Detection method for starting material A in bulk drug of landiolol hydrochloride

A technology of landiolol hydrochloride and a detection method is applied in the field of detection of starting material A in the raw material medicine of landiolol hydrochloride, and can solve the problems affecting the use safety, detection interference and detection sensitivity of landiolol hydrochloride drug. Less than requirements and other problems, to achieve the effect of short detection time, low-cost detection, and ensure the safety of use

Active Publication Date: 2016-12-21
SHANDONG ANALYSIS & TEST CENT
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0004] (S)-(+)-glycidyl m-nitrobenzenesulfonate (starting material A) is an essential raw material for the synthesis of landipolol hydrochloride, but even if it exists in a trace amount in the drug raw material, it will also affect the hydrochloric acid. The safety of Landyrolol drug use
If the conventional liquid chromatography method is used for detection, not only the detection sensitivity cannot meet the requirements, but also the main component landisolol hydrochloride has relatively large interference to its detection

Method used

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  • Detection method for starting material A in bulk drug of landiolol hydrochloride
  • Detection method for starting material A in bulk drug of landiolol hydrochloride
  • Detection method for starting material A in bulk drug of landiolol hydrochloride

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Embodiment 1: the detection of starting material A in landipolol hydrochloride crude drug

[0035] Specific steps are as follows:

[0036] (1) Pretreatment of samples

[0037] Accurately weigh about 20.0 mg of landisolol hydrochloride raw material, put it in a 10 mL volumetric flask, add the dilution solvent to the scale, shake well, and ultrasonically for 10 minutes, transfer 1.0 mL to a centrifuge tube and centrifuge at 12,000 r / min for 10 minutes. Inject 5 μL of the supernatant for detection.

[0038] (2) Liquid chromatography-tandem mass spectrometry detection

[0039] High-performance liquid chromatography / mass spectrometer was used for detection, and the content of starting material A in the landiprolol hydrochloride raw material drug was calculated by the internal standard method.

[0040] The parameter conditions of the liquid chromatograph are:

[0041] XDB-C18 chromatographic column, column temperature: 30°C, injection volume 5 μL, flow rate 0.4mL / min, mob...

Embodiment 2

[0059] Embodiment 2: the methodological investigation of detection method of the present invention

[0060] 1. Exclusiveness

[0061] (1) Preparation of raw material blank sample of landyrolol hydrochloride (2.0mg / mL): Accurately weigh 20.0mg of blank landyrolol hydrochloride sample, put it in a 10mL measuring bottle, add diluting solvent to the mark, shake well and then sonicate 10 minutes, as a blank sample solution. Pipette 1.0mL into a centrifuge tube, centrifuge at 12000r / min for 10 minutes, take the supernatant and inject 5.0μL, and detect according to the detection conditions of liquid chromatography / tandem mass spectrometry in Example 1. The mass spectrogram is as follows: figure 2 shown.

[0062] (2) Preparation of the sample solution of Landisolol hydrochloride API spiked (starting material A): Accurately weigh 20.0 mg of Landisolol hydrochloride sample, place it in a 10 mL measuring bottle, and accurately add the concentration to be 2.0 mg / mL (S)-(+)-glycidyl m-...

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Abstract

The invention discloses a detection method for a starting material A in the bulk drug of landiolol hydrochloride. The detection method comprises the following steps: pretreatment of the bulk drug of landiolol hydrochloride; liquid chromatographic-mass spectrometric detection of the pretreated bulk drug of landiolol hydrochloride; and quantitative analysis of the starting material A in the bulk drug of landiolol hydrochloride by using an internal standard method. The method has detection sensitivity of 0.50 mg/kg, and the precision and recovery rate of the method meets detection requirements on (S)-(+)-glycidyl nosylate. The method is simple to operate and reliable in results and can realize rapid and low-cost detection of trace (S)-(+)-glycidyl nosylate in the bulk drug of landiolol hydrochloride.

Description

technical field [0001] The invention relates to a method for detecting starting material A in landillol hydrochloride raw material medicine, in particular to a method for detecting starting material A in landivolol hydrochloride raw material medicine by liquid chromatography-tandem mass spectrometry. Background technique [0002] Landisolol hydrochloride is a selective β1 receptor blocker, which mainly antagonizes the β1 receptors present in the heart, and improves tachycardia and arrhythmias by inhibiting the increase in heartbeat caused by catecholamines. At present, the drug is still in the research stage in China, and the process transformation is mainly aimed at foreign expired patents in order to achieve the purpose of reducing the cost of drug use. According to the synthetic route of the landiprolol hydrochloride provided by the cooperative enterprise, (S)-(+)-glycidyl m-nitrobenzenesulfonate (starting material A), its structural formula is as follows: [0003] ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 王珊珊宁凡盛赵汝松苑金鹏王晓利陈相峰陈跃赵金
Owner SHANDONG ANALYSIS & TEST CENT
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