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
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[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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