Separation method of blonanserin intermediate IV and other intermediates by high performance liquid chromatography

A technology of blonanserin and high-efficiency liquid phase, applied in the direction of material separation, analysis materials, measuring devices, etc., can solve problems such as the inability to achieve effective separation of blonanserin intermediate IV, and achieve the effect of improving symmetry

Inactive Publication Date: 2012-12-12
江苏万全特创医药生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The purpose of the present invention is to overcome the shortcomings that current isocratic elution cannot realize the effective separation of blonanserin intermediate IV from other intermediates, and provide a metho

Method used

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  • Separation method of blonanserin intermediate IV and other intermediates by high performance liquid chromatography
  • Separation method of blonanserin intermediate IV and other intermediates by high performance liquid chromatography
  • Separation method of blonanserin intermediate IV and other intermediates by high performance liquid chromatography

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Experimental program
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Effect test

Embodiment 1

[0034] Shimadzu LC-20AT high performance liquid chromatograph, Welch Materials brand octane silane bond and silica gel are used as the chromatographic column as the packing agent.

[0035] A high-efficiency liquid-phase separation method of blonanserin intermediate IV and other intermediates, comprising the following steps:

[0036] (1) Take 8 mg of blonanserin intermediate IV and intermediates I, II, and III respectively, put them in a 10 mL volumetric flask, add methanol to dissolve and dilute to the mark, shake well, and use it as the test solution;

[0037] (2) Set the mobile phase of the liquid chromatograph, that is, the A pump is an organic modifier, the B pump is a buffer solution, and the gradient elution procedure of the liquid chromatograph is set as follows:

[0038] Gradient 1: Time (min) A pump mobile phase (%) B pump mobile phase (%)

[0039] 10 45 55

[0040] 20 80 20

[0041] 30 80 20

[0042] 40 45 55

[0043] ...

Embodiment 2

[0048] The new Shimadzu LC-20AT high performance liquid chromatograph, Welch Materials brand octane silane bond and silica gel are used as the packing agent.

[0049] A high-efficiency liquid-phase separation method of blonanserin intermediate IV and other intermediates, comprising the following steps:

[0050] (1) Take 10 mg of blonanserin intermediate IV, put it in a 10 mL volumetric flask, add methanol to dissolve and dilute to the mark, shake well, and use it as the test solution;

[0051] (2) Set the mobile phase of the liquid chromatograph, that is, the A pump is an organic modifier, the B pump is a buffer solution, and the gradient elution procedure of the liquid chromatograph is set as follows:

[0052] Gradient 2: Time (min) A pump mobile phase (%) B pump mobile phase (%)

[0053] 10 20 80

[0054] 30 100 0

[0055] 35 100 0

[0056] 45 20 80

[0057] 50 20 80

[0058] (3) Set the mobile phase flow rate of the liquid chrom...

Embodiment 3

[0063] Shimadzu LC-20AT new model high performance liquid chromatograph, Welch Materials brand octane silane bond and silica gel are used as chromatographic columns. The specifications of the chromatographic column are 250mm in length, 4.6mm in inner diameter, and 5μm in particle size.

[0064] A high-efficiency liquid phase separation method for blonanserin intermediate IV and other intermediates, comprising the following steps:

[0065] (1) Take 5 mg of blonanserin intermediate IV and intermediates I, II, III, and IV respectively, put them in a 10mL volumetric flask, add methanol to dissolve and dilute to the mark, shake well, and use it as the test solution;

[0066] (2) The mobile phase of the liquid chromatograph is set, that is, the A pump is an organic modifier, and the B pump is a buffer solution, and the gradient elution program of the liquid chromatograph is set as follows:

[0067] Gradient 3: Time (min) A pump mobile phase (%) B pump mobile phase (%)

[0068] ...

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Abstract

The invention discloses a separation method of a blonanserin intermediate IV and other intermediates by high performance liquid chromatography. The separation method selects octylsilane chemically bonded and silica as a chromatographic column of a filling agent (250mm multiplied by 4.6mm, 5mum), adopts a buffer solution and an organic modifier with different proportions as flowing phase, and the blonanserin intermediate IV and other intermediates which has the similar polarity with the blonanserin intermediate IV can be separated under the normal temperature by gradient elution, so that the accurate control of the quality of blonanserin can be realized.

Description

technical field [0001] The invention relates to a high-performance liquid chromatography separation method, in particular to a high-performance liquid chromatography method for effectively separating blonanserin intermediate IV from other intermediates by adopting a gradient elution method. Background technique [0002] Blonanserin is an atypical antipsychotic with fewer side effects than other antipsychotics. Molecular formula of blonanserin intermediate IV: C 17 h 17 FClN, the chemical name is 2-chloro-4-(4-fluorophenyl)-5,6,7,8,910-hexahydrocyclooctano[b]pyridine, and the structural formulas of intermediates I, II, III and IV are as follows : [0003] [0004] Intermediate Ⅰ [0005] [0006] Intermediate Ⅱ [0007] [0008] Intermediate III [0009] [0010] Intermediate IV [0011] In order to effectively separate blonanserin intermediate IV from other intermediates and accurately control the quality of blonanserin intermediates, the current high-effi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 王爱霞翟富民李艳丽
Owner 江苏万全特创医药生物技术有限公司
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