Separation and determination method for 9-demethylation-alpha-dihydrotetrabenazine and impurities thereof

A technology of dihydrotetrabenazine and determination method, applied in the direction of material separation, measuring device, analysis material, etc., to achieve the effect of ensuring purity and labeling rate, benefiting effectiveness and safety, and sensitive detection method

Active Publication Date: 2017-05-31
JIANGSU INST OF NUCLEAR MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The first technical problem to be solved in the present invention is that the prior art cannot realize the 9-DM-α-DTBZ and its main impurities α-DTBZ and N in the 9-desmethyl-α-dihydrotetrabenazine bulk drug -The problem of complete separation of methylaniline, the second technical problem to be solved in the present invention is that prior art cannot realize 9-DM-α-DTBZ in 9-desmethyl-α-dihydrotetrabenazine crude drug The problem of simultaneous determination of the content of its main impurities α-DTBZ and N-methylaniline

Method used

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  • Separation and determination method for 9-demethylation-alpha-dihydrotetrabenazine and impurities thereof
  • Separation and determination method for 9-demethylation-alpha-dihydrotetrabenazine and impurities thereof
  • Separation and determination method for 9-demethylation-alpha-dihydrotetrabenazine and impurities thereof

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Embodiment 1

[0061] The separation and determination method of present embodiment 9-demethyl-alpha-dihydrotetrabenazine and impurities thereof comprises the following steps:

[0062] Weigh an appropriate amount of 9-desmethyl-α-dihydrotetrabenazine bulk drug to be tested, add ammonium acetate buffer solution (concentration is 50mM, pH value is 4.5)-methanol with a volume ratio of 70:30 to dissolve, and prepare Become the solution that concentration is 1mg / mL, as need testing solution;

[0063] Take an appropriate amount of reference substance of 9-desmethyl-α-dihydrotetrabenazine to make a solution with a concentration of 1 mg / mL as 9-desmethyl-α-dihydrotetrabenazine reference substance solution;

[0064] Take an appropriate amount of reference substance of α-dihydrotetrabenazine to make a solution with a concentration of 1 mg / mL as the α-dihydrotetrabenazine reference substance solution;

[0065] Take an appropriate amount of reference substance of N-methylaniline to make a solution with...

Embodiment 2

[0071] The separation and determination method of present embodiment 9-demethyl-alpha-dihydrotetrabenazine and impurities thereof comprises the following steps:

[0072] Weigh an appropriate amount of 9-desmethyl-α-dihydrotetrabenazine bulk drug to be tested, add ammonium acetate buffer solution (concentration is 50mM, pH value is 4.5)-methanol that the volume ratio is 50:50 and dissolve, prepare A solution with a concentration of 1.0 mg / mL was used as the test solution;

[0073] Take an appropriate amount of reference substance of 9-desmethyl-α-dihydrotetrabenazine to make a solution with a concentration of 1 mg / mL as 9-desmethyl-α-dihydrotetrabenazine reference substance solution;

[0074] Take an appropriate amount of reference substance of α-dihydrotetrabenazine to make a solution with a concentration of 1 mg / mL as the α-dihydrotetrabenazine reference substance solution;

[0075] Take an appropriate amount of reference substance of N-methylaniline to make a solution with ...

Embodiment 3

[0081] The separation and determination method of present embodiment 9-demethyl-alpha-dihydrotetrabenazine and impurities thereof comprises the following steps:

[0082] Weigh an appropriate amount of 9-desmethyl-α-dihydrotetrabenazine bulk drug to be tested, add ammonium acetate buffer solution (concentration is 50mM, pH value is 4.5)-methanol with a volume ratio of 75:25 to dissolve, and prepare Become the solution that concentration is 1mg / mL, as need testing solution;

[0083] Take an appropriate amount of reference substance of 9-desmethyl-α-dihydrotetrabenazine to make a solution with a concentration of 1 mg / mL as 9-desmethyl-α-dihydrotetrabenazine reference substance solution;

[0084] Take an appropriate amount of reference substance of α-dihydrotetrabenazine to make a solution with a concentration of 1 mg / mL as the α-dihydrotetrabenazine reference substance solution;

[0085] Take an appropriate amount of reference substance of N-methylaniline to make a solution with...

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Abstract

The invention belongs to the field of pharmaceutical analysis and in particular relates to a separation and determination method for 9-demethylation-alpha-dihydrotetrabenazine and impurities thereof. The separation and determination method provided by the invention has the advantages that complete separation of 9-DM-alpha-DTBZ and impurities thereof, namely alpha-DTBZ and N-methyl phenylamine, can be realized, contents of the 9-DM-alpha-DTBZ and the impurities thereof, namely alpha-DTBZ and N-methyl phenylamine, can be determined at the same time, and a simple, quick and sensitive detection method is provided for determination of content of 9-demethylation-alpha-dihydrotetrabenazine in 9-demethylation-alpha-dihydrotetrabenazine raw materials and the determination of the content of related substances, so that quality control on the 9-DM-alpha-DTBZ raw materials can be realized, and further the purity and labeling efficiency of a PET imaging drug 11C-alpha-DTBZ are guaranteed, and effective and safe application of the PET imaging drug 11C-alpha-DTBZ are facilitated.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for separating and measuring 9-desmethyl-α-dihydrotetrabenazine and impurities thereof. Background technique [0002] Vesicular monoamine transporter type II (VMAT2) is a membrane protein located on the membrane of intracytoplasmic vesicles in neurons and plays a key role in the reuptake of monoamine transmitters. Molecular cloning technology identification shows that VMAT2 is mainly distributed in the central nervous system and pancreatic tissue of humans and mammals. Changes in VMAT2 are associated with various diseases, such as Parkinson's disease (PD), Alzheimer's disease (AD), Huntington's disease (HD), diabetes, etc. In recent years, using VMAT2 as a target to conduct radioactive tracer imaging for early diagnosis, grading, differential diagnosis, and curative effect monitoring of related diseases has become one of the hot spots in nuclear medicine research. So far, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 刘春仪陈正平李晓敏唐婕曹丽华薛丹露
Owner JIANGSU INST OF NUCLEAR MEDICINE
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