Method for extracting lignan compounds from Chinese magnolia vine fruit

Abstract

The invention provides a method for extracting lignan compounds from Chinese magnolia vine fruit, and belongs to the technical field of traditional Chinese medicine extracts. The method comprises thefollowing steps: firstly, soaking Chinese magnolia vine fruit sample powder with a proper amount of absolute ethyl alcohol, then extracting lignan compounds in the Chinese magnolia vine fruit througha magnetic stirring assisted supercritical CO2 extraction method to obtain a solid-liquid mixture after the extraction is finished, then transferring the obtained solid-liquid mixture into a centrifugal tube for centrifugal separation, collecting all supernatants, and concentrating under reduced pressure to obtain extract; and performing vacuum drying and crushing on the extract to form powder, thereby obtaining the Chinese magnolia vine fruit lignan extract. According to the method, magnetic stirring and supercritical CO2 extraction are combined for the first time, the magnetic stirring is beneficial to fully mixing the extraction solvent and the sample, and the contact frequency between the extraction solvent and the sample is increased, so that the extraction efficiency is improved. Besides, before supercritical CO2 extraction, a small amount of absolute ethyl alcohol is adopted as an auxiliary extraction solvent in advance to impregnate the sample, so that the dissolving power andselectivity of supercritical CO2 in the extraction process are enhanced, and the extraction pressure is reduced.

Description

technical field

[0001] The invention belongs to the technical field of traditional Chinese medicine extracts, and in particular relates to a method for extracting lignan compounds in Schisandra chinensis. Background technique

[0002] Schisandra, a plant of the genus Schisandra in the family Magnoliaceae, can be divided into northern Schisandra and southern Schisandra due to different growth regions. Schisandra chinensis is irregular spherical or oblate, with a diameter of 5-8mm. The surface of Schisandra chinensis is red, purple or dark red, the skin is shrunken, oily, and the flesh is soft, and some of the surface is black red or "hoarfrost". The granules of Schisandra chinensis are small, the surface is brown-red or dark brown, the peel is shriveled and shrunken, and the pulp often clings to the seeds. Traditional Chinese medicine believes that Schisandra is sour and warm in nature and non-toxic. It is usually used to treat cough and asthma caused by senile diseases cau...

Examples

Embodiment 1

[0042] Take 0.5mg of schisandrin A, gomisin D, schisandrin B, schisandrin, schisandrin A, schisandrin, schisandrin B, and schisandrin C respectively in a 10mL brown volumetric flask, add chromatographic grade methanol to dilute to Scale, sonication, so that the eight lignan compounds can be better dissolved in methanol, and the dissolved solution is stored in a refrigerator at 4°C for future use. With the concentration as the abscissa and the peak area as the ordinate, draw a standard curve, such as figure 2 shown.

[0043] Turn on the low-temperature constant temperature tank 3, set the temperature to 5°C, and when the set temperature is reached, open the high-purity air valve 1 and the high-purity CO 2 Valve 2, into high-purity air and CO 2 , make the system full of gas, at the same time, weigh 5g schisandra sample powder in the extraction kettle 6, and add 10mL of dehydrated ethanol, the concentration of the dehydrated alcohol is 100%, tighten the seal, then put the extr...

Embodiment 2

[0047] The specific steps and conditions are the same as in Example 1, except that the extraction pressure in the extraction kettle is respectively 0, 3, 7.5 and 12 MPa; the impact on the extraction rate of lignans under the different extraction pressures of Examples 1 and 2 like Figure 4 shown.

[0048] Figure 4 Note: without CO 2 In the case of , the extraction rate of the target substance is low, but with the increase of the extraction pressure, the supercritical CO 2 Continuously entering the inside of the sample greatly improves the mass transfer efficiency. When the extraction pressure is 9MPa, the extraction rate of the target analyte reaches the maximum. Description supercritical CO 2 As an extraction solvent, its dosage will have a crucial impact on the extraction rate of the target substance.

Embodiment 3

[0050] The specific steps and conditions are the same as in Example 1. The difference is that the concentration of ethanol is 40, 60, and 80% respectively. The effects on the extraction rate of lignans under different ethanol concentrations in Examples 1 and 3 are as follows: Figure 5 shown.

[0051] Figure 5 It shows that the higher the concentration of ethanol, the higher the extraction rate of the target compound. On the one hand, due to the large polarity of ethanol molecules, which greatly increases the lignans in supercritical CO 2 On the other hand, ethanol, as an organic solvent, is easy to form hydrogen bonds with lignans, which can significantly improve the extraction efficiency. Therefore, the use of absolute ethanol as an impregnating solvent has a good effect.

technical field

[0001] The invention belongs to the technical field of traditional Chinese medicine extracts, and in particular relates to a method for extracting lignan compounds in Schisandra chinensis. Background technique

[0002] Schisandra, a plant of the genus Schisandra in the family Magnoliaceae, can be divided into northern Schisandra and southern Schisandra due to different growth regions. Schisandra chinensis is irregular spherical or oblate, with a diameter of 5-8mm. The surface of Schisandra chinensis is red, purple or dark red, the skin is shrunken, oily, and the flesh is soft, and some of the surface is black red or "hoarfrost". The granules of Schisandra chinensis are small, the surface is brown-red or dark brown, the peel is shriveled and shrunken, and the pulp often clings to the seeds. Traditional Chinese medicine believes that Schisandra is sour and warm in nature and non-toxic. It is usually used to treat cough and asthma caused by senile diseases cau...

Examples

Embodiment 1

[0042] Take 0.5mg of schisandrin A, gomisin D, schisandrin B, schisandrin, schisandrin A, schisandrin, schisandrin B, and schisandrin C respectively in a 10mL brown volumetric flask, add chromatographic grade methanol to dilute to Scale, sonication, so that the eight lignan compounds can be better dissolved in methanol, and the dissolved solution is stored in a refrigerator at 4°C for future use. With the concentration as the abscissa and the peak area as the ordinate, draw a standard curve, such as figure 2 shown.

[0043] Turn on the low-temperature constant temperature tank 3, set the temperature to 5°C, and when the set temperature is reached, open the high-purity air valve 1 and the high-purity CO 2 Valve 2, into high-purity air and CO 2 , make the system full of gas, at the same time, weigh 5g schisandra sample powder in the extraction kettle 6, and add 10mL of dehydrated ethanol, the concentration of the dehydrated alcohol is 100%, tighten the seal, then put the extr...

Embodiment 2

[0047] The specific steps and conditions are the same as in Example 1, except that the extraction pressure in the extraction kettle is respectively 0, 3, 7.5 and 12 MPa; the impact on the extraction rate of lignans under the different extraction pressures of Examples 1 and 2 like Figure 4 shown.

[0048] Figure 4 Note: without CO 2 In the case of , the extraction rate of the target substance is low, but with the increase of the extraction pressure, the supercritical CO 2 Continuously entering the inside of the sample greatly improves the mass transfer efficiency. When the extraction pressure is 9MPa, the extraction rate of the target analyte reaches the maximum. Description supercritical CO 2 As an extraction solvent, its dosage will have a crucial impact on the extraction rate of the target substance.

Embodiment 3

[0050] The specific steps and conditions are the same as in Example 1. The difference is that the concentration of ethanol is 40, 60, and 80% respectively. The effects on the extraction rate of lignans under different ethanol concentrations in Examples 1 and 3 are as follows: Figure 5 shown.

[0051] Figure 5 It shows that the higher the concentration of ethanol, the higher the extraction rate of the target compound. On the one hand, due to the large polarity of ethanol molecules, which greatly increases the lignans in supercritical CO 2 On the other hand, ethanol, as an organic solvent, is easy to form hydrogen bonds with lignans, which can significantly improve the extraction efficiency. Therefore, the use of absolute ethanol as an impregnating solvent has a good effect.

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