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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.

Inactive Publication Date: 2013-04-17
DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In China, the solvent method is generally used to extract picroside, which has the disadvantages of high operating temperature, low yield, and long time consumption. The difference of the present invention is that the ultrasonic extraction method is mainly used, and the macroporous resin is used to purify lilypicroside in the later stage. The product Not only high yield, but also high purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention belongs to the field of natural organic chemistry, and relates to a method for extracting convallamarin from wild convallaria in great khingan, in particular to a novel method for purifying by using ultrasonic extraction, ultrafiltration separation, macroporous resin adsorption and combining with column chromatography. The method has the advantages that 1, an ultrasonic extraction technique is adopted, so that effective components are dissolved out rapidly; the loss of active components is less; 2, a macroporous resin purification technique is adopted, so that purification effects of the effective components are good; the method facilitates industrial mass production; and 3, ultrafiltration is conducted at a room temperature, so that structural changes, loss and biological activity reduction of the effective components caused by a heating effect are avoided; and the yield of the effective components is increased. The method adopts the ultrasonic extraction and a macroporous resin coupling technique; alcohol serves as an extraction solvent; the ultrafiltration separation is conducted; then macroporous resin purification is conducted; the column chromatography is adopted for further purification; and the purity of convallamarin in convallaria is increased to 98.7%.

Description

Technical field: [0001] The invention belongs to the field of natural organic chemistry, and relates to a method for extracting lily of the valley from wild lily of the valley in Daxing'an Mountains, in particular to a new method utilizing ultrasonic extraction, ultrafiltration separation, macroporous resin adsorption and column chromatography purification . Background technique: [0002] Lily of the valley, Liliaceae Lily of the valley, aliased as perfume flower, deer bell flower, grass jade bell, grass magnolia, small reed, mountain corn, born in the edge of the forest under the forest. Huzhong, Tahe, Jiagedaqi and other places in Daxingan Mountains have production. [0003] Plant form: perennial herb. Rhizome slender, with nodes, where numerous branched fibrous roots grow. Leaves 2, rarely 3, petiole 8-22 cm long, several membranous sheath leaves at base, blade oblong or ovate-lanceolate, 6-20 cm long, 2-8 cm wide, attenuate at base, Scapes derived from rhizomes, slig...

Claims

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Application Information

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IPC IPC(8): C07J71/00
Inventor 张亚红姚德坤姚德利万莉祁佩时
Owner DAXINGANLING LINGOBERRY BOREAL BIOTECH CO LTD
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