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Preparation method of baicalein and scutellaria baicalensis flavone total-aglycone extractives
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A technology of baicalein and baicalein, which is applied to medical preparations containing active ingredients, drug combinations, and pharmaceutical formulas, etc., can solve the problems of low baicalein content, affecting the yield and purity of total aglycones of baicalein, and achieve content High, ideal industrial production feasibility, simple and convenient steps
Active Publication Date: 2013-10-23
SICHUAN ACAD OF CHINESE MEDICINE SCI
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Problems solved by technology
When using organic solvents for extraction, more fat-soluble impurities will be brought in, which affects the yield and purity of the total aglycones of baicalein flavones in the product, resulting in the main active ingredient baicalein in the total aglycone extract of baicalein flavones. lower content
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Embodiment 1
[0017] Experiments on the relationship between the solubility of baicalin in water and the pH value:
[0018] Take 500ml of distilled water, add 8g of pure baicalin, stir at room temperature (~15°C) for 30 minutes, it can be seen that baicalin is basically insoluble, and the pH value of the test liquid is 3.8; take a sample, and the content of baicalin in it is determined by HPLC method to be 0.024mg / ml. With continuous stirring, 10% sodiumhydroxide solution was added dropwise to the liquid until the baicalin was completely dissolved, and the pH of the solution was detected to be 5.8. Therefore, when the pH value is ≥ 5, especially ≥ 6, baicalin is easily dissolved in water and leached out at a lower temperature.
Embodiment 2
[0020] Experiments on the relationship between the activity of baicalinase and temperature:
[0021] Take the crude powder of Scutellaria baicalensis, add 8 times of water, stir and extract twice at 0°C and pH 6, combine the extracts, and determine the contents of baicalin and baicalein in them are 6.05 mg / ml and 0.74 mg / ml, respectively, by HPLC.
[0022] Take 2ml of the extract, and enzymatically hydrolyze it at 0, 10, 20, 30, 40, 50, 60, 70, and 80°C for 1 hour, add methanol to make the volume to 50ml, and determine the content of baicalin and baicalein by HPLC. The results are shown in Table 1. The results in Table 1 show that the activity of baicalinase is low below 30°C and is in an inhibited state; the enzyme activity is stronger at 40-60°C; it is basically inactivated at 70°C.
[0023] Table 1 The relationship between baicalinase activity and temperature
[0024] Temperature (°C) 0 10 20 30 40 50 60 70 Before enzymatic digestion Amount...
Embodiment 3
[0027] Experiments on the relationship between the activity of baicalinase and the pH value:
[0028] Take the crude powder of Scutellaria baicalensis, add 8 times of water, stir and extract twice at 0°C and pH 6, combine the extracts, and determine the content of baicalin by HPLC to be 5.93 mg / ml. Take an appropriate amount of extract, adjust the pH value to 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, enzymatically hydrolyze at 50°C for 1 hour, take the supernatant and centrifuge, and determine the content of baicalin by HPLC. Content, the results are shown in Table 2. The results in Table 2 show that baicalinase has strong activity at pH4~8.
[0029] Table 2 Relationship between baicalinase activity and pH
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Abstract
The invention relates to a preparation method of baicalein and scutellaria baicalensis flavone total-aglycone extractives, which comprises the following steps of: after sufficiently leaching crushed scutellaria baicalensis raw material by using water at the temperature of being less than 30 DEG C when the pH value is 5-9, collecting the leach liquor, keeping for 3-20 h when heating to the temperature of being less than 70 DEG C, and collecting separated sediment, namely baicalein and scutellaria baicalensis flavone total-aglycone extractives. According to the method disclosed by the invention, flavonoidglycoside components and activity inhibited scutellaria baicalensisenzyme are sufficiently leached by using low-temperature water according to physicochemical properties of baicalein, scutellaria baicalensisflavonesglucoside components and self scutellaria baicalensisenzyme; then, after the activity of scutellaria baicalensis enzyme is recovered and the flavonesglucoside components are subjected to enzymolysis under the heating conditions, aglycone components, such as baicalein and the like, are separated by utilizing indissoluble property in water; and the scutellaria baicalensis flavone total-aglycone extractives with the baicalein content of being more than 50% are obtained. The preparation method disclosed by the invention is simple and convenient in step and low in cost; and the industrial production process is feasible.
Description
technical field [0001] The invention relates to a preparation method of extract components of traditional Chinese medicine raw materials, especially baicalein and baicalin total aglycone (or called baicalin total aglycone, baicalin total flavone aglycon) extract. Background technique [0002] Scutellaria baicalensis Georgi is a commonly used medicinal material recorded in the Chinese Pharmacopoeia, which has the effects of clearing away heat, purging fire and detoxifying. Studies have shown that the main active ingredients of Scutellaria baicalensis are flavonoids such as baicalin, wogonin, baicalein (baicalein) and wogonin. A comparative study on the pharmacological effects of baicalin and baicalein was reported in "Modern Research and Application of Traditional Chinese Medicine" (edited by Zheng Huzhan et al., Beijing Academy Press, January 1998, p3960), which proved that baicalein has a stronger effect than Baicalin. Hu Shilin et al. ("Chinese Journal of Pharmaceutical...
Claims
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Application Information
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