Chlorogenic acid calcium salt sesquihydrate and application thereof
A technology of sesquihydrate and calcium chlorogenic acid, applied in the field of calcium chlorogenic acid sesquihydrate, can solve problems such as limitations, and achieve the effect of good stability and improved activity
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Embodiment 1
[0051] Add 40.0g of chlorogenic acid (113mmol) and 600mL of purified water into the reaction flask, slowly add 113mL of sodium bicarbonate aqueous solution (1mol / L) dropwise at 20°C, and stir at the same temperature for 30min after the dropping is complete. Then slowly add 58ml of calcium chloride solution (1mol / L) to the system dropwise, stir at 20°C for 1h, filter, rinse the filter cake with a small amount of purified water, and dry it in vacuum at 55°C for 20h to obtain off-white solid calcium salt of chlorogenic acid Sesquihydrate 40.97g, yield 90.6%.
[0052] The thermogravimetric analysis results show that the right weight loss is 7.079% at 150°C, which is the characteristic weight loss of 1.5 molecules of water; the X-ray powder diffraction test results show that the crystal is a new crystal form, and the X-ray powder diffraction spectrum of the crystal is detailed in figure 1 , see the thermogravimetric analysis spectrum for details figure 2 .
Embodiment 2
[0054] Add 40.0g of chlorogenic acid (113mmol) and 600mL of purified water into the reaction flask, slowly add 113mL of sodium bicarbonate aqueous solution (1mol / L) dropwise at 20°C, and stir at the same temperature for 30min after the dropping is complete. Then slowly add 58ml of calcium chloride solution (1mol / L) dropwise to the system, stir at 10°C for 30min, filter, rinse the filter cake with a small amount of purified water, and dry it in vacuum at 45°C for 25h to obtain off-white solid calcium salt of chlorogenic acid Sesquihydrate 41.32g, yield 91.4%. Moisture test result: 6.8%. Corresponding X-ray powder diffraction spectrogram and thermogravimetric analysis spectrogram are with embodiment 1.
Embodiment 3
[0056] Add 40.0g of chlorogenic acid (113mmol) and 600mL of purified water into the reaction flask, slowly add 113mL of sodium bicarbonate aqueous solution (1mol / L) dropwise at 20°C, and stir at the same temperature for 30min after the dropping is complete. Then slowly drop 58ml of calcium chloride solution (1mol / L) into the system, stir at 30°C for 1.5h, filter, rinse the filter cake with a small amount of purified water, and dry it in vacuum at 65°C for 20h to obtain off-white solid calcium chlorogenic acid Salt sesquihydrate 38.54g, yield 85.3%. Moisture test result: 7.1%. Corresponding X-ray powder diffraction spectrogram and thermogravimetric analysis spectrogram are with embodiment 1.
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