A method for identification of illegally added cyclohexyl nortadalafil in food

A technology of nortadalafil and illegal addition, applied in instruments, measuring devices, scientific instruments, etc., can solve the problems of lack of preparation and identification methods of new tadalafil derivatives, and achieve high resolution and high sensitivity , the effect of ensuring accuracy

Active Publication Date: 2022-05-24
广西东盟食品检验检测中心
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Problems solved by technology

[0007] The purpose of the present invention is to provide an identification method for the illegal addition of cyclohexyl nortadalafil in food, so as to solve the technical problems of the preparation and identification method of novel tadalafil derivatives that lack commercial standards in the prior art

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  • A method for identification of illegally added cyclohexyl nortadalafil in food
  • A method for identification of illegally added cyclohexyl nortadalafil in food
  • A method for identification of illegally added cyclohexyl nortadalafil in food

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Embodiment 1

[0035] An identification method for illegal addition of cyclohexyl desmethyltadalafil to food, including the following steps:

[0036] (1) Preparation of samples:

[0037] S1: UPLC-Q-OrbitrapHRMS Ultra High Performance Liquid Chromatography - Four-Stage Rod / Electrostatic Orbital Well High Resolution Mass Spectrometer and HPLC High Performance Liquid Chromatograph for Test Solution Preparation

[0038] Take 10 mg of the sample, add 100 mL of methanol, sonic for 30 min, filter, as UPLC-Q-Orbitrap HRMS and HPLC test solution.

[0039] S2: Separation and purification of compounds

[0040] Take 2g of the sample, add 10mL of methanol, ultrasound 30min, filter, take the filtrate appropriate amount of injection, collect the main chromatographic peak components, reduce pressure evaporation to remove the solvent, that is, the purifier 10mg, the puritate purity of 97%.

[0041] S3: NMR NMR for sample preparation: Take 15 mg of the purified compound obtained in step S2 and dissolve it into th...

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Abstract

The invention discloses an identification method for illegally adding cyclohexyl nortadalafil to food, and belongs to the field of medicinal chemistry. Described identification method comprises the following steps: (1) prepares the need testing solution of UPLC-Q-Orbitrap HRMS ultra-high performance liquid chromatography-quadrupole / electrostatic orbitrap high-resolution mass spectrometer and HPLC high-performance liquid chromatography Need testing solution; (2) get need testing and carry out compound separation and purification, obtain purified matter; (3) get gained purified matter, prepare NMR nuclear magnetic resonance instrument need testing; (4) need testing is detected, including using LC‑20AR prepared liquid chromatography, PAD diode array detector, analyzed the obtained primary and secondary mass spectra and characteristic absorption spectra, and obtained the structural formula of cyclohexyl nortadalafil through nuclear magnetic resonance, Finally, the illegally added cyclohexyl nortadalafil was identified. Using the method of the invention, the illegally added cyclohexyl nortadalafil in food can be effectively identified.

Description

Technical field [0001] The present invention relates to the field of medicinal chemistry, in particular to an identification method for the illegal addition of cyclohexyl desmethyltadalafil in a food. Background [0002] China's laws and regulations strictly prohibit the addition of chemical substances other than food additives to food, and such illegal additions have always been severely cracked down. Under the high-pressure crackdown, criminals opportunistically added other analogues outside the detection range of the current standard. An unknown tadalafil derivative, a selective reversible phosphodiesterase 5 (PDE5) inhibitor for the treatment of erectile dysfunction in men, was found using ultra-high performance liquid chromatography-quad rod electrostatic field orbital ion trap mass spectrometry screening techniques. The derivative has the same parent nucleus as tadalafil, which has been approved for marketing, with small structural differences. The establishment of this met...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 刘珈伶戴向东陈小聪杨方方袁光蔚廖强刘欣宜
Owner 广西东盟食品检验检测中心
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