Method for extracting podophyllotoxin from umbrella leaf

A technology of podophyllotoxin and mountain lotus leaf, which is applied in the field of purification of podophyllotoxin, can solve the problems of large loss of target components, large amount of organic reagents, complicated operation, etc., and achieve the effect of low cost, short cycle and simple production process

Inactive Publication Date: 2011-02-16
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] As mentioned above, the existing process of extracting podophyllotoxin has the probl...

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The lotus leaves are crushed to 20 mesh, 1 kg is put into a flask, 6 times the amount of 85% methanol solution is added, ultrasonically extracted 3 times, each extraction is 1 hour, the combined extracts are concentrated to obtain an extract, and the extract is used 4 times more Ethyl acetate was ultrasonically extracted twice, each time for 1.5 hours, suction filtered, the filtrate was concentrated to 1 / 6 of the original volume, left to crystallize, and the crude product was obtained after filtration. The above crude product was dissolved in 300ml of anhydrous methanol, 3g of activated carbon was added, and refluxed 1h, filter, add 2L chloroform to the filtrate, centrifuge, concentrate the organic layer, place crystals, add 200ml of anhydrous methanol to reflux to dissolve the above crystals, concentrate, let cool to crystallize, repeat 3 times, filter out the crystals, and vacuum dry to obtain podophyllotoxin 38g, content 91.2%.

Embodiment 2

[0023] The lotus leaves are crushed to 40 mesh, 1 kg is put into a flask, 8 times the amount of 80% methanol solution is added, ultrasonic extraction is performed twice, each extraction is 2 hours, the combined extracts are concentrated to obtain an extract, and the extract is then 3 times acetic acid Ultrasonic extraction of ethyl ester for 3 times, 2 hours each time, filtration, the filtrate was concentrated to 1 / 5 of the original volume, left to crystallize, and the crude product was obtained after filtration; the above crude product was dissolved in 300ml of anhydrous methanol, 5g of activated carbon was added, and refluxed for 1h. Filtrate, add 3L chloroform to the filtrate, centrifuge, concentrate the organic layer, place crystals, add 180ml of anhydrous methanol to reflux the above crystals to dissolve, concentrate, let cool to crystallize, repeat 4 times, filter crystals, vacuum dry to obtain 28g of podophyllotoxin, The content is 89.6%.

Embodiment 3

[0025] The lotus leaves are crushed to 80 mesh, 2kg is put into a flask, 7 times the amount of 70% methanol solution is added, ultrasonically extracted 3 times, each time for 2 hours, the combined extracts are concentrated to obtain an extract, and the extract is then added with 5 times acetic acid Ethyl ester was ultrasonically extracted twice, each time for 2 hours, filtered, the filtrate was concentrated to 1 / 8 of the original volume, left to crystallize, and filtered to obtain a crude product, which was dissolved in 900ml of anhydrous methanol, 10g of activated carbon was added, and refluxed for 1h. Filtrate, add 4.5L chloroform to the filtrate, centrifuge, concentrate the organic layer, place crystals, add 400ml of anhydrous methanol to reflux to dissolve the above crystals, concentrate, let cool to crystallize, repeat 5 times, filter crystals, and vacuum dry to obtain 62g of podophyllotoxin , content 88.4%.

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Abstract

The invention relates to a method for extracting podophyllotoxin from umbrella leaves, comprising the following steps of: using the umbrella leaves as raw materials; ultrasonically extracting 75-85 percent of methanol; decompressing and condensing to obtain extract; ultrasonically extracting by using ethyl acetate; concentrating an extracting solution; placing crystals; dissolving the crystals by using absolute ethyl alcohol; refluxing and decoloring by adding active carbon; filtering, extracting an organic solvent; concentrating, crystallizing; and recrystallizing and drying absolute methanol to obtain the podophyllotoxin. The invention has simple technical operation and low cost.

Description

Technical field: [0001] The invention relates to a method for extracting podophyllotoxin from lotus leaves, in particular to a process for purifying podophyllotoxin by using methanol extraction, ethyl acetate extraction, active carbon decolorization and recrystallization. Background technique: [0002] Podophyllotoxin: 5R-5,8,8a,9-tetrahydro-9-hydroxy-5-(3,4,5-trimethoxyphenyl)furan(3′,4′:6,7)naphtho- [2,3-d]-1,3-dioxolen-6(5aH)-one. Soluble in chloroform, acetone, ethyl acetate and benzene, soluble in ethanol, ether, insoluble in water. Podophyllotoxin for condyloma acuminatum, multiple superficial epitheliomas (eg, multiple superficial or infiltrating basal cell tumors, squamous cell tumors, and basal squamous cell tumors), preepitheliomatous keratosis Seborrheic keratosis, actinic keratosis and ray keratosis, juvenile laryngeal papilloma, warts (vulgaris vulgaris, filiform warts). Podophyllotoxin can effectively inhibit herpes virus, inhibit cell metaphase mitosis, and...

Claims

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Application Information

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IPC IPC(8): C07D493/04
Inventor 刘东锋万冬梅杨成东
Owner NANJING ZELANG MEDICAL TECH
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