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Analysis method of mercapto amine tropine content

A thioamine tropine and analysis method technology, applied in the field of instrument analysis, can solve the problems of lack of chromophore, difficult detection by ultraviolet detector, no content detection method reported in literature, etc., and achieve the effect of simple method

Inactive Publication Date: 2008-02-13
JIANGSU INST OF NUCLEAR MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the lack of chromophoric groups in the structure of TRODAT-1, it is difficult to detect with general ultraviolet detectors, and no literature has reported its content detection method

Method used

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  • Analysis method of mercapto amine tropine content
  • Analysis method of mercapto amine tropine content
  • Analysis method of mercapto amine tropine content

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The selection of embodiment 1 mobile phase

[0017] The reaction formula of preparing thiolamine tropine is:

[0018]

[0019] Since compound 9 (2β-[N-[2-[S-(4-methoxybenzyl)thio]ethyl]-N-[[N-[2-[S-(4-methoxybenzyl) base)thio]ethyl]amino]formylmethyl]aminomethyl]-3β-(4-chlorophenyl)tropane) and compound 10 (2β-[N-[2-[S-(4- Methoxybenzyl)thio]ethyl]-N-[2-[N-[2-[S-(4-methoxybenzyl)thio]ethyl]amino]ethyl]aminomethyl ]-3β-(4-chlorophenyl)tropane) is the synthetic intermediate of TRODAT-1; therefore, the separation of TRODAT-1 and them should be investigated. The following solutions were respectively used as mobile phases, and experiments were carried out with a C8 column (Symmetry, 5 μm, 4.6×150 mm).

[0020] (A) Methanol-water (80:20)

[0021] (B) Methanol-water (60:40)

[0022] (C) Acetonitrile - water (80:20)

[0023] (D) Acetonitrile-water (60:40)

[0024] (E) methanol-water-TFA (80:20:0.1)

[0025] (F) Acetonitrile-water-TFA (80:20:0.1)

[0026] (G) methano...

Embodiment 2

[0028] Example 2 Setting of drift tube temperature

[0029] The temperature of the drift tube was set at 40°C to 100°C for experiments, and the results showed that the chromatographic separation was better when the temperature of the drift tube was 60°C to 80°C. Therefore, the chromatographic conditions are determined as follows: Instruments: WATERS 600 high performance liquid chromatography, WATERS 2420 evaporative light scattering detector. Chromatographic column Hypersil C8 column, 5μm, 4.6×250mm, mobile phase: methanol-acetonitrile-water-TFA (80:10:10:0.1), filter and degas through a 0.45μm organic filter membrane before use, flow rate: 1.0ml / min; injection volume: 5μl; column temperature at room temperature; ELSD drift tube temperature 60℃~80℃, carrier gas (N 2 ) pressure is 35psi.

Embodiment 3

[0030] Embodiment 3 carrier gas (N 2 ) flow setting

[0031] Carrier gas (N 2 ) pressure selection 15, 25, 35, 45psi test, the chromatographic effect is better when the pressure is 35psi.

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Abstract

The invention relates to a content analysis method for sulfhydryl-amine tropine. It uses high efficiency liquid phase chromatogram-vaporizing light scattering detector to test sulfhydryl-amine tropine. The devices that are used for chromatographic analyzing are WATERS 600 high efficiency liquid phase chromatograph, WATERS 2420 vaporizing light scattering detector, and the chromatographic column of Hypersil C8 column, 5um, 4.6*250mm. The results shows that it has good separation of the main constituents peak and the impurity peak, the linear range is 12.5-50ug / mL, and the minimum detecting quality is 3.0ng (S / N>=3), and that has about 3.6% error compared to relative standard error. The invention could test content and impurity of sulfhydryl-amine tropine, and it is simple and convenient.

Description

technical field [0001] The invention discloses a method for analyzing the content of thiolamine-tropine, which belongs to the technical field of instrumental analysis. Background technique [0002] Thiamine tropine (TRODAT-1), Chinese chemical name: 2β-[N,N'-bis(2-mercaptoethyl)ethylenediamine]methyl-3β-(4-chlorophenyl)tropane , its chemical structure is as follows: [0003] [0004] Thiaminetropine by technetium[ 99m Tc] labeled product is technetium [ 99m Tc] Thiaminetropine ( 99m Tc-TRODAT-1), Chinese chemical name: Technetium [ 99m Tc]-2β-[N,N'-bis(2-mercaptoethyl)ethylenediamine]methyl-3β-(4-chlorophenyl)tropane, this compound is a new type of dopamine successfully developed in recent years Transporter protein imaging agent is the first technetium successfully used in clinical research in the world[ 99m Tc] labeled brain receptor imaging agent, in technetium [ 99m Tc] labeled radiopharmaceuticals, nuclear pharmacy, and brain receptor imaging are all breakthrou...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02A61K51/00
Inventor 周杏琴陈正平王颂佩李晓敏唐婕曹国宪张建康邹美芬徐希杰钦晓峰
Owner JIANGSU INST OF NUCLEAR MEDICINE
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