Method for extracting lycopodine from lycopodium clavatum
A technology of lycoporine and sarcocarpus, which is applied in the field of natural medicinal chemicals, can solve problems such as complex ingredients, and achieve the effects of simple operation, environmental protection, and less solvent
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Embodiment 1
[0017] Take Shenjin herb and crush it into 80-100 mesh, weigh 1kg, add 5L of 90% methanol for reflux extraction for 1 hour, filter the extract, add 3L of 90% methanol for reflux extraction for 1 hour, filter the extract and add 3L of reflux for extraction for 1 hour, combine Recover methanol from the extract to extract, add 120ml of 2% acetic acid aqueous solution to dissolve, filter, add 240g of calcium oxide to dry, add 500ml of petroleum ether for ultrasonic extraction for 1 hour, filter out petroleum ether, add 600ml of chloroform for ultrasonic extraction for 1 hour, and chloroform extraction Chloroform is recovered from the liquid, add 20g of silica gel (120-200) mesh to dry, and 200g of silica gel is packed into the column, chloroform methanol mixed solution (33:9) is eluted, thin-layer detection is collected high-concentration fraction recovery reagent, and then uses anhydrous Dissolved in ethanol and recrystallized three times, and dried to obtain 805 mg of pure lycopi...
Embodiment 2
[0019] Take Shenjin herb and crush it into 80-100 meshes, weigh 1kg, add 5L99% methanol for reflux extraction for 1 hour, filter the extract, add 5L99% methanol for reflux extraction for 1 hour, combine the extracts to recover methanol to the extract, add 100ml 4% Dissolve in acetic acid aqueous solution, filter, add 200g of calcium oxide to dry, add 400ml of petroleum ether for ultrasonic extraction for 1 hour, filter out the petroleum ether, add 500ml of chloroform for ultrasonic extraction for 1 hour, recover chloroform from the chloroform extract, add 30g of silica gel (120-200 ) order drying, and 150g of silica gel column packing, chloroform methanol mixed solution (27:9) eluting, thin-layer detection, collects high-concentration fraction recovery reagent, dissolves and recrystallizes 2 times with dehydrated alcohol again, dries to obtain lycoperme Pure product 826mg, content 95.5%.
Embodiment 3
[0021] Take Shenjin herb and crush it into 80-100 mesh, weigh 10kg, add 50L 90% methanol for reflux extraction for 1 hour, filter the extract, add 30L 90% methanol for reflux extraction for 1 hour, combine the extracts to recover methanol to the extract, add 1L 2% Dissolve acetic acid aqueous solution, filter, add 2.5kg of calcium oxide to dry, add 4L of petroleum ether for ultrasonic extraction for 1 hour, filter out the petroleum ether, add 6L of chloroform for ultrasonic extraction for 1 hour, recover chloroform from the chloroform extract, add 200g of silica gel (120- 200) mesh drying, and 1000g silica gel column packing, chloroform-methanol mixed solution (31:9) elution, TLC detection, collect high-concentration fractions to recover reagents, then dissolve and recrystallize 3 times with absolute ethanol, and dry to obtain Lycopodium The pure alkali product is 8.15g, the content is 97.1%.
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