Method for separating and extracting bomeol glycoside from Ophiopogon japonicus
A technology of borneolside and Ophiopogon japonicus is applied in the field of separation and purification of traditional Chinese medicines, which can solve the problems of successful extraction or synthesis without a reference substance of borneolside, and a way to purchase the reference substance without borneolside, etc., and achieves short cycle, low cost, Simple steps to operate
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Embodiment 1
[0025] Take 4 parts of 2 kg of Ophiopogon japonicus roots (underground part, collected according to the 2015 edition of the Chinese Pharmacopoeia) (the content of borneoside in the medicinal material is 0.013%, that is, 0.26g of borneoside), and extract them in the following ways, and calculate Extraction rate of borneoside:
[0026] ① Add 2kg of Ophiopogon japonicus roots, add 4L of 85% ethanol aqueous solution to reflux and extract 3 times, each time for 1 hour, keep slightly boiling, filter the medicinal residues, combine the extracts, detect by HPLC-ELSD method, the quality extraction rate is 89.3 %.
[0027] ② Add 2kg of Ophiopogon japonicus roots, add 8L of 85% ethanol aqueous solution to reflux and extract twice, each time for 2 hours, keep slightly boiling, filter the medicinal residues, combine the extracts, detect by HPLC-ELSD method, the quality extraction rate is 91.2 %.
[0028] ③ 2 kg of Ophiopogon japonicus roots, add 8 L of ethanol aqueous solution with volum...
Embodiment 2
[0032] Get 20kg of root tubers of Ophiopogon japonicus (medicinal material borneoside detection content is 0.014%, namely containing borneoside 2.8g), add 60L volume concentration 90% ethanol aqueous solution reflux extraction 2 times, each time 2 hours, keep slight boiling, Filter the medicinal residues and combine the extracts; after concentrating to alcohol-free (about 6L), add deionized water to 80L, mix well and then refrigerate at 2-10°C for 36 hours to precipitate and remove impurities, and take the supernatant and filter it through a plate containing activated carbon Obtain 75L of water-sinking liquid, then go to D101 macroporous resin (8L) to separate, use 80L deionized water and 25L volume concentration 20% ethanol aqueous solution, 25L volume concentration 30% ethanol aqueous solution, 30L volume concentration 40% ethanol aqueous solution as washing Deliquidation and segmental elution, in which ethanol eluents with different concentrations need 5L as a receiving port...
Embodiment 3
[0034]Get 200kg of root tubers of Ophiopogon japonicus (medicinal material borneoside detection content is 0.016%, promptly contain borneoside 32.0g), add 600L volume concentration 90% ethanol aqueous solution reflux extraction 3 times, the first, the second time each time 2 hour, the third time for 1 hour, keep slightly boiling, filter the dregs, and combine the extract; after concentrating until alcohol-free, add deionized water to 500L, mix well, and then refrigerate at 2-10°C for 24h to precipitate and remove impurities, take the above The clear liquid was filtered through a plate frame containing activated carbon to obtain 480L of water-sinking liquid, and then separated by D1400 macroporous resin (80L), followed by 800L deionized water and 250L volume concentration of 20% ethanol aqueous solution, 250L volume concentration of 30% ethanol aqueous solution, and 300L volume concentration Concentration of 40% ethanol aqueous solution is used as the eluent for segmental elutio...
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