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Method for extracting chlorogenic acid
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A chlorogenic acid and phase separation technology, applied in the field of medicine and chemical industry, can solve the problems of poor adsorption effect and small adsorption capacity, and achieve the effect of easy operation and simple process.
Inactive Publication Date: 2012-06-27
INST OF APPLIED CHEM JIANGXI ACAD OF SCI
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But the resin adsorption effect that this invention selects is poor, and this is because chlorogenic acid belongs to polyhydric phenolic acid, contains polar groups such as hydroxyl, phenolic carboxyl in its molecular structure, and whole molecule is medium weak polarity, and for non- Polar resin (such as HPD-100, HPD-300), its adsorption capacity is small
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Embodiment 1
[0022] a. Water extraction: Eucommia leaves are pretreated and dried at 45°C to 65°C for 5-6 hours. The samples were crushed to 40-60 mesh. Use water as the extraction solvent, solid-to-liquid ratio = 1:10, extract 3 times at 65°C, 45min / time, and filter.
[0023] b. Pass through the column: the filtrate obtained in step a is adjusted to pH2, put on a 306-type macroporous resin column, the flow rate is 2ml / min, eluted with 70% ethanol, and the eluent is concentrated;
[0024] c. Extraction: adjust the pH of the concentrated solution obtained in step b to 2, add ethyl acetate for extraction.
[0025] d. Phase separation: add petroleumether to the extract obtained in step c, which is 40% of the volume of the extract, fully mix, and collect the lower aqueous phase;
[0026] e. Recrystallization: the aqueous phase obtained in step d is crystallized, recrystallized, and vacuum-dried to obtain the finished product of chlorogenic acid.
[0027] The purity of the sample can reach ...
Embodiment 2
[0029] a. Water extraction: honeysuckle pretreatment, at 45°C to 65°C, dry for 5-6 hours; crush the sample to 40-60 mesh; use water as extraction solvent, solid-liquid ratio = 1:10, 65°C, 45min / time, Extract 3 times and filter.
[0030] b. Pass through the column: the filtrate obtained in step a is adjusted to pH 1, put on the XAD-6 type macroporous resin column, the flow rate is 2ml / min, elute with 70% ethanol, and the eluent is concentrated;
[0031] c. Extraction: adjust the pH of the concentrated solution obtained in step b to 1, add ethyl acetate for extraction.
[0032] d. Phase separation: add chloroform to the extract obtained in step c, which is 40% of the volume of the extract, fully mix, and collect the lower aqueous phase;
[0033] e. Recrystallization: the aqueous phase obtained in step d is crystallized, recrystallized, and vacuum-dried to obtain the finished product of chlorogenic acid.
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Abstract
The invention relates to a method for extracting chlorogenic acid, which belongs to the technical field of pharmaceutical chemicals. The method combines macroporous resin enrichment, ethyl acetate extraction and a mixed solvent split-phase method to achieve multi-step gradient purification of the chlorogenic acid so as to obtain a chlorogenic acid product with high purity. The method comprises the processes of water extraction, column passing, extraction, phase splitting and recrystallization. The macroporous resin adopted by the column passing process is 306 type or XAD series resin; and thesplit-phase agent adopted by the split-phase method is petroleumether, chloroform or the mixture of the petroleumether and the chloroform. The method is applicable to the process of extracting and preparing the chlorogenic acid from honeysuckles, cortex eucommiae leaves and cortex eucommiae barks.
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