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Method for detecting Raltitrexed enantiomer by capillary tube electrophoresis

An enantiomeric and capillary electrophoresis technology, applied in measuring devices, material analysis by electromagnetic means, instruments, etc., can solve the problems of easy decline in column efficiency, increased difficulty in separation, and poor separation effect, etc. The effect of low cost, environmental friendliness and broad application prospects

Active Publication Date: 2012-01-04
YANGTZE RIVER PHARM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The commonly used method for checking the enantiomers of chiral drugs is chiral high performance liquid chromatography, by adding a chiral selector to the mobile phase or using a chiral chromatographic column for separation and inspection. The former often has a poor separation effect and the exclusive The latter chromatographic column is more expensive, the cost is higher, and the column efficiency is very easy to drop during use, resulting in poor separation effect. In addition, the structure of raltitrexed and its isomers contains both carboxyl and Containing amino groups, it is easy to twist in the molecule during liquid chromatography analysis, which increases the difficulty of separation; gas chromatography is used for the inspection of chiral drug enantiomers, requiring samples to have certain volatility and thermal stability. Application Very limited

Method used

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  • Method for detecting Raltitrexed enantiomer by capillary tube electrophoresis
  • Method for detecting Raltitrexed enantiomer by capillary tube electrophoresis
  • Method for detecting Raltitrexed enantiomer by capillary tube electrophoresis

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] The experiment was carried out on an Agilent 3D CE capillary electrophoresis instrument from Agilent Technologies, USA, with hydrodynamic sample injection, a fused silica capillary column with an effective capillary length of 40 cm and an inner diameter of 50 μm. The sample preparation process is as follows:

[0010] Prepare a 75mmol / L tris (Tris) solution, adjust the pH to 8.0 with 0.1M phosphoric acid as a buffer, add 8mmol / L carboxymethyl-β-cyclodextrin (CM-β-CD ) and 30mmol / L sodium lauryl sulfate. Use methanol:water=1:1 (volume ratio) solution to prepare raltitrexed (s-raltitrexed) solution and raltitrexed and its enantiomer (r-and s-raltitrexed) mixed solution, raltitrexed The concentration of trexet was 50 μg / ml. Rinse with buffer solution for 3 min before sample injection. Experimental temperature: 25°C, detection wavelength: 228nm, hydrodynamic injection at 50mbar for 5 seconds; see results figure 1 .

Embodiment 2

[0012] Electrophoresis conditions were the same as in Example 1. Prepare with methanol:water=1:1 (volume ratio) solution, respectively prepare a series of raltitrexed (s-raltitrexed) and raltitrexed enantiomer (r-raltitrexed) solutions, inject samples, and record the response value The electropherogram which is 3 times of the baseline noise is the detection limit of raltitrexed and its enantiomer, and the detection limit is 1 μm / ml. see results figure 2

Embodiment 3

[0014] Use 50mmol / L~200mol / L Tris-phosphoric acid solution as a buffer, adjust the pH to 8.0 with 0.1M phosphoric acid, add 8mmol / L carboxymethyl-β-cyclodextrin (CM-β-CD) and The sodium lauryl sulfate of 30mmol / L; Others are with embodiment 1, the results see image 3 .

[0015] 1. A method for checking enantiomers of chiral drug raltitrexed.

[0016] 2. The method is high performance capillary electrophoresis

[0017] The invention is used for checking the single enantiomer of raltitrexed, the method is simple, the separation efficiency is high, the separation speed is fast, the injection volume is small, and the analysis cost is low. Generally, only some commonly used reagents are needed, and the amount of all reagents is less, and the analysis cost is much lower than that of high-performance liquid phase methods. Its beneficial effects are mainly manifested in:

[0018] (1) Less sample consumption: only a few nL of samples are required for each injection;

[0019] (2) ...

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Abstract

The invention relates to a method for detecting a raltitrexed enantiomer by adopting a capillary electrophoresis method which calculates the limitation of the raltitrexed to the enantiomer in the raltitrexed according to a self-contrast method of main components by separating the raltitrexed and the enantiomer through the capillary electrophoresis; uses a solution with the volume ratio of 1 to 1 between methanol and water for preparing a sample solution; an electrophoresis buffer liquid of the capillary electrophoresis is Tris-H3PO4 with a pH value between 6.0 to 10; adds a chiral selection agent and sodium dodecyl sulfate into the buffer liquid. The method overcomes the defects that the use of a chiral flowing phase and a chiral column for separating the enantiomer is difficult and has higher cost because the molecule structures of the raltitrexed not only comprises carboxyl, but also comprises amidogen. The method has the advantages of good separating effect, no pollution, low cost and being suitable for checking the raltitrexed enantiomer.

Description

technical field [0001] The invention relates to a method for detecting raltitrexed enantiomers by capillary electrophoresis. Background technique [0002] The commonly used method for checking the enantiomers of chiral drugs is chiral high performance liquid chromatography, by adding a chiral selector to the mobile phase or using a chiral chromatographic column for separation and inspection. The former often has a poor separation effect and the exclusive The latter chromatographic column is more expensive, the cost is higher, and the column efficiency is easily reduced during use, resulting in poor separation effect. In addition, the structure of raltitrexed and its isomers contains both carboxyl and Containing amino groups, it is easy to twist in the molecule during liquid chromatography analysis, which increases the difficulty of separation; gas chromatography is used for the inspection of chiral drug enantiomers, requiring samples to have certain volatility and thermal st...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/447
Inventor 孙海胜陆小平刘虎威马超刘一付晓芳钟加胜陈娟朱玲玲
Owner YANGTZE RIVER PHARM GRP CO LTD
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