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Method for determining 2beta-methyl-3beta-(4-chlorphenyl) tropine and related substances thereof

A technology of related substances and chlorophenyl, which is applied in the field of content analysis of 2β-carbomethoxy-3β-tropane and related substances, and can solve the problem of inability to detect the quality of β-CCT, inability to detect β-CCT and related substances. Separation and other problems, to achieve the effect of good accuracy, high sensitivity and good separation

Active Publication Date: 2022-05-13
JIANGSU INST OF NUCLEAR MEDICINE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Therefore, the present invention solves the defect that the existing analytical method cannot separate β-CCT and its related substances, and cannot detect the quality of β-CCT, thereby providing a method for simultaneously determining 2β-carbocarboxylate-3β-(4-chlorobenzene base) methods for tropanes and related substances

Method used

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  • Method for determining 2beta-methyl-3beta-(4-chlorphenyl) tropine and related substances thereof
  • Method for determining 2beta-methyl-3beta-(4-chlorphenyl) tropine and related substances thereof
  • Method for determining 2beta-methyl-3beta-(4-chlorphenyl) tropine and related substances thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] β-CXCT, β-CCT, and α-CCT were used to make methanol mixed solution, and the concentrations of β-CXCT, β-CCT, and α-CCT in the mixed solution were 42 μg / mL, 336 μg / mL, and 66 μg / mL, respectively.

[0057] The mixed solution was separated on a high-performance liquid chromatograph, and the chromatographic column was a C18 column (4.6mm×150 mm, 5 μm, ), the mobile phase was a mixed solution of methanol-water-trifluoroacetic acid in different proportions, the flow rate was 1.0mL / min, the detection wavelength was 220nm, and the column temperature was set at 30°C.

[0058] (1) The ratio of mobile phase methanol-water-trifluoroacetic acid is 25:75:0.1 (v / v / v). Such as figure 2 As shown, the retention times of β-CXCT, β-CCT, and α-CCT are 5.9, 11.3, and 18.4 minutes respectively, and the three can achieve baseline separation, but the peak shape of β-CXCT is relatively broad. The separation degrees of β-CCT, β-CXCT and α-CCT were 4.1 and 8.3, respectively.

[0059] (2) When...

Embodiment 2

[0062] Embodiment 2 specificity verification

[0063] In order to investigate the specificity of the method of the present invention for β-CCT analysis, that is, to verify that the method provided by the present invention can analyze the impurities that may exist in the sample, the research method (i.e. the international human drug registration technology) Coordination Committee (ICH) recommended method), the degradation test of pure β-CCT under different conditions was carried out, and the samples were processed under the conditions of acid, alkali, oxidation, heating and light respectively. The samples after the test were then analyzed by high performance liquid chromatography.

[0064] The high-performance liquid chromatography analysis conditions are: the chromatographic column is a C18 column (4.6mm×150mm, 5 μm, ), the mobile phase was methanol-water-trifluoroacetic acid (30:70:0.1, v / v / v), the flow rate was 1.0mL / min, the UV detection wavelength was 220nm, and the colu...

Embodiment 3

[0073] Embodiment 3 lowest limit of quantitation

[0074] The lower limit of quantification refers to the concentration of the sample at which the signal number of the chromatographic peak is 10 times that of the noise. First prepare methanol standard solutions of 1.0mg / mL β-CCT, β-CXCT and α-CCT respectively, then dilute them into sample solutions with different concentrations, and inject them into HPLC for analysis. The chromatographic column is a C18 column (4.6mm×150mm, 5 μm, ), the ratio of methanol-water-trifluoroacetic acid is 30:70:0.1 (v / v / v) as the mobile phase, the flow rate is 1.0 ml / mL, and the chromatogram is recorded until the peak height of the sample is 10 times of the noise. The concentration is the lower limit of quantitation. Results The lower limits of quantitation in β-CCT, β-CXCT and α-CCT were 1.5μg / mL, 1.2μg / mL and 1.5μg / mL, respectively. Concentrations above the minimum quantification limit can be accurately measured, and the minimum quantification...

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Abstract

The invention provides a method for simultaneously determining 2beta-methyl-3beta-(4-chlorphenyl) tropane and related substances thereof, belongs to the field of pharmaceutical analysis, and overcomes the defects that beta-CCT and related substances thereof cannot be separated and the quality of beta-CCT cannot be detected in the conventional analysis method. According to the method for simultaneously determining the 2beta-methyl-3beta-(4-chlorphenyl) tropane and the related substances thereof, high performance liquid chromatography is adopted, a used chromatographic column is a C18 reversed-phase column, a mobile phase comprises methanol, water and an acidic additive, and the volume ratio of the methanol to the water to the acidic additive is (25-40): (60-75): (0.05-1.5); the detection method is ultraviolet detection; the related substances are 2 [alpha]-methyl ester-3 [beta]-(4-chlorphenyl) tropine alkane and 2 [beta]-carboxyl-3 [beta]-(4-chlorphenyl) tropine alkane. According to the method disclosed by the invention, the beta-CXCT, the beta-CCT and the alpha-CCT can be subjected to baseline separation under the same HPLC (High Performance Liquid Chromatography) condition.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a method for simultaneously measuring 2β-carbomethoxy-3β-(4-chlorophenyl)tropane and its related substances and 2β-carbomethoxy-3β-(4-chlorophenyl) Content analysis method of phenyl)tropane and its related substances. Background technique [0002] The dopamine transporter (DAT for short) of the central nervous system is a transmembrane protein located on the presynaptic membrane of dopamine neurons in the brain, and plays a key role in the regulation of neurotransmitters in the brain (German CL, et al. Pharmacol. Rev. 2015, 67: 1005-1024; Ciliax B, et al. J. Neurosci. 1995, 15: 1714-1723). Studies have shown that the pathological changes of various neurological diseases are related to changes in DAT, such as Parkinson's disease, drug addiction, ADHD, depression, dementia, anxiety, etc. (Palermo G, etal. Cells 2019, 8:872; Zhu L, et al. Chem. Soc. Rev. 2014, 43: 6683-6691). In rece...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/34G01N30/74
CPCG01N30/02G01N30/34G01N30/74
Inventor 陈正平黄彩云谢敏浩刘春仪唐婕方毅李庆明胡潜岳季林阳
Owner JIANGSU INST OF NUCLEAR MEDICINE
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