Radix scrophulariae iridoid reference extract and preparation method and application thereof
A ginseng iridoid and extract technology, which is applied in the field of scrophulariid iridoid control extract and its preparation, and achieves the effects of less impurities, high transfer rate and good reproducibility
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[0033]The preparation method of the Scrophulariaceae iridoid reference extract of the present invention comprises the following steps: 1) the preparation step of the Scrophulariaceae crude extract; 2) the preparation step of the Scrophulariaceae iridoid reference extract I; 3) the Scrophulariaceae iridoid reference extract I preparation step; Preparation steps of iridoid reference extract II; 4) Preparation steps of reference iridoid extract of Scrophulariaceae iridoids.
[0034]
[0035] (a) Reflux extracting the Scrophulariaceae medicinal material with water as a solvent for 2 to 3 times, each time for 1 to 2 hours, to obtain reflux extracts respectively. Preferably, reflux extraction is performed twice, each time for 1-1.5 hours. The water consumption each time is 9-12 times, preferably 9-11 times, more preferably 10-11 times the weight of the Scrophulariaceae medicinal material. The refluxing extracts are combined and concentrated until the relative density is 1.18-1.22...
preparation example 1
[0080] Preparation Example 1-Preparation of Scrophulariaceae Crude Extract
[0081] Adopt water as solvent, heat reflux extraction method to extract 100g of Radix Scrophulariae medical material, the extraction frequency is 2 times, the water consumption of each extraction is 10 times of the weight of Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Radix Scrophularis medicinal material for each extraction time, and each extraction time is 1 hour, merging the reflux extract, reducing Concentrate under pressure to a relative density of 1.20 to obtain the water extract of Scrophularia scrophulariae.
[0082] Add 95 vol% ethanol to the water extract of Scrophulariaceae until the ethanol concentration is 80 vol%, refrigerate at 4°C for 24 hours, filter with suction, concentrate under reduced pressure, and dry to...
Embodiment 1
[0084] The preparation of embodiment 1-Scrophulariaceae iridoid reference extract I
[0085] The crude extract of Scrophulariaceae in Preparation Example 1 was ultrasonically dissolved with 50 times the mass of methanol, and centrifuged to obtain a mother liquor, which was concentrated to obtain a methanol solution of 0.1 g / mL crude extract of Scrophulariaceae, and the crude extract of Scrophulariaceae was extracted Mix the methanol solution of the substance with the blank silica gel at a mass ratio of 1:2 to obtain the first mixed sample silica gel.
[0086] The first mixed sample silica gel is loaded on the first silica gel column with a diameter-to-height ratio of 1:15 (the crude extract of Scrophulariaceae in the first mixed sample silica gel is 3g, and the mass ratio of blank silica gel used in the first silica gel column is 1:50), and then eluted with the first eluent of 3.0BV to obtain the first silica gel column after elution; wherein, the first eluent is dichloro di...
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