Method for rapidly extracting different sanshool monomers

Abstract

The invention belongs to the technical field of natural medicine extraction and separation and local anesthesia medicine preparations, and particularly relates to a method for rapidly and simultaneously extracting hydroxyl-alpha-sanshool and hydroxyl-beta-sanshool and application of the hydroxyl-alpha-sanshool obtained through extraction in preparation of a nano-lipid carrier. The method comprises the following steps: (1) extracting with ethanol and n-hexane to obtain a crude sanshool product; and (2) respectively obtaining high-purity hydroxyl-alpha-sanshool and hydroxyl-beta-sanshool by adopting a column chromatography method and a freeze drying method. The preparation method disclosed by the invention is simple to operate, mild in condition, recyclable in polyamide and high in recovery rate, not only ensures the purity of the two sanshool, but also reduces the operation cost. Meanwhile, the invention discloses the hydroxyl-alpha-sanshool nanostructure lipid carrier and a preparation method thereof. The preparation is released through slow release and has a good analgesic effect.

Description

technical field

[0001] The invention belongs to the technical field of extraction and separation of natural medicines and local anesthetic preparations, in particular to a method for quickly and simultaneously extracting hydroxyl-α-sanshool and hydroxyl-β-sanshool, and simultaneously extracting and obtaining hydroxyl-α-sanshool in the preparation of nano Applications in Lipid Carriers. Background technique

[0002] Pepper (Zanthoxylum L) belongs to the Rutaceae plant, and its fruit is commonly used as a food seasoning in my country. It has a strong aroma and a spicy taste. Not only that, Zanthoxylum bungeanum is also a traditional Chinese medicine, which has the functions of warming the middle and dispelling cold, dehumidification, killing insects, and relieving pain. It can be used to treat vomiting, diarrhea, and insect repellent. Its active ingredients have the functions of antibacterial, anti-inflammatory, anti-wrinkle, lowering blood sugar and blood fat, protecting gas...

Examples

Embodiment 1

[0057] The method for rapidly extracting hydroxy-α-sanshool and hydroxy-β-sanshool simultaneously:

[0058] (1) Take 20 g of dried Zanthoxylum bungeanum residue, add a 30% ethanol solution with a volume fraction of 1:15 (g / mL), extract in a water bath at 60°C for 1 hour, extract 3 times, combine the extracts, and store at 30°C Concentrate under reduced pressure to obtain pepper extract.

[0059] (2) Add n-hexane to the Zanthoxylum bungeanum extract obtained in step (1) for extraction, the volume ratio of n-hexane and Zanthoxylum bungeanum extract is 1:1 (v / v), extract in a water bath at 55°C for 1 hour, repeat the extraction 3 times, The n-hexane extracts obtained from the combined extraction were concentrated under reduced pressure at 25°C, placed in a refrigerator at low temperature (-4°C) for freezing and crystallization for 12 hours, filtered, and this step was repeated 3 times to obtain 0.3 g of crude sanshool.

[0060] (3) Add 10mL of absolute ethanol to the crude produ...

Embodiment 2

[0063] Reclaim the used polyamide resin of above-mentioned embodiment 1:

[0064] Discard the mixed sample polyamide resin in the upper layer, and use 4 times column volume of absolute ethanol solution, 1 times column volume of aqueous solution, 3 times column volume of 5% sodium hydroxide aqueous solution, 1 times column volume of aqueous solution at a flow rate of 5mL / min, 3 times the column volume of 10% glacial acetic acid aqueous solution to wash the polyamide resin after use, and finally elute with water until the pH is neutral.

Embodiment 3

[0066] The method for rapidly extracting hydroxy-α-sanshool and hydroxy-β-sanshool simultaneously:

[0067] (1) Take 20g of dried Zanthoxylum bungeanum, add ethanol solution with a volume fraction of 50%, the ratio of solid to liquid is 1:15 (g / mL), extract in a water bath at 60°C for 1 hour, extract 3 times, combine the extracts, Concentrate under reduced pressure to obtain pepper extract.

[0068] (2) Add petroleum ether to the Zanthoxylum bungeanum extract obtained in step (1) for extraction, the volume ratio of petroleum ether and Zanthoxylum bungeanum extract is 1:1 (v / v), extract in a water bath at 55°C for 1 hour, and repeat the extraction 3 times, The n-hexane extracts obtained from the combined extraction were concentrated under reduced pressure at 25°C, placed in a refrigerator at low temperature (-4°C) for freezing and crystallization for 12 hours, filtered, and this step was repeated 3 times to obtain 0.4 g of crude sanshool.

[0069] (3) Add 10mL of absolute etha...

technical field

[0001] The invention belongs to the technical field of extraction and separation of natural medicines and local anesthetic preparations, in particular to a method for quickly and simultaneously extracting hydroxyl-α-sanshool and hydroxyl-β-sanshool, and simultaneously extracting and obtaining hydroxyl-α-sanshool in the preparation of nano Applications in Lipid Carriers. Background technique

[0002] Pepper (Zanthoxylum L) belongs to the Rutaceae plant, and its fruit is commonly used as a food seasoning in my country. It has a strong aroma and a spicy taste. Not only that, Zanthoxylum bungeanum is also a traditional Chinese medicine, which has the functions of warming the middle and dispelling cold, dehumidification, killing insects, and relieving pain. It can be used to treat vomiting, diarrhea, and insect repellent. Its active ingredients have the functions of antibacterial, anti-inflammatory, anti-wrinkle, lowering blood sugar and blood fat, protecting gas...

Examples

Embodiment 1

[0057] The method for rapidly extracting hydroxy-α-sanshool and hydroxy-β-sanshool simultaneously:

[0058] (1) Take 20 g of dried Zanthoxylum bungeanum residue, add a 30% ethanol solution with a volume fraction of 1:15 (g / mL), extract in a water bath at 60°C for 1 hour, extract 3 times, combine the extracts, and store at 30°C Concentrate under reduced pressure to obtain pepper extract.

[0059] (2) Add n-hexane to the Zanthoxylum bungeanum extract obtained in step (1) for extraction, the volume ratio of n-hexane and Zanthoxylum bungeanum extract is 1:1 (v / v), extract in a water bath at 55°C for 1 hour, repeat the extraction 3 times, The n-hexane extracts obtained from the combined extraction were concentrated under reduced pressure at 25°C, placed in a refrigerator at low temperature (-4°C) for freezing and crystallization for 12 hours, filtered, and this step was repeated 3 times to obtain 0.3 g of crude sanshool.

[0060] (3) Add 10mL of absolute ethanol to the crude produ...

Embodiment 2

[0063] Reclaim the used polyamide resin of above-mentioned embodiment 1:

[0064] Discard the mixed sample polyamide resin in the upper layer, and use 4 times column volume of absolute ethanol solution, 1 times column volume of aqueous solution, 3 times column volume of 5% sodium hydroxide aqueous solution, 1 times column volume of aqueous solution at a flow rate of 5mL / min, 3 times the column volume of 10% glacial acetic acid aqueous solution to wash the polyamide resin after use, and finally elute with water until the pH is neutral.

Embodiment 3

[0066] The method for rapidly extracting hydroxy-α-sanshool and hydroxy-β-sanshool simultaneously:

[0067] (1) Take 20g of dried Zanthoxylum bungeanum, add ethanol solution with a volume fraction of 50%, the ratio of solid to liquid is 1:15 (g / mL), extract in a water bath at 60°C for 1 hour, extract 3 times, combine the extracts, Concentrate under reduced pressure to obtain pepper extract.

[0068] (2) Add petroleum ether to the Zanthoxylum bungeanum extract obtained in step (1) for extraction, the volume ratio of petroleum ether and Zanthoxylum bungeanum extract is 1:1 (v / v), extract in a water bath at 55°C for 1 hour, and repeat the extraction 3 times, The n-hexane extracts obtained from the combined extraction were concentrated under reduced pressure at 25°C, placed in a refrigerator at low temperature (-4°C) for freezing and crystallization for 12 hours, filtered, and this step was repeated 3 times to obtain 0.4 g of crude sanshool.

[0069] (3) Add 10mL of absolute etha...

Images