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A method for the separation and determination of pet imaging agent precursor tsop-(+)-dtbz and its optical isomers

A technology of PET imaging agent and optical isomer, which is applied in the field of analytical chemistry to achieve the effect of good peak symmetry

Active Publication Date: 2018-10-19
JIANGSU INST OF NUCLEAR MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Therefore, the technical problem to be solved by the present invention is to overcome the defect that there is no separation and detection method for the labeling precursor TsOP-(+)-DTBZ and its optical isomers in the prior art, thereby providing a PET imaging agent precursor TsOP- The separation and determination method of (+)-DTBZ and its optical isomers, and then realize the separation and determination of the precursor and its optical isomers

Method used

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  • A method for the separation and determination of pet imaging agent precursor tsop-(+)-dtbz and its optical isomers
  • A method for the separation and determination of pet imaging agent precursor tsop-(+)-dtbz and its optical isomers
  • A method for the separation and determination of pet imaging agent precursor tsop-(+)-dtbz and its optical isomers

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Instruments and Conditions

[0046] Mobile phase: n-hexane-1,2-dichloroethane-absolute ethanol-trifluoroacetic acid-triethylamine=65:33:2:0.01:0.005

[0047] Flow rate: 0.8mL / min

[0048] Column temperature: 25°C

[0049] Injection volume: 20μL

[0050] UV detection wavelength 280nm

[0051] Experimental steps:

[0052] Accurately weigh 5 mg of TsOP-(+)-DTBZ and its isomers respectively, put them in a 10 mL brown volumetric flask, add mobile phase to dissolve and dilute to the mark, shake well, and use it as the test solution. Get need testing solution and carry out high performance liquid chromatography analysis according to above-mentioned conditions, record chromatogram.

[0053] see attached results figure 1 , it can be seen that TsOP-(+)-DTBZ and its isomers achieve baseline separation under this condition, and the high performance liquid chromatography shows a resolution of 2.5.

Embodiment 2

[0055] Instruments and Conditions

[0056] Mobile phase: n-hexane-1,2-dichloroethane-absolute ethanol-trifluoroacetic acid-triethylamine=64.6:32.3:3.1:0.01:0.005

[0057] Flow rate: 0.8mL / min

[0058] Column temperature: 30°C

[0059] Injection volume: 20μL

[0060] UV detection wavelength 280nm

[0061] Experimental steps:

[0062] Accurately weigh 10 mg of TsOP-(+)-DTBZ and its isomers respectively, put them in a 10 mL brown volumetric flask, add mobile phase to dissolve and dilute to the mark, shake well, and use it as the test solution. Get need testing solution and carry out high performance liquid chromatography analysis according to above-mentioned conditions, record chromatogram.

[0063] see attached results figure 2 , showing that the separation and detection method of the present invention can separate TsOP-(+)-DTBZ and its isomers, and the high-performance liquid chromatography shows that the separation degree is 2.2.

Embodiment 3

[0065] Instruments and Conditions

[0066] Mobile phase: n-hexane-1,2-dichloroethane-absolute ethanol-trifluoroacetic acid-triethylamine=64:32:4:0.01:0.005

[0067] Flow rate: 0.8mL / min

[0068] Column temperature: 25°C

[0069] Injection volume: 20μL

[0070] UV detection wavelength 280nm

[0071] Experimental steps:

[0072] Accurately weigh 5 mg of TsOP-(+)-DTBZ and its isomers respectively, put them in a 10 mL brown volumetric flask, add mobile phase to dissolve and dilute to the mark, shake well, and use it as the test solution 1. In addition, accurately weigh 10 mg of TsOP-(+)-DTBZ bulk drug, put it in a 10 mL brown volumetric flask, add mobile phase to dissolve and dilute to the mark, shake well, and use it as the test solution 2.

[0073] Get need testing solution and carry out high performance liquid chromatography analysis by above-mentioned conditions, record chromatogram, the result sees attached image 3 .

[0074] image 3 It is proved that this method ca...

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Abstract

The invention discloses a PET developing agent precursor TsOP-(+)-DTBZ and a separation and measurement method of an optical isomer thereof and belongs to the field of analytical chemistry. The separation and measurement method is a normal-phase chromatography by means of a Pirkle type chiral stationary phase chromatographic column and with a normal-phase mixed solvent serving as a mobile phase for separation. By means of the method, the PET developing agent precursor and the optical isomer of the PET developing agent precursor can be easily, quickly and accurately separated and detected, and the mass of the precursor TsOP-(+)-DTBZ can be effectively controlled.

Description

technical field [0001] The invention relates to the field of analytical chemistry, in particular to a method for separating and measuring PET imaging agent precursor TsOP-(+)-DTBZ and its optical isomers. Background technique [0002] Parkinson's disease (PD) is a common degenerative disease of the central nervous system, which is more common in the elderly. Work and life, because people are not familiar with the early symptoms, the best time for treatment has been missed by the time of diagnosis, so early diagnosis and early treatment are extremely important. The pathogenesis of PD is still unclear, and the degeneration of dopaminergic neurons in the nigrostriatum is the main pathological feature of PD. Studies suggest that the reduction of central vesicular monoamine transporter (VMAT2) caused by genetic or environmental factors is an important determinant of PD pathogenesis. Therefore, using molecular imaging techniques, positron emission tomography (PET) and The develo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/60
CPCG01N30/02G01N30/60G01N2030/027
Inventor 李晓敏陈正平刘春仪唐婕薛丹露曹丽华徐栋
Owner JIANGSU INST OF NUCLEAR MEDICINE
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