Preparation method of chebulaic acid in myrobalan meat and content determination method of chebulaic acid in myrobalan meat

A technology of chelic acid and a determination method, which is applied to the preparation method of chelic acid in myrobalan meat and the field of content determination thereof, can solve the problems of high cost, imperfect technology, complicated equipment, etc., and achieves a precise content determination method and promotes The effect of industrialization development and low equipment requirements

Active Publication Date: 2022-04-29
LIAONING UNIV OF TRADITIONAL CHINESE MEDICINE
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Problems solved by technology

[0005] At present, the separation and preparation of chrysalis acid is still in its infancy at home and abroad, and the technology is not perfect enough.
CN102020682A, disclosed on April 20, 2011 a method for preparing ellagic acid from chebula leaves, the purity of the obtained chebula acid product can reach more than 98%, but strong alkali and strong acid are needed, and 10 kg of raw materials Only 35 g of the product was obtained, and the yield was low; CN104945447A disclosed a method for preparing ellagic acid from the leaves of Myrobalan chebula on September 30, 2015. The raw material was subjected to enzymatic hydrolysis, ultrasonic extraction, ceramic membrane separation, macroporous Resin adsorption and other steps, the steps are cumbersome, and the product purity is below 90%; CN105949252A, disclosed on September 21, 2016, a method for preparing challelac from chebula medicinal materials by high-speed countercurrent chromatography, but the equipment used is complicated, Expensive, and its product yield is less than 0.004%, and the purity is only greater than 95%
CN109867704A, on June 11, 2019, disclosed a method for preparing chellia acid by ethanol warm soaking method, and CN110724172A, on January 24, 2020, disclosed a method for preparing chellia acid by ethanol reflux method, both methods Using Amla emblica as raw material, separated by macroporous resin column, the purity of the obtained challelac acid products is above 98%, but only about 2 g of challek acid products can be obtained from 100 g of medicinal materials.
Hu Qiping is equal to " Chinese herbal medicine " published a kind of method about the determination of the content of chebula acid in Myrobalan, and the extraction solvent of used test sample is methanol, but the inventor's long-term experience of researching chebula has found that chebula acid is in methanol Extremely unstable in the solvent, and the higher the methanol content in the solvent, the worse its stability, this feature will have a great impact on the accuracy of its content determination

Method used

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  • Preparation method of chebulaic acid in myrobalan meat and content determination method of chebulaic acid in myrobalan meat
  • Preparation method of chebulaic acid in myrobalan meat and content determination method of chebulaic acid in myrobalan meat
  • Preparation method of chebulaic acid in myrobalan meat and content determination method of chebulaic acid in myrobalan meat

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Embodiment 1

[0044] Embodiment 1, a kind of method of extracting chellia from chebula meat.

[0045] The method described in the embodiment of the present invention one high-efficiency liquid chromatography detects the content of chellia acid, if no special instructions, is the following method:

[0046] Preparation of the test solution: Accurately weigh 0.1 g of the sample, add 25 mL of 70% methanol, accurately weigh the weight, sonicate for 30 min, let it cool, use the extraction solvent to make up for the lost weight, filter, and take 2 mL of the filtrate to volume into a 10 mL volumetric flask, and filtered through a 0.45 µm microporous membrane;

[0047] Chromatographic conditions: Dikma Platisil chromatographic column (250 mm×4.6 mm, 5 µm); mobile phase: phase A is formic acid-water (0.1:100 v / v), phase B is methanol, elution gradient: 0-2 min, B is 5%→38%; 2-12 min, B is 38%; 12-13 min, B is 38%→48%; 13-20 min, B is 48%; 20-25 min, B is 48% →100%; injection volume: 5 μL; column te...

example 1

[0049] Example 1: a kind of method for preparing chellia acid reference substance from chebula meat - the extraction process of cheliale acid in chebula, comprising the following steps:

[0050] (1) Remove the pit from the fruit of Myrobalan, crush the pulp, and pass through a 65-mesh sieve. Weigh 5 g of the chebula powder, add 25 times the amount of 70% ethanol aqueous solution and ultrasonically extract twice, each time for 20 min. Extraction at 3000 r·min -1 Centrifuge at a high speed for 10 min, take the supernatant and recover ethanol under reduced pressure to dryness;

[0051] (2) Take the above-mentioned dry paste equivalent to 0.1 g of the original medicinal material to prepare the test solution, and the extraction amount of Helilelic acid detected by HPLC method is 97.36 mg / g, and the extraction rate is 69.44%.

example 2

[0052] Example 2: a kind of method for preparing chellia acid reference substance from chebula meat - the extraction process of cheliale acid in chebula, comprising the following steps:

[0053] (1) Remove the pit from the fruit of Myrobalan, crush the pulp, and pass through a 120-mesh sieve. Weigh 5 g of the chebula powder, add 25 times the amount of 70% ethanol aqueous solution and ultrasonically extract twice, each time for 20 min. Extraction at 3000 r·min -1 Centrifuge at a high speed for 10 min, take the supernatant and recover ethanol under reduced pressure to dryness;

[0054] (2) Take the above-mentioned dry paste equivalent to 0.1 g of the original medicinal material to prepare the test solution. The extraction amount of chellia acid detected by HPLC is 106.99 mg / g, and the extraction rate is 76.31%.

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Abstract

The invention relates to the field of preparation and detection of traditional Chinese medicine chemical components, in particular to a preparation method and a content determination method of chebulaic acid in myrobalan meat. According to the method for preparing the chebulinic acid from the myrobalan meat, the product purity can reach 99% or above, the total yield can reach 60% or above, and the method can be applied to quality control of the chebulinic acid as a standard substance or a reference substance. Moreover, the method is simple in operation steps, low in equipment cost, applicable to industrial production and suitable for preparation of a large number of chebulaic acid reference substances. The method for determining the content of chebulagic acid in myrobalan can accurately detect the content of chebulagic acid in myrobalan meat, lays a theoretical basis and an experimental basis for establishing a quality standard of myrobalan, and has important significance for promoting industrial development of myrobalan.

Description

technical field [0001] The invention relates to the field of preparation and detection of chemical components of traditional Chinese medicines, in particular to a preparation method and content determination method of chebula acid in chebula meat. Background technique [0002] Myrobalan is a plant of Junziceae Myrobalan ( Terminalia chebula Retz.) or myrobalan ( Terminalia chebula Retz.var. tomentella Kurt.) has the effects of astringing the intestines to stop diarrhea, astringing the lungs and relieving cough. Modern chemical research shows that the main chemical constituents of Myrobalan are tannins, including hydrolyzable gallotannins and ellagitannins. Among them, the component with a relatively high content of Helile acid is formed by the condensation of multiple gallic acids, and its structure is as follows: [0003] [0004] Preliminary studies have shown that chebula acid has strong antioxidant and anti-inflammatory capabilities. It is the main medicina...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8634
Inventor 王巍鞠成国张强陈九妹胡佳旭周灵丽郭美岑
Owner LIAONING UNIV OF TRADITIONAL CHINESE MEDICINE
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