Preparation method for ardisia mamillata triterpenoid saponin reference substance
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A technology of abatin and pyranoside, which is applied in the field of medicine, can solve problems such as unseen preparation methods, and achieve the effect of non-toxic, non-polluting solvents and less organic solvents
Active Publication Date: 2016-02-03
四川恩威制药有限公司
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However, there is currently no preparation method for the reference substance of tiger tongue red pigment B. In order to further explore the druggability and pharmacological activity of this product, we extracted and separ
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Embodiment 1
[0023] 1. Preparation of reference substance
[0024] 1) Take Hutonghong medicinal material, crush it through a 10-mesh sieve, add 10 times the amount of 80% ethanol to reflux for extraction for 2 hours, repeat the extraction 3 times, filter, combine the filtrates and recover the ethanol under reduced pressure to obtain Hutonghong extract;
[0025] 2) Put the extract on a D141 macroporous adsorption resin column, wash with water until the eluent is nearly colorless, discard the eluent; elute with 30% ethanol until the eluent is nearly colorless, discard the eluent; use 80 % ethanol to elute until the eluate is nearly colorless, collect the eluate, concentrate and dry under reduced pressure to obtain tiger tongue red extract;
[0026] 3) Mix the extract from 2) with an equal amount of silica gel, dry and finely grind it and pour it evenly into the upper end of the packed silica gel column, slowly add the mobile phase ethyl acetate:methanol (7:3) at an appropriate flow rate Car...
Embodiment 2
[0045] 1 Influence of the extraction process of tibatin B on the extraction rate
[0046] 1) The influence of the extraction method on the extraction rate
[0047] Take 3 parts of 10-mesh tiger tongue red medicine powder, each 50.00g. Add 10 times the amount of 80% ethanol respectively, after soaking for 30 minutes, one part was ultrasonically extracted at room temperature for 30 minutes; one part was reflux extracted for 30 minutes; The extract was filtered through a 200-mesh sieve, and the filtrate was concentrated under reduced pressure. The concentrate was evaporated to dryness in a water bath. The dry paste was dried in an oven at 70°C under reduced pressure for 8 hours, and the content of bechatin B was determined. The results are shown in Table 1.
[0048] Table 1 Comparison of extraction methods
[0049]
[0050] 2) The influence of extraction solvent on the extraction rate of tiger lipin B
[0051] Take 5 parts of tiger tongue red powder of 10 mesh, 50.00 g ea...
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Abstract
The invention discloses a preparation method for an ardisia mamillata triterpenoid saponin reference substance. The preparation method comprises the following steps: (1) performing extraction on the herb of ardisia mamillata; (2) performing macroporous adsorption resin column separation; (3) performing silica column chromatography; (4) performing preparative high performance liquid chromatography separation and purification, so as to obtain cyclamiretin A3-O-alpha-rhamnopyranoside-(1 to 2)-beta-D-glucopyranose-(1 to 4)-[beta-D-glucopyranose-(1 to 2)-]-alpha-L-arabinopyranoside. When the reference substance is detected by utilizing a plurality of development systems and developing systems of thin-layer chromatography, one spot is displayed in the chromatography; when the reference substance is further defected according to a high performance liquid chromatography-evaporative light scattering detection (HPLC-ELSD) method, the target peak of the reference substance is calculated according to a peak area normalization method, and the mass concentration of the reference substance is higher than 98%; when different chromatographic columns and a plurality of mobile phase systems are adopted for detection, the detection results are kept consistent and show that the reference substance, namely prepared cyclamiretin A3-O-alpha-rhamnopyranoside-(1 to 2)-beta-D-glucopyranose-(1 to 4)-[beta-D-glucopyranose-(1 to 2)-]-alpha-L-arabinopyranoside, meets the requirements of chemical reference substances for traditional Chinese medicine quantitative analysis. The preparation method adopts a safe and non-toxic extraction solvent, and is relatively high in finished product yield.
Description
technical field [0001] The invention belongs to the technical field of medicine, and relates to the preparation of a chemical reference substance of active ingredients of traditional Chinese medicines, in particular to a preparation method of a tiger tongue triterpene saponin reference substance. Background technique [0002] Tiger Tongue Red is the dry whole plant of Ardisiama millata Hance, a plant of the genus Purple Gold Bovine, which is not only a famous ornamental plant, but also a commonly used herbal medicine in my country. The medicinal value has been recorded in the "Compendium of Materia Medica", and it has miraculous effects on the treatment of hepatitis, rheumatism, and malnutrition in children. Its main active ingredient is one of the triterpene saponins - cyclamine A3-O-α-rhamnopyranose-(1→2)-β-D-glucopyranose-(1→4)- [β-D-Glucopyranose-(1→2)-]-α-L-arabinopyranoside (abbreviated as basilicin B), which is present in the plant of the genus Aurantiaceae genus A. ...
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