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Method for purifying quercetin glucoside in semen lepidii

A technology for quercetin glycoside and purification method, which is applied in the field of purification of quercetin glycoside, can solve the problems of being difficult to achieve, incomplete separation of gentiobiglycoside, low purity and the like, and achieves high product purity and simple extraction and separation method. Easy to operate, good to promote the effect of application value

Active Publication Date: 2021-07-23
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Literature search, the separation and purification process of quercetin-3-O-β-D-glucose-7-O-β-D-gentiobioside in Tinglizi chinensis is generally separated by macroporous resin, polyamide, etc. , and then through silica gel column chromatography or SephadexLH-20, the separation of quercetin-3-O-β-D-glucose-7-O-β-D-gentiobioside is not complete, the purity is low, and it is difficult to Meet the technical requirements of the national standard of traditional Chinese medicine with a purity of 98.5%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A practical separation and purification process for quercetin glycosides in Tinglizi, comprising the following steps:

[0023] S1. Take 200 kg of dried Tinglizi seeds and pass through a No. 4 sieve, add 4000 L of deionized water, heat and extract in a water bath, the extraction temperature is 80 ° C, and the water bath time is 1.5 h. Repeat the extraction three times, and combine the filtrates to concentrate and spray dry to obtain a dried sample.

[0024] S2. Take 500 g of the dried sample, dissolve it ultrasonically in 3.4 L of 60% ethanol for 15 min, keep it in the dark for 21 h, and then filter it. The filtrate is concentrated and freeze-dried to obtain a freeze-dried sample.

[0025] S3. Take 200g of freeze-dried sample, dissolve it in 1L of acid water with pH 4.5 and ultrasonically dissolve it for 15 minutes, take acid water with pH 4.5 to elute the activated LX-68G macroporous resin, and load the sample. After 1.2 column volumes of water elution, gradient elution...

Embodiment 2

[0039] A practical separation and purification process for quercetin glycosides in Tinglizi, comprising the following steps:

[0040]S1. Take 200 kg of dried Tinglizi seeds and pass through a No. 4 sieve, add 4000 L of deionized water, heat and extract in a water bath, the extraction temperature is 80 ° C, and the water bath time is 1.5 h. Repeat the extraction three times, and combine the filtrates to concentrate and spray dry to obtain a dried sample.

[0041] S2. Take 550 g of the dried sample, dissolve it ultrasonically in 3.8 L of 60% ethanol for 20 min, let it stand in the dark for 26 h, and then filter it. The filtrate is concentrated and freeze-dried to obtain a freeze-dried sample.

[0042] S3. Take 145 g of freeze-dried samples, dissolve them in 2.8 L of acidic water with pH 4.5 and ultrasonically dissolve them for 30 minutes, take acidic water with pH 4.5 to elute the activated LX-68G macroporous resin, and load the samples, and let stand for 1.5 hours after loading....

Embodiment 3

[0056] A practical separation and purification process for quercetin glycosides in Tinglizi, comprising the following steps:

[0057] S1. Take 200 kg of dried Tinglizi seeds and pass through a No. 4 sieve, add 4000 L of deionized water, heat and extract in a water bath, the extraction temperature is 80 ° C, and the water bath time is 1.5 h. Repeat the extraction three times, and combine the filtrates to concentrate and spray dry to obtain a dried sample.

[0058] S2. Take 400 g of the dried sample, ultrasonically dissolve it in 3 L of 60% ethanol for 25 min, keep it in the dark for 20 h, and then filter it. The filtrate is concentrated and dried under reduced pressure to obtain a dried sample.

[0059] S3. Take 139 g of dried sample, dissolve it with 3.6 L of acidic water with pH 4.5 and ultrasonically dissolve it for 25 minutes, take acidic water with pH 4.5 to elute the activated LX-68G macroporous resin, and load the sample. After 1 column volume was eluted with deionized w...

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PUM

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Abstract

The invention discloses a method for purifying quercetin glucoside in semen lepidii. The method is characterized by comprising the following steps of (1) carrying out primary water extraction on quercetin-3-O-beta-D-glucose-7-O-beta-D-gentiobioside in the semen lepidii; (2) performing alcohol precipitation and impurity removal on the semen lepidii water extract; (3) eluting and separating by using LX-68G type macroporous resin; (4) eluting and purifying with a CM-agarose gel FF column; and (5) carrying out preparative liquid phase purification, so as to obtain a quercetin-3-O-beta-D-glucose-7-O-beta-D-gentiobioside monomeric compound. Experimental results show that the CM-agarose gel FF has a good purification effect on quercetin-3-O-beta-D-glucose-7-O-beta-D-gentiobioside, the purity of a sample subjected to preparative liquid phase separation and purification can reach 99.0% or above, the technical requirement that the purity of the sample is larger than 98.5% of a national traditional Chinese medicine reference substance is met, and the obtained product can be used as the traditional Chinese medicine reference substance.

Description

technical field [0001] The invention relates to a method for purifying quercetin glycoside in Tinglizi, in particular to the purification of quercetin-3-O-β-D-glucose-7-O-β-D-gentiobioside in Tinglizi craft. Background technique [0002] Tinglizi is the dry and mature seed of Artemisia soponica or L. chinensis of Cruciferae. The former is commonly called "Nan Tinglizi" and the latter is commonly called "Northern Tinglizi". Tinglizi is generally not used in prescriptions as a monarch drug in traditional Chinese medicine. It is generally used as an adjuvant drug or a single herb, and is often used to treat cough and asthma caused by lung heat caused by various reasons. In modern clinical applications, it is mostly used in compound Chinese medicines in combination with other drugs for the treatment of cardiovascular diseases and respiratory diseases. [0003] Quercetin-3-O-β-D-glucose-7-O-β-D-gentiobioside is the characteristic component in Tinglizi chinensis, which is used t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/07C07H1/08C07H1/06
CPCC07H17/07C07H1/08C07H1/06C07B2200/07
Inventor 李桂生周兰英马成俊
Owner YANTAI UNIV
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