Preparation method of high-purity monascus pigment component

Abstract

The invention provides a novel process for preparing high-purity monascus pigment. The process comprises the following steps of: crushing red yeast rice as a raw material; and separating and purifying to obtain 6 kinds of monascus pigment components by adopting a composite technology of extraction liquid extraction and high-speed countercurrent chromatography separation and crystallization, wherein the six monascus pigment components comprise rubropunctamine, monascorubramine, monascin, ankaflavin, rubropunctatin and monascorubin, and the purities of all the pigments are higher than 95 percent and can be used for preparing foods, cosmetic colorants and health products. The invention adopts easily-recovered organic solvent for separation to save the consumption of separation materials andovercome the problems of small treatment amount and inefficient single pigment component separation and purification of a TLC (Thin Layer Chromatography), an HPLC (High Performance Liquid Chromatography), a resin method and a silica gel column chromatography. The invention adopts the composite technology of the extraction liquid extraction and the high-speed countercurrent chromatography separation and the crystallization to prepare six kinds of high-purity monascus pigment crystals and has the advantages of simple steps and high yield.

Description

technical field

[0001] The invention belongs to the technical field of biochemical products, and in particular relates to a preparation method of high-purity monascus pigment. Background technique

[0002] High-speed counter-current chromatography (High-Speed ​​Counter-Current Chromatography, HSCCC) is a chromatographic method that uses the difference in the distribution coefficient of the solute in two immiscible solvent systems to separate. High-speed countercurrent chromatography technology does not require solid-phase support, avoiding sample loss and denaturation caused by irreversible adsorption. The organic solvent used for separation is easy to recycle and use, and saves the consumption of separation materials. This technology has been widely used in the separation and preparation of flavonoids, alkaloids, plant polyphenols, esters, terpenes, lignans, coumarins, saponins and other natural phytochemical components and antibiotics. The preparation of six high-purity m...

Examples

Embodiment 1

[0022] Red yeast rice has a rice color value of 5100 U / g, contains red pigments (erythematine and monascorubin) 10.1 g / Kg, orange pigments (erythematin and monascorubin) 48.3 g / Kg, and yellow pigments (monasculin and red Triflavin) 41.9 g / Kg. After crushing to a particle size of 0.1mm, using 70% (weight ratio, the same below) ethanol solution extraction (60°C water bath, solid-liquid ratio 1:10), vacuum concentration to 1 / 2 the original volume to precipitate the crude monascus pigment extract , The yield is 10.1%.

[0023] A high-speed countercurrent chromatography system with a column volume of 300 mL was used for separation. Select n-hexane-methanol-water as the solvent system, according to the ratio of 10:7.5:2.5 (v:v:v:v), dispose the above solvent components in the separatory funnel, shake well and stand for stratification. Take the upper layer as the stationary phase and the lower layer as the mobile phase.

[0024] Weigh 200 mg of crude monascus pigment extract and dissol...

Embodiment 2

[0028] Red yeast rice has a color value of 3000 U / g, crushed to a particle size of 1 mm, extracted with a 70% (weight ratio, the same below) methanol solution (60℃ water bath, solid-liquid ratio 1:15), and then concentrated to the original volume 1 / 3. The crude monascus pigment is separated out, the yield is 6.7%.

[0029] A high-speed countercurrent chromatography system with a column volume of 1000 mL was used for separation. Select petroleum ether-ethyl acetate-ethanol-water as the solvent system, according to the ratio of 2.5:7.5:5:5 (v:v:v:v), dispose the above solvent components in the separatory funnel, shake well and then stand still 置layered. Take the upper layer as the stationary phase and the lower layer as the mobile phase.

[0030] Weigh 800mg of the crude monascus pigment extract and dissolve it with 50mL stationary phase for use. Before injection, fill the entire column volume with the stationary phase, adjust the host speed to 900rpm / min, pump the mobile phase in...

Embodiment 3

[0033] Red yeast rice has a color price of 4000 U / g, crushed to a particle size of 1 mm, and extracted with a 90% acetone aqueous solution (60°C water bath, solid-liquid ratio 1:5), and the extracted extract is vacuum concentrated to 1 / 3 of the original volume to precipitate. The crude extract of monascus pigment component has a yield of 8.5%.

[0034] A high-speed countercurrent chromatography system with a column volume of 1000 mL was used for separation. Choose cyclohexane-chloroform-isopropanol-water as the solvent system, according to the ratio of 5:6:8:2.5 (v:v:v:v), dispose the above solvent components in the separatory funnel, shake well Let stand for layering. Take the upper layer as the stationary phase and the lower layer as the mobile phase.

[0035] Weigh 800mg of the crude monascus pigment extract and dissolve it with 50mL stationary phase for use. Before injection, fill the entire column volume with the stationary phase, adjust the host speed to 900rpm / min, pump t...

technical field

[0001] The invention belongs to the technical field of biochemical products, and in particular relates to a preparation method of high-purity monascus pigment. Background technique

[0002] High-speed counter-current chromatography (High-Speed ​​Counter-Current Chromatography, HSCCC) is a chromatographic method that uses the difference in the distribution coefficient of the solute in two immiscible solvent systems to separate. High-speed countercurrent chromatography technology does not require solid-phase support, avoiding sample loss and denaturation caused by irreversible adsorption. The organic solvent used for separation is easy to recycle and use, and saves the consumption of separation materials. This technology has been widely used in the separation and preparation of flavonoids, alkaloids, plant polyphenols, esters, terpenes, lignans, coumarins, saponins and other natural phytochemical components and antibiotics. The preparation of six high-purity m...

Examples

Embodiment 1

[0022] Red yeast rice has a rice color value of 5100 U / g, contains red pigments (erythematine and monascorubin) 10.1 g / Kg, orange pigments (erythematin and monascorubin) 48.3 g / Kg, and yellow pigments (monasculin and red Triflavin) 41.9 g / Kg. After crushing to a particle size of 0.1mm, using 70% (weight ratio, the same below) ethanol solution extraction (60°C water bath, solid-liquid ratio 1:10), vacuum concentration to 1 / 2 the original volume to precipitate the crude monascus pigment extract , The yield is 10.1%.

[0023] A high-speed countercurrent chromatography system with a column volume of 300 mL was used for separation. Select n-hexane-methanol-water as the solvent system, according to the ratio of 10:7.5:2.5 (v:v:v:v), dispose the above solvent components in the separatory funnel, shake well and stand for stratification. Take the upper layer as the stationary phase and the lower layer as the mobile phase.

[0024] Weigh 200 mg of crude monascus pigment extract and dissol...

Embodiment 2

[0028] Red yeast rice has a color value of 3000 U / g, crushed to a particle size of 1 mm, extracted with a 70% (weight ratio, the same below) methanol solution (60℃ water bath, solid-liquid ratio 1:15), and then concentrated to the original volume 1 / 3. The crude monascus pigment is separated out, the yield is 6.7%.

[0029] A high-speed countercurrent chromatography system with a column volume of 1000 mL was used for separation. Select petroleum ether-ethyl acetate-ethanol-water as the solvent system, according to the ratio of 2.5:7.5:5:5 (v:v:v:v), dispose the above solvent components in the separatory funnel, shake well and then stand still 置layered. Take the upper layer as the stationary phase and the lower layer as the mobile phase.

[0030] Weigh 800mg of the crude monascus pigment extract and dissolve it with 50mL stationary phase for use. Before injection, fill the entire column volume with the stationary phase, adjust the host speed to 900rpm / min, pump the mobile phase in...

Embodiment 3

[0033] Red yeast rice has a color price of 4000 U / g, crushed to a particle size of 1 mm, and extracted with a 90% acetone aqueous solution (60°C water bath, solid-liquid ratio 1:5), and the extracted extract is vacuum concentrated to 1 / 3 of the original volume to precipitate. The crude extract of monascus pigment component has a yield of 8.5%.

[0034] A high-speed countercurrent chromatography system with a column volume of 1000 mL was used for separation. Choose cyclohexane-chloroform-isopropanol-water as the solvent system, according to the ratio of 5:6:8:2.5 (v:v:v:v), dispose the above solvent components in the separatory funnel, shake well Let stand for layering. Take the upper layer as the stationary phase and the lower layer as the mobile phase.

[0035] Weigh 800mg of the crude monascus pigment extract and dissolve it with 50mL stationary phase for use. Before injection, fill the entire column volume with the stationary phase, adjust the host speed to 900rpm / min, pump t...

Images