Isotope psychoactive substance labeled compound and preparation method and application thereof

A technology of active substances and compounds, which is applied in the field of preparation and application of reference substances of psychoactive substances, and can solve the problems of low detection accuracy and sensitivity of psychoactive substances

Pending Publication Date: 2021-08-31
无锡诺平医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] Aiming at the problem of low detection accuracy and sensitivity of psychoactive substances existing in the prior art, the present inve

Method used

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  • Isotope psychoactive substance labeled compound and preparation method and application thereof
  • Isotope psychoactive substance labeled compound and preparation method and application thereof
  • Isotope psychoactive substance labeled compound and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] 2-(1-(5-fluoropentyl)-indole-3-amide)--methyl 4,5,6,7-d4-3,3-dimethylbutanoate (D4-5F-MDMB- PICA) preparation method.

[0060] At -20°C, N-(formyloxy) tert-leucine methyl ester (567 mg, 3 mmol) was dissolved in 50 mL of anhydrous anhydrous carbon tetrachloride, and aluminum trichloride (400 mg, 3 mmol), then N-5-fluoropentylindole (200 mg, 1 mmol) in anhydrous carbon tetrachloride solution (25 mL) was added dropwise, stirred and slowly warmed to room temperature, and kept at room temperature for 12 hours Heat to 40 °C and heat for 2 hours. After cooling, add ammonium chloride solution to quench the reaction, remove the solvent by rotary evaporation, add 150 mL ethyl acetate to dissolve, remove insoluble matter by diatomaceous earth filtration, wash diatomaceous earth with 30 mL diethyl ether-ethyl acetate 1:1 solution, The organic phases were combined, washed with 5% hydrochloric acid aqueous solution, and the aqueous phase was extracted with ethyl acetate, and the co...

Embodiment 2

[0062] With 2-(1-(5-fluoropentyl)-indole-3-amide)-4,5,6,7-d4-3,3-dimethylbutanoic acid methyl ester (D4-5F-MDMB- PICA) was used as the internal standard to detect the content of 2-(1-(5-fluoropentyl)-indole-3-amide)-3,3-dimethylbutyric acid methyl ester (5F-MDMB-PICA) in hair.

[0063] (1) Liquid chromatography-mass spectrometry detection conditions:

[0064] a) Instrument model: Agilent 1290-6470QQQ;

[0065] b) Column: Poroshell120 PFP 3.0 x100mm 1.9um;

[0066] c) Column temperature: 30°C;

[0067] d) Mobile phase: A: acetonitrile (0.01% formic acid), B: water (0.01% formic acid, 5% ammonium formate), gradient: 1min 10%A, 2min 50%A, 4min 90%A, 6min 95%A;

[0068] e) Flow rate: 0.5 mL / min;

[0069] f) Injection volume: 5 μL;

[0070] g) Ion source: electrospray ion source, positive mode (ESI+);

[0071] h) The spray voltage is 3500 V;

[0072] i) Ion source temperature: 340°C;

[0073] j) Collision gas: nitrogen;

[0074] The ion pairs and corresponding conditions a...

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PUM

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Abstract

The invention discloses an isotope psychoactive substance labeled compound and a preparation method and application thereof. The isotope psychoactive substance labeled compound can be used for an internal standard for measuring the content of a psychoactive substance 2-(1-(5-fluoropentyl)-indole-3-amide)-3,3-dimethyl methyl butyrate in a hair sample. 2-(1-(5-fluoropentyl)-indole-3-amide)-3,3-dimethyl methyl butyrate is subjected to qualitative detection according to the retention time and ion pair matching, and specifically, corresponding compounds are subjected to quantitative detection according to the chromatographic peak area of the 2-(1-(5-fluoropentyl)-indole-3-amide)-3,3-dimethyl methyl butyrate. When the isotope labeled compound is used as the internal standard substance, the matrix effect of a detected material can be reduced, and the isotope psychoactive substance labeled compound has a good application prospect in the aspects of judicial expertise and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation and application of psychoactive substance standard substances, and specifically relates to an isotope [0002] Labeled compound of prime psychoactive substance and its preparation method and use. Background technique [0003] For the detection of trace and trace substances in test materials, liquid chromatography-mass spectrometry combined with isotope labeling [0004] Isotope dilution mass spectrometry of quasi-substance internal standard is the most common and efficient detection method. isotopically labeled [0005] The standard substance is used as an internal standard, and the isotope-labeled internal standard and the compound to be tested have complete chemical properties except molecular weight. [0006] All consistent, therefore, isotope dilution mass spectrometry can achieve high detection accuracy and sensitivity, is a trace [0007] Indispensable tool for accurate detection of ...

Claims

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Application Information

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IPC IPC(8): C07K5/078C07K1/06C07K1/107G01N30/02
CPCC07K5/06139G01N30/02
Inventor 陈飚许浩
Owner 无锡诺平医药科技有限公司
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