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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.

Inactive Publication Date: 2017-06-30
YUNNAN INST OF MATERIA MEDICA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the poor solubility of crocetin, it is very difficult to separate and purify it
Using conventional chromatographic separation methods, the amount of sample loaded is very small, and a large amount of elution solvent will be consumed, which is not suitable for its large-scale preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention relates to a preparation method of high purity crocetin, and belongs to the field of Chinese herbal medicine extraction separation. The concrete step of the method is as follows: dissolving crude crocetin in an alkaline solution, standing, crystallizing, and reacting crystal with an acid to obtain the high purity crocetin. The method has the advantages of easy-to-repeat steps, easy-to-control operation conditions, easy-to-process alkaline solution, easy industrialized batch amplification production, no organic solvent residue in the whole process, products capability of being used as food and drug additives, and the purity of the final product crocetin is detected by HPLC, and can reach above 98%.

Description

technical field [0001] The invention belongs to the technical field of extraction and separation of Chinese herbal medicines, in particular to a method for further preparing high-purity crocetin from crude crocetin. Background technique [0002] Crocetin is a carotenoid component naturally present in plants such as saffron and gardenia. It has multiple unsaturated conjugated enoic acid structures. Safflower glycosides and gardenia yellow pigment) forms exist in plants such as saffron and gardenia. Crocetin has a wide range of pharmacological activities, including anti-tumor, anti-atherosclerosis, anti-hypertension and treatment of hemorrhagic shock. Development and application of cosmetics and other aspects. [0003] The binding ester glycoside of crocetin has a relatively high content in saffron, but saffron is expensive, and the cost of extracting crocetin therefrom is very high. The source of raw materials of gardenia is very rich, and the gardenia yellow pigment extra...

Claims

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Application Information

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IPC IPC(8): C07C57/13C07C51/41C07C51/02
CPCC07C51/02C07C51/412C07C57/13
Inventor 万近福李晋玉韦迪梅双喜
Owner YUNNAN INST OF MATERIA MEDICA
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