A kind of synthetic method of deuterium-labeled zearalenone and its derivatives
A technology of zearalenone and zearalenone, which is applied in the synthesis of deuterium-labeled zearalenone and its derivatives, and the application field of mass spectrometry detection methods, which can solve the problem of low concentration of substances to be tested and complex sample matrices , diverse metabolites and other issues, to achieve the effect of simple synthesis method, high isotope abundance and high purity
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Embodiment 1
[0055] The synthetic method of the deuterium-labeled zearalenone of formula (1)
[0056]
[0057] Step 1): In a round bottom flask protected by a nitrogen atmosphere, add CD 3 OD (100mL), sodium (1.6g, 70mmol), and stir until the sodium is completely dissolved to obtain the reactant; step 2): add zearalenone (7.3g, 23mmol) to the reactant, and react at 50°C for 3 hours .
[0058] Purification process after the reaction is completed: after cooling the product obtained in step 2), add hydrochloric acid ethanol solution to adjust the pH value to 3, and spin to dry the solvent. After adding 50mL of water, it was adjusted to alkaline with aqueous ammonia, and extracted three times with dichloromethane. The combined organic phases were washed with saturated brine and dried over anhydrous sodium sulfate. After filtration, the solvent was spin-dried and recrystallized to obtain 5.6 g of deuterium-labeled zearalenone of formula (1), with a yield of 75%, a purity of 99.8% (HPLC), ...
Embodiment 2
[0061] The synthetic method of the deuterium-labeled zearalane of formula (2)
[0062]
[0063] The reaction conditions and purification process are the same as in Example 1, and details are not repeated here.
Embodiment 3
[0065] The synthetic method of the deuterium-labeled zearalane of formula (2)
[0066]
[0067] The compound of formula (1) prepared in Example 1 is used to prepare the compound of formula (2);
[0068] Add platinum oxide (500mg), ethanol (20mL) into a round bottom flask, freeze and degas with liquid nitrogen, add deuterium-labeled zearalenone (515mg, 1.6mmol) of formula (1) in ethanol (10mL) at 0°C ), and reacted with hydrogen (0.1MPa) for 3 hours.
[0069] After filtration, the solvent was spin-dried, dissolved in ethyl acetate and purified on a silica gel column to obtain 192 mg of deuterium-labeled zearalenone of formula (2), with a yield of 37%, a purity of 99.7% (HPLC), and an isotopic abundance of 99.2% (atom%, HRMS).
[0070] 1 H NMR (300MHz, acetone-d 6 )δ6.70(1H,s),6.12(1H,s),5.17(1H,m),3.58(2H,d),2.42(2H,m),2.10(2H,m),1.86(2H,m ), 1.66(2H,m), 1.52(2H,m), 1.34(3H,d).
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