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The detection method of starting material a in the raw material 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, which can solve the problem that the detection sensitivity fails to meet the requirements and affects the safety of the use of the landiolol hydrochloride drug. , detection interference and other problems, to achieve the effect of short detection time, guaranteed use safety, and low-cost detection

Active Publication Date: 2017-10-10
SHANDONG ANALYSIS & TEST CENT
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  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • The detection method of starting material a in the raw material drug of landiolol hydrochloride
  • The detection method of starting material a in the raw material drug of landiolol hydrochloride
  • The detection method of starting material a in the raw material drug of landiolol hydrochloride

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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 method for detecting starting material A in landiolol hydrochloride raw material drug, which comprises: a step of pre-treating landiolol hydrochloride raw material drug, and pre-treated landiolol hydrochloride raw material The drug is detected by liquid chromatography-tandem mass spectrometry, and the internal standard method is used to quantitatively analyze the starting material A in the landiprolol hydrochloride raw material drug. The detection sensitivity of the method of the invention can reach 0.50 mg / kg, and the precision and recovery rate of the method can both meet the detection requirements of (S)-(+)-m-nitrobenzene sulfonic acid glycidyl ester. The invention has the advantages of simple operation and reliable results, and can realize rapid and low-cost detection of trace (S)-(+)-m-nitrobenzenesulfonate glycidyl ester in the raw material drug of landipolol 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 Patents(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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