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Preparation method of test article for detecting carboxyatractyloside and/or atractyloside by use of HPLC (High Performance Liquid Chromatography)

A technology of carboxy atractylodes and atractylodes, applied in the field of preparation of test products, can solve the problems of high requirements on instrument conditions, complex components, low component content, etc., and achieve the effect of improving sensitivity and detection limit

Active Publication Date: 2015-07-01
SICHUAN ACAD OF CHINESE MEDICINE SCI
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Problems solved by technology

For cocklebur medicinal material or decoction pieces, the conventional water ultrasonic extraction solution can be directly used as the test solution, but for the compound preparation of traditional Chinese medicine, because of its complex composition, the content of atractylodes glycosides in it is low, and it is weakly absorbed at the end, so Due to the large interference of other components, the test solution prepared in a conventional way is often difficult to meet the requirements of HPLC analysis and detection
For this reason, Chen Lulu et al. reported the use of LC-MS in "Determination of the content of atractyloside, the toxic component in four kinds of compound granules containing Xanthium Fructus" (New Drugs and Clinical Pharmacology of Chinese Medicine, 2013,24(3):297). Chromatography has been used to determine the content of atractylodes in several compound granules, but it is difficult to be widely used because of its high requirements on instrument conditions

Method used

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  • Preparation method of test article for detecting carboxyatractyloside and/or atractyloside by use of HPLC (High Performance Liquid Chromatography)

Examples

Experimental program
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Effect test

Embodiment 1

[0018] Take about 1.0 g of Fructus Xanthii powder (passed through No. 3 sieve), weigh it accurately, put it into a stoppered Erlenmeyer flask, add 20 mL of water precisely, and process it ultrasonically (power 300 W, frequency 40 kHz) for 40 min, take it out, and centrifuge , take 10ml of the supernatant (pH 6.2), adjust the pH to 5 with hydrochloric acid solution, put it on a D101 macroporous adsorption resin column (with an inner diameter of about 1cm, and a column height of about 10cm), and wash it with about 3 times the column bed volume of pH 5 water to remove Miscellaneous, discard the water, then elute with 50 (v)% ethanol about 4 times of the column bed volume, collect the ethanol eluate, and reclaim the solvent under reduced pressure below 60°C to obtain the said test product. Or after recovering the solvent from the ethanol eluent, transfer it directly to a 10ml measuring bottle with water, add water to the mark, shake well, filter, and take the subsequent filtrate as...

Embodiment 2

[0020] Take about 0.5 g of Biyuan pill powder, weigh it accurately, put it into a stoppered Erlenmeyer flask, add 25 mL of water precisely, ultrasonicate (power 300 W, frequency 40 kHz) for 40 min, take it out, centrifuge, and take 15 ml of supernatant ( The pH value is about 6), adjust the pH to 5 with hydrochloric acid solution, pass through a D101 macroporous resin column (about 1.2 cm in inner diameter, about 10 cm in height), wash with 30 mL of pH 5 water and 40 mL of 50% ethanol for elution, and collect the alcohol The eluate was concentrated under reduced pressure below 60 ℃ to about 5 mL, passed through a WAX solid-phase extraction column (pre-activated with 6 mL each of methanol and water), washed with an appropriate amount of water, and passed through the column together, 5% formic acid aqueous solution, 5% Each 6mL methanol solution of formic acid was rinsed sequentially to remove impurities, and then eluted with 9mL 2% ammonia water methanol solution, the eluate was...

Embodiment 3

[0022] Take about 0.5 g of Tongqiao rhinitis granule powder, weigh it accurately, put it into a stoppered Erlenmeyer flask, add 25 mL of pH 5 buffer solution accurately, ultrasonicate (power 100 W, frequency 40 kHz) for 50 min, take it out, centrifuge it, and take it out. 15ml supernatant (pH 5), adjust pH 4 with sulfuric acid solution, pass through D101 macroporous resin column (inner diameter about 1.2 cm, column height about 10 cm), wash with pH 6 water 25mL and 70% ethanol 50mL to elute , collect the alcohol eluate and concentrate it under reduced pressure below 60 ℃ to about 5 mL, pass through a WAX solid-phase extraction column (pre-activated with 6 mL each of methanol and water), wash the utensils with an appropriate amount of water, and pass through the column together, 1% formic acid aqueous solution 10mL, 4mL of 7% methanol solution of formic acid were rinsed in order to remove impurities, and then eluted with 8mL of 5% ammonia water methanol solution, the eluate was ...

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Abstract

The invention relates to a preparation method of a test article for detecting carboxyatractyloside and / or atractyloside by use of HPLC (High Performance Liquid Chromatography). A tested article extract aqueous solution containing carboxyatractyloside and / or atractyloside and with the pH value of less than or equal to 6 is adsorbed by macroporous adsorption resin, water with the pH value of less than or equal to 6 is used for washing to remove impurities, an alcohol-water solution with the alcohol volume content of 50-70% is used for elution, eluant is collected and a solvent is removed, therefore, the test article is acquired; and the alcohol-water solution for elution is an ethanol-water solution or methanol-water solution. According to the method, impurity interference can be removed sufficiently, the sensitivity and the detection limit are improved, the detected atractyloside ingredient cannot be lost or damaged, the factors such as chromatographic separation effect (separation degree), reproducibility, stability, precision, recovery rate and the like meet the requirements of the standard traditional Chinese medicine quality analytical method.

Description

technical field [0001] The invention relates to a preparation method of a test sample for detecting carboxy atractyloside and / or atractyloside by high performance liquid chromatography. Background technique [0002] Fructus Xanthii is a commonly used poisonous traditional Chinese medicine with a long history of clinical use. It has the effects of dispersing wind and dehumidification, clearing the nose and resuscitating the nose. In recent years, there have been reports of adverse reactions such as kidney, liver, and heart damage or abdominal pain, nausea, and vomiting after taking Xanthium. Regarding the toxic material basis of Xanthium Fructus, modern researches generally believe that its toxic components are mainly water-soluble carboxyatractyloside (CAT, carboxyatractyloside), atractyloside (AT, atractyloside) and their derivatives. [0003] For the components of atractylodes glycosides in Fructus Xanthii, including carboxy atractylodes glycosides, atractylodes glycosid...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 易进海刘鹏刘玉红刘云华黄志芳陈燕
Owner SICHUAN ACAD OF CHINESE MEDICINE SCI
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