting to make the target peak exist in a sample loop; carrying out back flushing through valve switching by using a two-dimensional system using a mass spectrum compatible mobile phase to make the target peak exist in the two-dimensional system and enter a two-dimensional ultraviolet and mass spectrum detector in order to complete impurity analysis and identification. The method has the advantages of no change of original separation conditions, high specificity, accuracy and resolution in impurity detection, and improvement of the reliability of nonvolatile buffer salt separation system impurity mass spectrometry and identification.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a method for identifying degradation products in compound cold medicines. Background technique [0002] Impurity research and control is one of the core contents of drug quality control. Adverse reactions in the clinical use of drugs are often related to impurities in the product. Therefore, impurity research and control are key elements of drug safety assurance and are also risk control in drug research and development. An important manifestation of consciousness. Through the forced degradation experiment of the drug, the structure of the degradation product is analyzed by liquid mass technology, the structure of the impurity is speculated, and the possible source is analyzed, which provides an important reference for the impurity control and process optimization of the drug. [0003] At present, liquid chromatography-mass spectrometry (LC / MS) has become the pref...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 石涛胥娜刘小柔朱丹王菲
Owner SHENZHEN NEPTUNUS PHARMA RES INST CO LTD
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