A method for detecting phenylethyl methanesulfonate substances

A technology for phenethyl methanesulfonate and substances, which is applied in the field of detection of phenethyl methanesulfonate substances, can solve problems such as difficult to avoid solvent effects, and achieve the effects of eliminating solvent effects, high degree of separation, and easy control.

Active Publication Date: 2021-02-12
SHANGHAI SCIENPHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method applies to (R)-2-(amino-2-phenylethylmethanesulfonic acid In the detection of esters), it is difficult to avoid the influence of the solvent effect on the peak shape of the analyte

Method used

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  • A method for detecting phenylethyl methanesulfonate substances
  • A method for detecting phenylethyl methanesulfonate substances
  • A method for detecting phenylethyl methanesulfonate substances

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Embodiment 1

[0055] Embodiment 1, the present invention detects the high-performance liquid chromatography method of phenylethyl methanesulfonate substance impurity

[0056] Chromatographic column: Inertsil ph-3, 4.6mm×250mm, 5μm;

[0057] Mobile phase I: 20mmo / L potassium dihydrogen phosphate (adjust pH to 3.0 with phosphoric acid)-acetonitrile (95:5)

[0058] Mobile Phase II: Acetonitrile-Methanol (90:10)

[0059] Solvent I: The solvent for preparing the test solution is methanol-water (50:50).

[0060] Solvent II: The solvent for preparing the reference solution is methanol-water-phosphoric acid (50:50:0.05);

[0061]Column temperature: 25°C; flow rate: 1.0ml / min; UV detector (detection wavelength: 210nm).

[0062] Injection volume: 10 μL. The injector temperature was 5°C.

[0063] Gradient elution conditions are as follows in Table 1:

[0064] Table 1

[0065] time (min) A％ B％ 0 95 5 5 95 5 20 30 70 21 95 5 30 95 5

[0066] Detect...

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Abstract

The invention discloses a method for detecting phenylethyl methanesulfonate substances; it comprises the following steps: a. preparing a reference substance solution; b. preparing a test solution; c. using high performance liquid chromatography to compare the reference substance respectively solution and the test solution are detected; d, the impurity content in the sample is obtained by calculating the peak area according to the external standard method. The invention provides a new detection method for detecting phenylethyl methanesulfonate substances, the separation degree between each chromatographic peak is high, there is no interference between each other, and the accurate detection of the impurity B in the substance A to be tested can be realized at the same time, An effective detection method is provided for monitoring the content of phenylethyl methanesulfonate.

Description

technical field [0001] The invention belongs to the field of analysis and detection in chemistry, and in particular relates to a method for detecting phenethyl methanesulfonate substances. Background technique [0002] The compound whose structure is (R)-2-((tert-butoxycarbonylamino)-2-phenethyl methanesulfonate) is known to be structurally unstable according to its chemical properties, and is easily degraded to produce a structure of (R)-2-( Amino-2-phenylethyl methanesulfonate), (R)-2-(amino-2-phenylethyl methanesulfonate) is weakly retained in the detection method and is prone to solvent effects, resulting in peak splitting , Influence accurate detection, thereby influence the product quality of (R)-2-((tert-butoxycarbonylamino)-2-phenylethyl methanesulfonate) compound. [0003] In order to detect the compound (R)-2-(amino-2-phenylethyl methanesulfonate), at the same time, in order to more comprehensively monitor the compound (R)-2-((tert-butoxycarbonylamino)-2 -pheneth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/60G01N30/30G01N30/34G01N30/16
CPCG01N30/02G01N30/06G01N30/16G01N30/30G01N30/34G01N30/6052G01N2030/047
Inventor 李惠姜春阳谢军马迪周小群
Owner SHANGHAI SCIENPHARM CO LTD
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