Method for leaching natural products from mulberry branch by catalytic activation of heteropoly acid solution
A catalytic activation and natural product technology, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., to achieve the effects of reducing safety hazards and environmental pollution treatment costs, simple operation, and low production costs
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Embodiment 1
[0023] A kind of method steps of catalyzing and activating mulberry branch to extract natural products with heteropolyacid solution are as follows:
[0024] (1) Preparation of Heteropolyacid Catalytic Activation Solution
[0025] Weigh 5g NaWO first 4 After adding 10 times the volume of water to dissolve, it was added dropwise to the HCl solution with a concentration of 0.8mol / L, stirred until the yellow-green precipitate no longer increased, allowed to stand, and suction filtered to obtain the yellow-green precipitate, namely tungstic acid (H 2 WO 4 ); where HCl and NaWO 4 The molar ratio is 2.5:1, then the ratio of phosphoric acid (ml): sodium tungstate (g) is 10ml:1g, and the dilute H with a concentration of 0.12mol / L is taken. 3 PO 4 Add to tungstic acid precipitation, and after the yellow-green solid is dissolved into a colorless clear solution, a heteropoly acid solution is obtained, which is for later use.
[0026] (2) Mulberry branch pretreatment
[0027] After c...
Embodiment 2
[0034]A method for catalyzing and activating mulberry twigs to extract natural products with heteropolyacid solution, with embodiment 1, wherein:
[0035] In step (1), 3gNaWO 4 Add 8 times the volume of water to dissolve, the concentration of HCl is 0.6mol / L, HCl and NaWO 4 The molar ratio is 2:1, H 3 PO 4 (ml): NaWO 4 The ratio of (g) is 7.5ml:1g, H 3 PO 4 The concentration is 0.10mol / L;
[0036] In step (2), mulberry branches are 60 meshes;
[0037] In step (3), the ratio of mulberry branch mass (g) to heteropolyacid ionic liquid (ml) is 1g:8ml, the volume ratio of mulberry branch mass (g): ethanol aqueous solution is 1:25, and the oven temperature is 150°C , the reaction is 100min, the centrifuge speed is 3000 rpm, the centrifugation time is 20min, and the ethanol concentration is 50%;
[0038] In step (4), the volume ratio of mobile phase acetonitrile: 0.1% phosphoric acid is 10ml:90ml, the flow rate is 0.8ml / min, the column temperature is 20°C, and the detection w...
Embodiment 3
[0040] A method for catalyzing and activating mulberry twigs to extract natural products with heteropolyacid solution, with embodiment 1, wherein:
[0041] In step (1), 7gNaWO 4 Add 12 times the volume of water to dissolve, the concentration of HCl is 1.0mol / L, HCl and NaWO 4 The molar ratio is 3:1, H 3 PO 4 (ml): NaWO 4 The ratio of (g) is 12.5ml:1g, H 3 PO 4 The concentration is 0.14mol / L;
[0042] In step (2), 100 meshes of mulberry branches;
[0043] In step (3), the ratio of mulberry branch mass (g) to heteropolyacid ionic liquid (ml) is 1g:12ml, the volume ratio of mulberry branch mass (g): ethanol aqueous solution is 1:35, and the oven temperature is 170°C , the reaction is 80min, the centrifuge speed is 4000
[0044] Transfer, centrifugation time 10min, ethanol concentration 70%;
[0045] In step (4), the volume ratio of mobile phase acetonitrile: 0.3% phosphoric acid is 30ml:70ml, the flow rate is 1.2ml / min, the column temperature is 30℃, and the detection wa...
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