Novel technology method for extracting convallamarin from wild convallaria
A technology of lily of the valley glycoside and a new method, applied in the field of natural organic chemistry, can solve the problems of high operating temperature, high purity, low yield, etc., and achieve the effects of short extraction time, good purification effect, and simple and easy-to-operate method.
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Embodiment 1
[0024] Embodiment 1: A new method for purifying lilypicroside using ultrasonic extraction, ultrafiltration separation, macroporous resin adsorption and column chromatography, the steps are as follows:
[0025] (1) 1000g lily of the valley whole grass was cut to 3cm, adding ethanol with a volume fraction of 70%, using ultrasonic extraction, ultrasonic frequency 50KHZ, solid-liquid ratio 1:4, ultrasonic time 30min, extraction temperature 40°C, recovered ethanol, thin-layer chromatography Detection and analysis, collection of lilypicroside part;
[0026] (2) Recover ethanol, detect and analyze by thin-layer chromatography, and collect the lilypicroside part;
[0027] (3) Ultrafiltration membrane separation is adopted, the operating pressure of the membrane is 0.2MPa, the molecular weight cut-off is 1000, and the rejection rate is 90%;
[0028] (4) Adopt macroporous adsorption resin to adsorb and purify lily of the valley, the resin model is AB-8, the best adsorption conditions a...
Embodiment example 2
[0033] Implementation Case 2: A new method for purifying lilypicroside using ultrasonic extraction, ultrafiltration separation, macroporous resin adsorption and column chromatography, the steps are as follows:
[0034] (1) 1000g lily of the valley whole grass was cut to 4cm, adding ethanol with a volume fraction of 75%, using ultrasonic extraction, ultrasonic frequency 80KHZ, solid-liquid ratio 1:5, ultrasonic time 40min, extraction temperature 45°C,
[0035] (2) Recover ethanol, detect and analyze by thin-layer chromatography, and collect the lilypicroside part. residue.
[0036] (3) adopt ultrafiltration membrane separation, membrane operating pressure is 0.3MPa, molecular weight cut-off 2000, rejection rate is 5%;
[0037] (4) Adopt macroporous adsorption resin to adsorb and purify lilypicroside, the resin model is HPD-100, the best adsorption conditions are diameter-to-height ratio 17, volume flow rate 3BV / h, flow rate 4BV / h, and adsorption pH value is 6;
[0038] (5) An...
Embodiment example 3
[0042] Implementation Case 3: An analysis method for purifying lilypicroside using ultrasonic extraction, ultrafiltration separation, macroporous resin adsorption and column chromatography, the steps are as follows:
[0043] (1) 500g lily of the valley whole grass was cut to 5cm, adding 80% ethanol by volume fraction, using ultrasonic extraction, ultrasonic frequency 100KHZ, solid-liquid ratio 1:6, ultrasonic time 50min, extraction temperature 50°C,
[0044] (2) Recover ethanol, detect and analyze by thin-layer chromatography, and collect the lilypicroside part. residue.
[0045] (3) Adopt ultrafiltration membrane to separate, membrane operating pressure is 0.2MPa, molecular weight cut off 5000, rejection rate is 95%;
[0046] (4) Adopt macroporous adsorption resin to adsorb and purify lilypicroside, the resin model is NKA-II, the best adsorption conditions are diameter-to-height ratio 18, volume flow rate 4BV / h, flow rate 5BV / h, and adsorption pH value is 7;
[0047] (5) An...
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