Preparation method of high purity crocetin
A crocus acid, high-purity technology, applied in the field of preparing high-purity crocus acid, can solve the problems of difficult separation and purification, small sample loading, consumption of elution solvent, etc.
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Embodiment 1
[0019] Preparation of crocetin crude product: 1000 g of gardenia water or ethanol extract, add 10 L of 4% sodium hydroxide aqueous solution to dissolve, hydrolyze at 50 ° C for 2.5 hours, add hydrochloric acid with a concentration of 20% by mass to adjust the pH value to 2.0, Stand still for 10 hours to precipitate a precipitate, centrifuge, take the precipitate and wash with water until the pH value of the washed water is neutral. The obtained precipitate was vacuum-dried at 50° C. for 3 hours to obtain 50.5 g of crude crocetin, whose mass percentage of crocetin was 10.6% as detected by HPLC.
[0020] Take 10.0 g of the crude crocetin prepared in this example, add 500 mL of 10% sodium hydroxide aqueous solution, heat to 50° C. to dissolve, and remove insoluble impurities by filtration while hot. The filtrate was left at room temperature (20-25° C.) for 10 hours, and crocetin crystals were precipitated. The crocetin salt crystals are recrystallized 1-3 times with 10% sodium h...
Embodiment 2
[0022] Take 10.0 g of the crude product of crocetin prepared in Example 1, add 500 mL of 20% potassium hydroxide aqueous solution by mass percentage, heat to 60° C. to dissolve, and remove insoluble impurities by filtration while hot. The filtrate was placed in the refrigerated layer of the refrigerator (2-8° C.) for 10 hours, and crocetin salt crystals were precipitated, and the crocetin salt crystals were recrystallized 3 times with an aqueous potassium hydroxide solution with a concentration of 20% by mass to obtain High-purity crocetin has a purity of 99.4% as detected by HPLC. Add 50% ethanol aqueous solution to the high-purity saffron salt, heat until it is completely dissolved, adjust the pH value to 4.0 with 30% hydrochloric acid, and let it stand for 10 hours to precipitate saffron The flower acid is precipitated, centrifuged, and the precipitate is washed repeatedly with water until the pH value of the washed water is neutral. The washed precipitate was vacuum-dried...
Embodiment 3
[0024] Take 10.0 g of the crude product of crocetin prepared in Example 1, add 500 mL of 50% ethanol in ammonia solution, heat to 40° C. to dissolve the solid, and remove insoluble impurities by filtration while hot. The filtrate was placed in the refrigerated layer of the refrigerator (2-8°C) for 10 hours, and crocetin crystals were precipitated. Crocetin salt crystals were recrystallized three times with 50% ethanol ammonia solution to obtain high-purity crocetin salt, and the purity was 98.8% as detected by HPLC. suspending high-purity crocetin in 10% sulfuric acid aqueous solution, stirring slowly until the suspended matter turns red, centrifuging, taking the precipitate and washing it repeatedly with water until the pH value of the washed water is neutral. The washed precipitate was vacuum-dried at 50° C. for 4 hours to obtain 0.89 g of crocetin, whose purity was 98.5% as detected by HPLC.
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