Chimonanthus salicifolius total alkaloid extract, and preparation method and application thereof
A technology for total alkaloids and extracts, applied in the fields of application, food preparation, food science, etc., can solve problems such as the research on alkaloid monomer compounds that have not been seen, and achieve simple and easy extraction and preparation processes, wide distribution, and reduced treatment. cost effect
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Embodiment 1
[0023] Example 1 : Preparation of total alkaloid extract
[0024] Take a dry weight of 2.0 kg of wax plum branches and leaves, crush them, and cold-soak them with 3 times the amount of 90% methanol at room temperature for 24 hours, a total of 3 times. Combine 3 extracts, concentrate under reduced pressure to obtain 300 g extract, suspend with 2 times the amount of 3% tartaric acid aqueous solution, extract three times with ethyl acetate equal to the volume of the suspension, and then use Na 2 CO 3 The tartaric acid aqueous solution was adjusted to pH = 10, and then extracted three times with chloroform, and the chloroform extracted part was concentrated under reduced pressure to obtain 2.3 g of extract, which was the total alkaloid extract of Waxwort.
Embodiment 2
[0025] Example 2 : Preparation of total alkaloid extract
[0026] Take 2.0 kg dry wintersweet branches and leaves, crush them, reflux with 80% ethanol at room temperature for 3 hours, repeat 3 times, combine the extracts, concentrate under reduced pressure to obtain 330 g of extract, use 2 times the amount of 3% tartaric acid for the extract Suspended in aqueous solution, extracted three times with ethyl acetate equal to the volume of the suspension, and then washed with Na 2 CO 3 The tartaric acid aqueous solution was adjusted to pH = 10, extracted three times with an equal volume of chloroform, and the chloroform extracted part was concentrated under reduced pressure to obtain 2.6 g of the total alkaloid extract of Wintersweet.
Embodiment 3
[0027] Example 3 : prepare alkaloid monomer compound ( 1−4 )
[0028] Mix 2.0 g of the prepared total alkaloid extract with equal-fold silica gel (100-200 mesh), and perform column chromatography with 50 times the amount of silica gel (200-300 mesh), using dichloromethane: methanol as the mobile phase Gradient elution (volume ratio 1:0-0:1). Collect dichloromethane:methanol (15:1, volume ratio) elution fraction, this fraction continues through silica gel column, adopts dichloromethane:methanol 50:1, 30:1, 10:1 elution, for 30: 1. The eluted fraction was purified by preparative HPLC, eluted isocratically with methanol:water:diethylamine (68:32:0.05%), and the fraction was collected for 17.2 minutes to obtain 12.2 mg of white amorphous powder (−) -chimonanthine ( 3 ), collected 13.0 min components to obtain 8.1 mg of white amorphous powder salicifoxazine B ( 2 ); was eluted isocratically with methanol:water:diethylamine (75:25:0.05%), and the components were collected for ...
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