Method for separating enantiomers of rotigotine and trihexyphenidyl

An enantiomer, trihexyphenidyl technology, applied in the field of capillary electrophoresis chiral separation, achieves the effects of less sample consumption, low ultraviolet absorption background, and high separation efficiency

Inactive Publication Date: 2009-09-30
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] At present, using sulfonated dextran as a chiral selector, a capillary electrophoresis method for simultaneous chiral separation of two anti-Parkinson drugs, rotigotine and trihexyphenidyl, has not been reported.

Method used

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  • Method for separating enantiomers of rotigotine and trihexyphenidyl
  • Method for separating enantiomers of rotigotine and trihexyphenidyl
  • Method for separating enantiomers of rotigotine and trihexyphenidyl

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] 1. Prepare running buffer and samples

[0053] Using ultrapure water as a solvent, prepare an aqueous solution of sodium dihydrogen phosphate with a concentration of 10 mmol / L as the background electrolyte. Slowly add phosphoric acid with a concentration of 1 mol / L dropwise into the prepared sodium dihydrogen phosphate aqueous solution to adjust the pH value of the buffer solution to 4. Sulfonated dextran with a molecular weight of 1,000,000 was added to the above buffer solution at a ratio of 2.0% (w / v), dissolved, filtered through a 0.22 μm filter membrane, and ultrasonicated for 5 minutes. Dissolve rotigotine and trihexyphenidyl in ultrapure water to obtain stock samples with a concentration of 10 mmol / L, and store them at 4°C. During sample injection, the stock sample was diluted with running buffer to obtain the sample to be separated with a concentration of 0.1 mmol / L.

[0054] 2. Instrument Preparation

[0055] The separation process was carried out in an unco...

Embodiment 2

[0063] 1. Prepare running buffer and samples.

[0064] Using ultrapure water as a solvent, prepare an aqueous solution of sodium dihydrogen phosphate with a concentration of 10 mmol / L as the background electrolyte. Slowly add phosphoric acid with a concentration of 1 mol / L dropwise into the prepared sodium dihydrogen phosphate aqueous solution to adjust the pH value of the buffer solution to 2.5. Sulfonated dextran with a molecular weight of 1,000,000 was added to the above buffer solution at a ratio of 2.0% (w / v), dissolved, filtered through a 0.22 μm filter membrane, and ultrasonicated for 5 minutes. Dissolve rotigotine and trihexyphenidyl in ultrapure water to obtain stock samples with a concentration of 10 mmol / L, and store them at 4°C. During sample injection, the stock sample was diluted with running buffer to obtain the sample to be separated with a concentration of 0.1 mmol / L.

[0065] 2. Instrument Preparation

[0066] The separation process was carried out in an u...

Embodiment 3

[0074] 1. Prepare running buffer and samples.

[0075] Using ultrapure water as a solvent, prepare an aqueous solution of sodium dihydrogen phosphate with a concentration of 10 mmol / L as the background electrolyte. Slowly add phosphoric acid with a concentration of 1 mol / L dropwise into the prepared sodium dihydrogen phosphate aqueous solution to adjust the pH value of the buffer solution to 2.5. Sulfonated dextran with a molecular weight of 500,000 was added to the above buffer solution at a ratio of 2.0% (w / v), dissolved and then filtered through a 0.22 μm filter membrane and ultrasonicated for 5 minutes. Dissolve rotigotine and trihexyphenidyl in ultrapure water to obtain stock samples with a concentration of 10 mmol / L, and store them at 4°C. During sample injection, the stock sample was diluted with running buffer to obtain the sample to be separated with a concentration of 0.1 mmol / L.

[0076] 2. Instrument Preparation

[0077] The separation process was carried out in...

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Abstract

The invention provides a method for separating enantiomers of rotigotine and trihexyphenidyl. The method comprises the steps of dissolving dextran sulfate in a buffer solution, obtaining an operational buffer solution containing the dextran sulfate as a chiral selector, dissolving rotigotine to be separated and trihexyphenidyl as samples to be separated in the operational buffer solution and separating enantiomers of two medicaments through a capillary electrophoresis instrument. The method is characterized in that the adopted chiral selector is the dextran sulfate of which the molecular weight is 500,000 or 1,000,000, and is low in background ultraviolet absorption, cheap and readily available. The adopted method has the advantages of high separation efficiency, low reagent consumption, environment-friendly property, convenient operation, capability of realizing the chiral separation of the enantiomers in a forward or backward voltage mode, as well as opposite transfer order of the enantiomers in two modes. The method is high in the degree of separating the enantiomers of the two medicaments.

Description

technical field [0001] The invention belongs to the field of chromatographic technology, drug analysis and enantiomer separation, and further, the invention belongs to the field of chiral separation analysis for anti-Parkinson drug molecules. Specifically, the present invention relates to a capillary electrophoresis chiral separation method for Rotigotine and Trihexyphenidyl. The method can be used for chiral separation of rotigotine and trihexyphenidyl in forward and reverse voltage modes, respectively. Background technique [0002] Each enantiomer of a chiral compound has the same physical and chemical properties in an isotropic environment, but shows different properties in an anisotropic biological system. The entire life system (including proteins, nucleic acids, carbohydrates, hormones, enzymes, biological receptors, etc.) in organisms is almost all chiral, so chiral drugs entering the organism must have enantioselective effects on them , resulting in different pharm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D333/20C07D295/092C07B57/00G01N27/447
Inventor 王志华楚宝临林金明
Owner BEIJING UNIV OF CHEM TECH
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